MXPA96003738A - Method for the continuous preparation of organopolisilox emulsions - Google Patents

Abstract

The present invention relates to a method capable of continuously mass producing organopolysiloxane emulsions, which includes processes (I) and (II). Process (I) is the continuous supply of (a) fluid or organopolysiloxane gum, (b) emulsifying agent, and (c) water to a mixer having a first stage cutting and stirring (SSM) mechanism with a stator and a turbine-type rotor having blades that are inclined obliquely from the radial direction, when viewed from the axial direction, and a second stage SSM with a stator and a turbine-type rotor, having blades defining spiral curves with respect to the axial direction, and the discharge of an organopolysiloxane emulsion in water with an organopolysiloxane content of 10 to 99% by weight. Process (II) is the introduction of dilution water and process emulsion (I) in a mixer as described for process (I). A gas can also be injected into the process (

Description

METHOD FOR THE CONTINUOUS PREPARATION OF ORGANOPOLISILOXAN EMULSIONS FIELD OF THE INVENTION This invention relates to a method for the continuous preparation of organopolysiloxane emulsions.

More particularly, the present invention relates to a highly productive method for the preparation of highly stable and uniform storage emulsions.

BACKGROUND OF THE INVENTION Organopolysiloxane emulsions are widely used in the industry as lubricants, release agents, agents for the treatment of fibers, agents for the treatment of fiberglass, bases for cosmetics, polishes, and paint additives. The known methods for the preparation of organopolysiloxane emulsions are exemplified by (a) the mixing of an initial organopolysiloxane fluid, the emulsifying agent, and water using a mixer that applies a stirring action, for example, a Henschel ™ mixer. or mixer, and (b) the REF. 23073 mixing of the initial materials through the application of a cutting action using a colloidal mill or homomixer. In addition, Japanese Patent JP-A 59-51565 teaches a method using a cylindrical container and, installed therein, a stirring element with at least 3 discs placed at a fixed interval on an axis of rotation. The diorganopolysiloxane agent, the emulsifying agent and the water are continuously fed into the cylindrical vessel and are cut and stirred by the stirring element. However, when mass production of the organopolysiloxane is sought through continuous production, the prior art methods are poorly adaptable to the production of uniform, highly dispersed emulsions of organopolysiloxane, and these suffer from the problem of poor productivity. In Japanese Patent JP-A-59-51565, cutting and mixing must be conducted together with the application of pressure to make a uniform emulsion. This automatically incurs disadvantages such as higher operating costs due to increased energy, as well as costs associated with the reinforcement of the equipment structure. In addition, the material provided by this reference is a water-based fluid, which contains silicone similar to grease.

The use of this fluid in the above applications requires that it be dissolved and diluted with water in a batch process, using an agitator. In order to solve these problems, a method capable of carrying out continuous mass production of a uniform and highly dispersed organopolysiloxane emulsion in 08 / 498,963, Japanese Patent Application No. 7-9248 has been previously described. This method uses a low driving force and is not carried out under high pressure. As a result of the additional investigation, a continuous method capable of performing the direct production of organopolysiloxane emulsions which are already diluted with water at appropriate concentrations for the above applications has been found.

