• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    1, A method for producing microspheroid particles of magnesium dihalide adducts with electron donor compounds containing active hydrogen atoms by dispersing the molten starting material in an inert, immiscible liquid to form a mixture, adhering the microcapsule and forming an adduct microparticle, and forming a portion of the adduct microparticle and forming an adduct with a mixture that is not mixed with it, before the mixture is obtained, the microcapsule is hardened and the adduct is injected. , 4 g / cm 3 and a sphericity factor of 0.81, 0, and urea particles with a diameter of 1000-2000 µm, a fluidity of not more than 10 s and a bulk density of 0.85 g / cm, characterized in that. In order to intensify the process by uniformly distributing the starting material in an inert liquid, the mixture with a surface tension between the melt and an immiscible liquid of 10-100 dyn / cm is additionally emulsified in a turbulent flow at a rate of 0.2–20 m / s until an emulsion is obtained, followed by its quenching. 2. A method according to claim 1, characterized in that an adduct between magnesium dihalide and alcohol is used as the starting material, and a hydrocarbon liquid in an amount of 0.1-0.3 amounts of the starting material is used as the inert immiscible liquid. 3. The method according to claim 1, about tl and h ayu and with the fact that urea is used as a starting material, and hydrocarbon liquid with a surface tension between it and urea less than 30 dyne as an inert, immiscible liquid cm. 4. Method according to clause 1-3, characterized by the fact that quenching is carried out in an inert immiscible liquid. 00
    公开号:SU1111678A3
    申请号:SU792783747
    申请日:1979-06-12
    公开日:1984-08-30
    发明作者:Феррарис Марио；Розати Франческо
    申请人:Монтэдисон С.П.А.(Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a process for the preparation of products in spherical form, solid at room temperature, on the basis of these products in the molten state, mixed together with. at least another immiscible liquid that reacts in the mixture. The most common process used for curing in the form of granules or spheres is the process carried out by spraying molten products, known as spray cooling (or cooling spraying). The spraying of the molten product can be achieved by cooling with a cold gas stream circulating in the direction of spraying or in opposite directions. Through this technique, it is quite easy to obtain products in solid form and with a narrow particle size distribution at room temperature, starting from products that melt at temperatures greater than 250 ° C. Ci:; It is more difficult and more expensive to obtain solid spheroidal particles, the outcome from molten products that have a long crystallization time. This disadvantage leads to an increase in the length at which small droplets of the sprayed molten product should be covered with a cooling gas, which solidifies. In this case, the cooling spray columns must have a considerable height, which may even reach 80 m, and there is an additional danger of contaminating the environment and the atmosphere in