BRIEF DESCRIPTION OF THE INVENTION In specific terms, the present invention takes as its objective the introduction of a highly productive continuous method for the preparation of organopolysiloxane emulsions that, through the use of special SSMs, make it possible without pressurization and with low driving force, the continuous production mass of organopolysiloxane emulsions highly homogeneous and very stable to storage, which are already diluted with water at appropriate concentrations for immediate use. In yet another aspect of the present invention, a gas can be injected into the starting materials during mixing and emulsification. The method of the present invention for the preparation of organopolysiloxane emulsions achieves these objectives, and is a method for the continuous preparation of organopolysiloxane emulsions by processes (I) and (II) described below. Process (I) involves the continuous supply of (a) a fluid or organopolysiloxane gum, (b) an emulsifying agent, and (c) water, as the starting materials in the supply gate of a mixer. The mixer is a cylindrical housing or housing in which there are installed between the supply gate and the unloading gate of the cylindrical envelope, at least a first stage SSM (SSM), and a second stage SSM. The first stage SSM is a turbine-type rotor having blades that are inclined obliquely from the radial direction, when viewed from the axial direction, and a stator installed around the circumference of the rotor. The second stage SSM is a turbine type rotor having blades that describe spiral curves with respect to the axial direction, and a stator installed around the circumference of the rotor. These mechanisms are arranged in series along the initial feed direction, and are separated from one another by a relaxation zone. The method involves holding the initial materials in the first stage SSM, mainly an admission action and a cutting action at a cutting speed of at least 100 / second and then, after passing through the relaxation zone , in the second stage, mainly to phase inversion and rotation effects, and a cutting action at a cutting speed of at least 100 / second; and then discharging from the discharge gate an organopolysiloxane emulsion in water with an organopolysiloxane content of 10 to 99% by weight, based on the weight of the emulsion. The resulting process (II) is the continuous supply of water for the dilution and the organopolysiloxane emulsion in water made in the process (I) to the supply port of the cylindrical casing of a mixer, which has a cylindrical envelope in which they are installed between the supply gate and the unloading gate of the cylindrical casing, at the hands a first stage SSM and a second stage SSM. The first stage SSM is a turbine-type rotor having blades that are inclined obliquely from the radial direction, when viewed from the axial direction, and a stator installed around the circumference of the rotor. The second stage SSM is a turbine type rotor that has blades that describe spiral curves with respect to the axial direction, and a stator installed around the circumference of the rotor. The mechanisms are arranged in series along the initial feeding direction, and are separated from one another by a relaxation zone. The method involves holding the initial materials in the first stage SSM mainly to an admission action, and to a cutting action at a cutting speed of at least 100 / second and then, after passing through the relaxation zone , in the second stage SSM mainly for the effects of phase inversion and rotation, and a cutting action at a cutting speed of at least 100 / second; and then in discharging an organopolysiloxane emulsion in water, diluted in water, from the discharge port of the cylindrical envelope. In the process (I), the initial materials are subjected to an admission action and a cutting action, at a cutting speed of at least 100 / second due to the particular structure of the first stage SSM, which is a rotor turbine type having blades that are inclined obliquely from the radial direction when viewed from the axial direction, and a stator installed around the circumference of the rotor. Due to the particular structure of the second stage SSM which is a turbine type rotor equipped with spiral blade, and a stator, this stage holds the mixture to a strong cutting action at a cutting speed of at least 100 / second, between the stator and the spiral blades of the turbine type rotor. At the same time, the mixture is also impacted against the lateral surfaces of the spiral blades, which are inclined with respect to the rotational axis. This results in strong inversion and rotation effects that forcefully alter the phase in the radial and circumferential directions. The emulsification of the organopolysiloxane proceeds through a synergistic interaction between these actions and effects. The emulsification is even carried out by repeating the emulsification effects described above on at least two stages, with a relaxation zone interposed between the SSMs connected in series, successively. The total result is the. production of a highly dispersed, uniform, organopolysiloxane emulsion. In the resulting process (II), the water for dilution and the highly concentrated organopolysiloxane emulsion, made by the process (I), are separated and continuously fed to the supply gate of a mixer, which includes an enclosure or cylindrical housing in which there is installed between the supply gate and the unloading gate of the cylindrical envelope, at least a first stage SSM and a second stage SSM. The first stage SSM is a turbine-type rotor having blades that are inclined obliquely from the radial direction, when viewed from the axial direction, and a stator installed around the circumference of the rotor. The second stage SSM is a turbine type rotor that has blades that describe spiral curves with respect to the axial direction, and a stator installed around the circumference of the rotor. The mechanisms are arranged in series along the direction of the initial material feed, and are separated from one another by a relaxation zone. The emulsion and water for dilution are subjected in the first stage SSM to an action of admission and a cutting action, at least at a cutting speed of at least 100 / second, and are then subjected in the SSM. of second stage for the purpose of investment and rotation, and a cutting action at a cutting speed at the lower of 100 / second. This directly and continuously provides an emulsion that is uniformly diluted with water at an appropriate concentration for application, which is free of undissolved high concentrations of organopolysiloxane emulsion. The "cutting speed" Vs (1 / second) referred to herein is the value given by the equation. (1) V (1 / sec) = V / C In which V is the peripheral speed of the turbine type rotor in cm / second, and C is the empty space in centimeters between the inner surface of the stator and the peripheral surface, moving at peripheral speed V. The mixer used in the process (II ) may or may not be identical to the mixer used in the process (I).

DESCRIPTION OF THE DRAWINGS Figure 1 is a schematic diagram partially in cross-section, of a mixer used to perform the method of the present invention, for the continuous preparation of organopolysiloxane emulsions.

Figure 2 is a cross-sectional view, taken along line 2-2 in Figure 1, when viewed in the direction of the arrows.

Figure 3 is a cross-sectional view, taken along line 3-3 in Figure 1, when viewed in the direction of the arrows.

Figure 4 is a cross-sectional view, taken along line 4-4 in Figure 1, when viewed in the direction of the arrows.

Figure 5 is a perspective view of a rotor of the first stage SSM in the mixing apparatus of Figure 1.

DESCRIPTION OF THE INVENTION To facilitate understanding of the invention, and the mixing apparatus of Figures 1-5, the names of the various parts have been added to the Figures, in addition to their reference numbers. In this way, one is the cylindrical housing or enclosure, 2 is the supply gate, 3 is the escape gate, 5 is the rotary axis or shaft, 5 and 7 are the turbine type rotors, 5a and 7a are the blades, 6 and 8 are the stators, 8b are the straight notches, 9 and 10 are the SSMs, 11 is the zone or relaxation space, 12 are the projections in the shape of a sawtooth, 13 is the stator part or element, 13a are the projections in the shape of a saw tooth, and 14 is the flow passage or passage. The supply gate 2 can be provided with a separate inlet (not shown) for injecting and feeding a gas into the gate 2. Preferably, the gas is introduced separately from the initial materials supplied by the gate 2. In Figure 1, 1_ denotes a cylindrical housing or housing whose axial direction is above the horizontal. One end of this casing or housing is equipped with a gate 2 of initial material supply, while the other end is equipped with a discharge gate 3 ^ for the emulsified mixture. A rotating shaft k_ is inserted in the center of the cylindrical envelope l ^. The rotating shaft k_ is inserted from the left end of the cylindrical shell _, and extends into the vicinity of the supply gate 2_ on the right end. This is driven by a motor (not shown) that is located outside the envelope. Rotary axis 4 ^ is equipped with a rotor _5 at its end in the supply gate 2_, and with a rotor 7., in its intermediate part. The stators 6 ^ and 8 ^, which are fixed to the inner peripheral wall of the cylindrical envelope 1_, are installed around the circumferences of the rotors _5 and 7_, respectively, and in each case are separated from it by a small empty space. . The rotor _5 and the stator (>, constitute the SSM 9_, of the first stage, while the rotor 1_ and the stator J3, constitute the SSM JjO of the second stage.In addition, a relaxation space 11 with a relatively large volume, is installed between the SSM 9_, first stage and SSM JJD second stage.The rotor 5_, in the first stage SSM 9_ is a turbine-type rotor, from which a plural number of blades 5a project radially in a manner similar to a cone, towards the supply gate 2_> as shown in Figures 2 and 5. These blades 5a are substantially parallel to the axial direction in the plan view, but are inclined relative to the axial direction in the side view, and are inclined obliquely with respect to the radial direction when viewed from the axial direction The stator 6 ^ in the SSM 9 ^ forms an inner, almost conical, peripheral surface containing the notches 6b extending in the direction The rotor _5 is inserted into the conical stator b_ with the formation of a narrow gap with the peripheral edges of the blades _5_a. The minimum empty space size is 2 mm or less, and preferably of approximately 1 mm, as seen in Figure 2. The rotor _7 in the second stage SSM 1_0 is also a turbine-type rotor, but contrary to SSM 9_, the blades 7_a describe a spiral with reference to the axial direction. The blades 7_a are also shorter in the axial direction than the blades 5a of the rotor 5_ of the SSM 9_ as seen in Figure 3. The stator jB of the SSM K) has an almost conical shape, and its inner peripheral surface contains a number of straight notches 8_b extending in the axial direction. The rotor 7 is inserted into the stator 8 ^ with the formation of a small void space with the outer surfaces of the epirale blades 7a. This void space is formed to become progressively narrower in a wedge-like manner, moving from the upstream side to the downstream side, as shown in Figure 1. The minimum size of the void space is 2 mm or less, and is preferably about 1 mm. A number of sawtooth-like projections J ^ 2_, projecting in a backward direction, are present on the downstream end surface (for example, the surface perpendicular to the axial direction) of the rotor 7_ of the second SSM H). stage. These projections 12 move alternately radially, with a number of sawtooth shaped projections 13a fixed on a stator element 13. A narrow empty space remains interposed between the projections _1_2 and the projections 13a. These projections J_2 and 13a are formed in a spirally curved pattern, which extends radially outwardly along the radial direction, as shown in Figures 1 and 4. To execute the method of the present invention, for the continuous preparation of organopolysiloxane emulsions, the three starting materials, for example, (a) the organopolysiloxane fluid or gum, (b) the emulsifying agent, and (c) the water, are supplied in the process (I) to the gate of supply _2 of initial material of the mixing device, in which at least the first stage SSM 9_, described above and the second stage SSM 1_0, described above, are installed in series. These initial materials can be supplies separately, or they can be supplied in the form of a prepared mixture. The first-stage SSM performs a capture action and also an initial emulsification action on the initial materials. The pick-up action is performed mainly through the radially extending shape with outward direction, of the blades 5_a_ on the rotor _5 which are obliquely inclined with reference to the radial direction, when viewed from the axial direction. The initial emulsifying action occurs through microparticulation and emulsification of the organopolysiloxane gum or fluid resulting from the cutting action applied to the three initial materials between the outer peripheral surface of the knives _5_a and the internal wall of the stator 6. This Cutting action must apply cutting at a cutting speed of at least 100 / second. After the initial emulsification by the first stage SSM 9_, the mixture is squeezed in or the intermediate flow conduit _1_4, then fed into the relaxation space _1_1_, where it is released from its compressed state, and after that it is supplied to SSM 1_0 of the second stage. In the second stage SSM _1_0, a grinding action of the coarse materials is carried out by the stator 8_ and the spiral blades 7_a of the rotor 7_, while a fine grinding action is developed by the cutting action generated by the constant intake between the projections _1_2 in the form of a sawtooth, on the end surface downstream of the rotor 7_ and the sawtooth-shaped projections 13a on the stator element 13. After insertion into the space circumscribed by the rotor blades 7 and the internal wall of the stator 8_, the mixture is subjected to the effects of phase inversion and rotation due to the action of the blades 7_a, which are diagonally curved in the axial direction. This works to alter the phase to the radial and circumferential directions. A more uniform and even finer emulsification is obtained as the mixture, while being subjected to these effects of inversion and rotation, is at the same time also subject to a cutting action between the peripheral surfaces of the blades 7a_ and the inner wall of the blade. another stator 8, which is equipped with a number of straight notches 8_b. This cutting action must apply cutting at a cutting speed of at least 100 / second. The resulting emulsified mixture becomes even finer emulsified in the fine milling region downstream between the sawtooth-shaped projections 12 and 13a, producing a highly dispersed and uniform organopolysiloxane emulsion which is discharged from the discharge gate _3 in the cylindrical envelope 1_, as an organopolysiloxane emulsion in water, preferably containing 10 to 99% by weight, and more preferably from 20 to 99% by weight of organopolysiloxane. The emulsion discharged from organopolysiloxane will generally contain (a) from 10 to 99% by weight of fluid or organopolysiloxane gum, (b) from 0.1 to 89% by weight of emulsifying agent, and (c) from 1.0 to 89% by weight of water. In the resulting process (II), the dilution water and the highly concentrated organopolysiloxane emulsion prepared by the process (I), are separated and fed continuously to the gate 2 of the initial material supply of the other mixer, in which the SSM and SSM H) described above, are installed in series. The SSM 9 ^ of the first stage mainly performs an admission action on the initial materials, while also effecting an initial mixing and dissolution, by holding the feeding materials to a cutting action. This cutting action must apply cutting at a cutting speed of at least 100 / second. After mixing and initial dissolution by the first stage SSM, the mixture is squeezed in the passage or duct 1? _ Of intermediate flow, then fed into the relaxation space 11, where it is released from its compressed state, and supplies the second stage SSM I Q_. The second stage SSM .0 performs a grinding action of the coarse materials and a fine grinding action. After introduction into the space circumscribed by the blades 7_a of the rotor 7 and the internal wall of the stator 8 ^, the mixture is subjected to phase inversion and rotation effects, due to the action of the blades 7_a, which are curved diagonally in the axial direction. This works to change the phase to the radial and circumferential directions. An even finer and more uniform solution is obtained, because the mixture, while subject to these effects of inversion and rotation, is at the same time also subject to a cutting action between the peripheral surfaces of the blades 7_a and the wall internal of the stator 8 ^, which is equipped with a number of straight notches 8b. This cutting action must apply cutting at a cutting speed of at least 100 / second. The water-organopolysiloxane emulsion mixture as described above becomes even more finely dissolved and homogenized in the fine milling region downstream between the sawtooth-shaped projections 1_2_ and 13a, producing a highly dispersed organopolysiloxane emulsion. and uniform, which is diluted with water to an appropriate concentration for a particular application. This product is discharged from the discharge gate 3 ^ into the cylindrical housing l_. The continuous production of organopolysiloxane emulsions by the method of the present invention can be carried out using separate feeds of fluid or initial organopolysiloxane gum., emulsifying agent and water to the gate 2 of initial material supply, in the process (I), or by preliminary mixing of these initial materials and supplying them as a mixture to the supply gate 2 for the process (I). The dilution water used in the process (II) is preferably supplied separately from the relatively highly concentrated organopolysiloxane emulsion, made in the process (I). It is important in the present invention that there be installed in series at least one first stage SSM having a stator and a turbine type rotor, whose blades are inclined obliquely from the radial direction when viewed from the axial direction, and a second SSM stage having a stator and a turbine-type rotor, whose blades describe spirals with respect to the axial direction. This serial combination of two stages can be repeatedly connected in series a number of times, to obtain an even finer emulsification, dissolution and homogenization, as may be desired. Extremely fine emulsification, dissolution and homogenization is achieved by at least the two-stage combination described above. But also, a front stage with the SSM of first stage that mainly implements the capture of initial material and cutting activities, and a later stage that has the second stage SSM that mainly implements the investment and rotation activities, simultaneously with a cutting activity, makes possible the emulsification, dissolution and homogenization of the mixture at low pressures together with a low impulse energy. The process is improved by the presence of a relatively large relaxation zone between the first stage and second stage SSMs. A cutting speed of at least 100 / second, but preferably from 10,000 to 300,000 / second, must be applied to the mixture between the stator and the turbine-type rotor in each SSM. When a cutting speed of less than 100 / second is applied to the mixture, the process can not produce a highly dispersed and uniform emulsion diluted with water at the proper concentration for an intended application. With respect to the SSM (s) of the second stage, it is preferred to perform the first cutting action in a grinding zone of coarse material to carry out an emulsification, dissolution and homogenization of coarse tnate-rial, and perform the second action of cutting in a zone of fine grinding, to carry out the dissolution and homogenization through friction or fine wear. In addition to holding the mixture at these high cutting velocities, the continuous method of the invention also applies a strong inversion activity through the action of the spiral blades on the turbine-type rotor. This inversion action constantly alters the mixing phase in the radial and differential directions, and the synergy between this action and the aforementioned cutting action makes possible a much more efficient conversion of the mixture into a uniform emulsion. The organopolysiloxane (a) can be any organopolysiloxane which is a fluid or gum at room temperature. Compounds with the following average unit formula are examples of organopolysiloxanes (a): RaSiO (, 4. A) / 2 R represents substituted and unsubstituted monovalent hydrocarbon groups, for example, alkyl groups, such as methyl, ethyl, and propyl; aryl groups such as phenyl and tolyl; and groups in which all or part of the hydrogen bonded to the carbon has been replaced by halogen, such as chloromethyl and 3,3,3-trifluoropropyl. The subscript a_ in the formula has a value of 1.9 to 2.1. The organopolysiloxane (a) is exemplified by dimethylpolysiloxanes with terminal trimethylsiloxy block, dimethylpolysiloxanes with silanol terminal block, dimethylsiloxane-methylphenylsiloxane copolymers with terminal block trimethylsiloxy, dimethyl-c-siloxane-methylphenylsiloxane copolymers with silanol terminal block, dimethylsiloxane-copolymers diphenylsiloxane with terminal trimethylsiloxy block, copolymers of dimethylsiloxane-diphenylsiloxane with silanol end block, dimethylsiloxane-methyl (3,3,3-trifluoropropyl) -loxane copolymers with trimethylsiloxy end block, and dimethylsiloxane-methyl copolymers (3,3 , 3-trifluoropropyl) siloxane with silanol terminal block. The molecular structure of the organopolysiloxane (a) can be a straight chain, a straight partially branched chain, or a network. Straight chain organopoly siloxanes are preferred. When the organopolysiloxane is a fluid, it preferably has a viscosity at 25 ° C of at least 10,000 mma / s (centistokes). When the organopolysiloxane has a high viscosity, as in the case of a gum, it can be used by dissolving it in a solvent. The organopolysiloxane may contain additives, in an optional base, such as silica, as long as the present method is not adversely affected. Nonionic surfactants, anionic surfactants and cationic surfactants can be used as the emulsifying agent (b). Nonionic surfactants are exemplified by polyoxyalkylene alkyl ethers, polyoxyalkylene alkyl phenol ethers, polyoxyalkylene alkyl esters, polyoxyalkylene sorbitan alkyl esters, polypropylene glycol, and diethylene glycol. The anionic surfactants are exemplified by salts of fatty acids such as sodium laurate, sodium stearate, sodium oleate, and sodium linolenate; alkylbenzenesulphonic acids such as hexylbenzenesulfonic acid, octylbenzenesulfonic acid and dodecylbenzenesulphonic acid; salts thereof; and by alkylsulfone-cough and sulfate of sodium alkylphenyl ether-polyoxyethylene-no. Cationic surfactants are exemplified by octyltrimethylammonium hydroxide, dodecyltrimethylammonium hydroxide, alkyltrimethylammonium chlorides, and benzylammonium salts. Two or more types of these surfactants can be used in combination. This component (b) is added in sufficient quantity to emulsify the organopolysiloxane fluid or gum (a) in water (c). Component (c) is preferably added in an amount to provide 0.1 by weight of emulsifying agent in the organopolysiloxane emulsion made by process (I). The component (b) is also preferably added in the range of 1.0 to 100 parts by weight per 100 parts by weight of the organopolysiloxane fluid or gum (a) The water (c) can be tap water or water subjected to ion exchange. The amount of water used in the process (I) should provide from 1.0 to 89% by weight, and preferably from 1.0 to 79% by weight of water in the emulsion prepared in the process (I). The amount of water used in the process (I) is also preferably 1 to 400 parts by weight per 100 parts by weight of the organopolysiloxane (a). The amount of water used for the dilution in the process (II) is preferably from 1 to 2,000 parts by weight per 100 parts by weight of the organopolysiloxane (a). The organopolysiloxane emulsions made by the continuous method of this invention are emulsions in which the organopolysiloxane fluid or gum (a) is emulsified and dispersed in water, and typically has an average particle diameter in the range of 0.1 to 50. micrometers The organopolysiloxane emulsions according to the present invention can be directly used for applications such as fiber treatment agents, lubricants, release agents, glass fiber treatment agents, oil bases for cosmetics, polishes, defoamers and additives for painting.

Example 1 This example employed two mixers as described in Figure 1, connected in series. 100 parts by weight of dimethyl polysiloxane with terminal trimethylsiloxy block, with a viscosity at 25 ° C of 60,000 mm2 / s (centistokes), 9.0 parts in the first supply vessel of the first mixer were fed continuously into the gate 2. weight of polyoxyethylene lauryl ether, 3.4 parts by weight of cetyltrimethylammonium chloride, and 3.6 parts by weight of water subjected to ion exchange. These materials were mixed by high cutting and stirring until homogeneous, and were discharged as a trans-lucid emulsion in paste form, with a dimethylpolysiloxane content of 86.2% by weight, from the discharge damper 3 ^ of the first mixer . 100 parts by weight of this paste-like emulsion and 71 parts by weight of water for dilution, were then continuously fed to the gate 2_ of the initial material supply of the second mixer, where the cutting and stirring until homegeneity produced an emulsion of dimethylpolysiloxane with a dimethylpolysiloxane content of 50.4% by weight. In the first mixer used in this process, the rotational speed of the rotating shaft 4_ was 4,200 rpm; the minimum free space was 0.2 mm in the SSM 9_ of the first stage and in the SSM jhO of the second stage. The cutting speed in the first stage SSM 9_ was 93,000 / second and the cutting speed in the second stage SSM H) was 70,000 / second. The pressure in the gate 2 of initial material supply was 0.4 kg / cm2 G, and the pressure in the discharge gate 3 ^ was 0.0 kg / cm2 G. In these measurements, G is the gauge pressure, for example, the atmospheric pressure = 0.0 kg / cm3 G. In the second mixer used in this process, the rotation speed of the rotating shaft h_ was 3,000 rpm; the minimum free space was 0.2 mm in the SSM 9_ of the first stage and in the SSM H) of the second stage; the cutting speed in the SSM 9_ of the first stage was 66,000 / second; the cutting speed in the second stage SSM 1_0 was 50,000 / second; the pressure in gate 2_ of initial material supply was 0.0 kg / cm2 G; and the pressure in the discharge gate 3 ^ was 0.0 kg / cm2 G. The resulting emulsion of dimethyl polysiloxane prepared by this cutting and stirring process was a white emulsion such as milk in which the dimethyl polysiloxane was uniformly emulsified and dispersed in Water. Its average particle size was 0.4 microns. This emulsion had a viscosity at 25 ° C of 200 mPa 's (centipoise). Even though this emulsion was maintained for 6 months at room temperature, the dimethylpolysiloxane and water did not separate, indicating that this emulsion was extremely stable.

Example 2 This example used two of the mixers shown in Figure 1, connected in series. The following were fed continuously to the gate 2_ of initial material supply of the first mixer: 10 parts by weight of polyoxyethylene lauryl ether, 5.0 parts by weight of deionized water, and 100 parts by weight of a mixture with a viscosity at 25 °. C of 100,000 mm2 / s (centistokes), prepared by dissolution to homogeneity, of 42 parts by weight of dimethylpolysiloxane gum with terminal trimethylsiloxy block, with a viscosity at 25 ° C of 10'500,000 mma / s (centistokes) , in 58 parts by weight of isoparaffin with a relative density of 0.79 and a viscosity at 40 ° C of 2.4 mm2 / s (centistokes). These ingredients were mixed by cutting and stirring until homogeneous, and discharged as a translucent emulsion in paste form, with a dimethylpolysiloxane content of 36.5% by weight, from the discharge gate 3 ^ of the first mixer. This emulsion in the form of a paste and 82.4 parts by weight of water for dilution, equivalent to 71 parts by weight per 100 parts by weight of the emulsion in the form of paste discharged from the first mixer, were then continuously fed to the gate 2 of the Initial material of the second mixer, where cutting and stirring until homogeneous produced an emulsion of dimethylpolysiloxane gum with a dimethylpolysiloxane content of 21.3% by weight. In the first mixer used in this process, the rotation speed of the rotating shaft h_ was 4,200 rpm; the minimum free space was 0.2 mm in the SSM 9_ of the first stage and in the SSM H_. second stage; the cutting speed in the SSM 9. of the first stage was 93,000 / second; the cutting speed in the second stage SSM JJ) was 70,000 / second; the pressure in gate 2_ of initial material supply was 0.4 kg / cm2 G; and the pressure in the discharge gate 3 ^ was 0.0 kg / cm2 G. In the second mixer used in this process, the rotation speed of the rotating shaft 4 was 3,000 rpm; the minimum free space was 0.2 mm in the SSM 9_ of the first stage and in the SSM H) of the second stage; the cutting speed in the SSM 9_ of the first stage was 66,000 / second; the cutting speed in the second stage SSM JJ) was 50,000 / second; the pressure in gate 2_ of initial material supply was 0.0 kg / cm2 G; and the pressure in the discharge gate 3 was 0.0 kg / cm2 G. The emulsion of dimethyl polysiloxane made by this cutting and stirring process was a white emulsion like milk in which the dimethyl polysiloxane gum was emulsified and dispersed until homogeneity in water. Its average particle size was 0.4 microns. Even though this emulsion was maintained for 6 months at room temperature, the dimethylpolysiloxane and water did not separate, indicating that this emulsion was extremely stable. The continuous preparative method, illustrated above, according to the present invention, is characterized by its ability to continuously mass produce organopolysiloxane emulsions which are uniform, highly dispersed, and very stable to storage. The cutting and stirring processes in the continuous production of the present organophosiloxane emulsions are also implemented by bubbling in a gas such as air, nitrogen, carbon dioxide, or an inert gas such as argon. This feature of the present invention enables the preparation of even more uniform and more stable organopolysiloxane emulsions, and also allows a reduction in pressure within the mixer. Accompanying this is a decrease in the driving force required for agitation. The gas is preferably injected into the gate 2_ of initial material supply. The gas used in this aspect of the present invention promotes the emulsification of the organopolysiloxane emulsion, and produces a homogeneous emulsion and very stable. While gas is generally exemplified by air, nitrogen, argon, and carbon dioxide, air and nitrogen are preferred for their safety and ease of acquisition. The organopolysiloxane must be supplied in an amount that provides ? > a value from 0.01 to 100 (NL / hour) / (kg / hour), and preferably from 0.1 to 10 (NL / hour) / (kg / hour), for a proportion of the amount of gas injected into NL / hour to the amount of fluid or organopolysiloxane gum that is supplied, in kg / hour NL is Liter Normal at 0 ° C and one atmosphere. A uniform and highly stable emulsion is difficult to obtain when the ratio is below 0.01 (NL / hour) / (kg / hour). When the proportion exceeds 100 (NL / hour) / (kg / hour), the non-emulsified organopolysiloxane can remain in the emulsion, because the admissions or feeds will pass through the SSM without being subject to perfect cutting and stirring. It is not completely understood how the gas promotes emulsification and stabilizes the emulsion. Thus, for the preparation of emulsion in general, it has been considered that the bubble mixture exerts negative influences on the stability of the emulsion. This occurs because the mixed bubbles adsorb the emulsion at its interface, whereupon they are consumed, and due to the same time, they also adsorb emulsified droplets and cause them to float upwards. As a result, it has been considered to avoid mixing the bubbles as essential for the preparation of emulsion. However, in the present method, the continuous injection of the gas promotes the agitation and mixing of the organopolysiloxane and the water feeds during its passage through the SSM zone, and thereby supports a complete adsorption of the emulsifying agent to the surface of the organopolysiloxane drops dispersed in the water Example 3 Using the mixer 1_ shown in the Figure 1, 100 parts by weight of dimethylpolysiloxane with terminal trimethylsiloxy block, with a viscosity at 25 ° C of 300,000 mPa's (centipoise), 9.0 parts by weight of lauryl ether of polyoxyethylene, 3.4 parts by weight of cetyltrimethylammonium chloride, and 3.6 parts by weight of deionized water. The compressed air was also continuously injected through a gas supply gate connected to gate 2, to provide a ratio of 1.0 (NL / hour) / (kg / hour) between its feed and the siloxane feed. The cutting and stirring to homogeneity were conducted to produce an emulsion of dimethyl polysiloxane. With respect to the mixer used in this example, the rotational speed of the rotating shaft was 4,200 rpm; the minimum free space was 0.2 mm in the SSMs 9 and 10; the pressure in gate 2_ of initial material supply was 0.4 kg / cm2 G; and the discharge pressure of the emulsion in the discharge gate 3 ^ was 0.0 kg / cm2 G. The emulsion of dimethyl polysiloxane prepared according to the cutting and stirring process of this example, was a translucent emulsion in the form of paste, in which dimethylpolysiloxane was uniformly dispersed and emulsified in water. The average particle size of the dimethylpolysiloxane in the emulsion was measured at 0.3 microns. A second emulsion was also prepared by the addition of 71 parts by weight of water per 100 parts by weight of this emulsion in paste form. This second emulsion was maintained at room temperature for 6 months without occurrence of separation between dimethylpolysiloxane and water, which indicated that it was extremely stable.

Example 4 This example used two mixers as shown in Figure 1, which were connected in series. The following materials were continuously fed to gate 2_ of initial material supply, of the first mixer: 10 parts by weight of polyoxyethylene lauryl ether, 5.0 parts by weight of deionized water, and 100 parts by weight of a mixture having a viscosity at 25 ° C of 100,000 mm2 / s (centis-tokes) prepared by dissolving to the homogeneity of 42 parts by weight of rubber of dimethyl polysiloxane with terminal trimethylsiloxy block, with a viscosity at 25 ° C of 10'500,000 mm2 / s (centistokes) in 58 parts by weight of isoparaffin with a relative density of 0.79 and a viscosity at 40 ° C of 2.4 mm2 / s (centistokes) ). Compressed air was also injected continuously through a gas supply gate, connected to gate 2_ of material supply, to provide a ratio of 1.0 (NL / hour) (kg / hour) between its power supply and the power supply. dimethylpolysiloxane. These ingredients were mixed by cutting and stirring until homogeneous, and discharged as a translucent emulsion in paste form, with a dimethylpolysiloxane content of 36.5 weight percent, from the discharge gate 3_ of the first mixer. This emulsion in paste form and 82.4 parts by weight of water for dilution (eg, equivalent to 71 parts by weight per 100 parts by weight of emulsion in the form of paste, discharged from the first mixer) were then fed continuously to gate 2_ of initial material supply of a second mixer, where the cutting and stirring to homogeneity produced an emulsion of dimethylpolysiloxane gum with a dimethylpolysiloxane content of 21.3 weight percent. The conditions in the first and second mixers used in the process carried out in this example were the same as the conditions used in Example 1, for example, the rotational speed of the rotating shaft 4, the minimum clearance, the cutting speeds, and the pressures in supply gate 2 and discharge gate 3. The emulsion of dimethylpolysiloxane prepared by this cutting and stirring process was a white emulsion such as milk, in which the dimethyl polysiloxane gum was emulsified and dispersed to homogeneity in water. Its average particle size was 0.4 micrometers. Even though this emulsion of dimethylpolysiloxane was maintained for 10 months at room temperature, the dimethylpolysiloxane and water did not separate, indicating that the emulsion was extremely stable.

Comparative Example The dimethylpolysiloxane, emulsifying agent and water were mixed as described in Example 3, but in this comparative example without injection of compressed air. An emulsion was obtained in paste form.

The average particle size of the dimethylpolysiloxane in this emulsion was measured at 0.4 microns. In the case of the second emulsion prepared by the addition of 71 parts by weight of water per 100 parts by weight of the emulsion in paste form, the dimethylpolysiloxane and the water underwent separation after standing for only one day at room temperature. It should therefore be apparent, by comparing the present Example 3 with this Comparative Example, that where the emulsification is carried out while continuously injecting a gas into the starting material, it is produced according to this aspect of the present invention. invention, an organopolysiloxane emulsion which is highly homogeneous and very stable to storage.

It is noted that in relation to this date, the best method known to the applicant to carry out the aforementioned invention, is that which is clear from the present description of the invention.

Having described the invention as above, property is claimed as contained in the following:

Claims (9)

1. A method for the preparation of organopolysiloxane emulsions, characterized in that it comprises (A) as a first process: the continuous feeding and supply of a liquid or organopolysiloxane gum, water and an emulsifying agent as materials in the supply gate of a first mixer having a cylindrical housing or housing, the cylindrical housing has mounted thereon between its supply gate and discharge gate, a first stage cutting and stirring mechanism (SSM) and a second stage cutting and stirring mechanism, the first stage cutting and stirring mechanism comprising a turbine rotor having blades inclined obliquely from the radial direction, when viewed in the axial direction, and a stator around the circumference of the rotor, the cutting and agitating mechanism second stage comprises a turbine rotor having blades that describe spiral curves with respect to the direction axially, and a stator around the circumference of its rotor, the first and second stage mechanisms are arranged in series along the direction of flow of the feedstocks, and are separated from each other by an area of relaxation; the feeding materials in the first stage cutting and stirring mechanism are subjected to an admission and cutting action at a cutting speed of at least 100 / sec; and then the passage through the relaxation zone, holding the materials in the second stage cutting and stirring mechanism to the phase inversion, rotational effects and the cutting action, at a cutting speed of at least 100 / second; and discharging from the discharge port of the cylindrical envelope, an organopolysiloxane emulsion in water having an organopolysiloxane content in the emulsion of 10-99 weight percent, based on the total weight of the emulsion; and (B) as a second process: water is continuously fed and supplied for dilution and the organopolysiloxane emulsion in water, produced in the first mixer by the first process, to a second mixer, and repeating in the second mixer the steps carried out in the first process in the first mixer, and discharging from the discharge gate of the cylindrical shell of the second mixer, an organopolysiloxane emulsion in diluted water, in water.

2. A method according to claim 1, characterized in that the rear surface of the turbine rotor in the second stage cutting and stirring mechanism has sawtooth-shaped projections, the second stage cutting and stirring mechanism includes a space free or intervening vacuum, followed by sawtooth-shaped projections on a stator surface of the second stage cutting and stirring mechanism, the two sets of sawtooth-shaped projections on the surfaces of the rotor and the stator of the Second stage mechanism, they interlock or concatenate one with the other.

3. The method according to claim 1, characterized in that the liquid or organopolysiloxane gum has a viscosity at 25 ° C of at least 10,000 mm2 / second (centistokes).

4. A method according to claim 1, characterized in that the organopolysiloxane emulsion in water produced in the first mixer by the first process comprises from 10 to 99 weight percent of the organopolysiloxane fluid or gum, from 0.1 to 89. percent by weight of the emulsifying agent, and from 1.0 to 89 percent by weight of water.

5. A method according to claim 1, characterized in that the amount of dilution water fed and supplied in the second process is from 1 to 2,000 parts by weight per 100 parts by weight of the organopolysiloxane emulsion in water, produced in the first mixer through the first process.

6. A method according to claim 1, characterized in that there is a minimum clearance between the turbine rotors and the stators of the mechanisms, of between 1-2 mm.

7. A method according to claim 1, characterized in that a gas is injected into the supply gate of the first mixer.

8. A method according to claim 7, characterized in that the ratio of the amount of gas injected in NL / hour to the amount of organopolysiloxane liquid or gum delivered in kg / hour is 0.01 to 100 (NL / hour) / ( kg / hour).

9. A method according to claim 8, characterized in that the gas is selected from the group consisting of air, nitrogen, carbon dioxide, and argon.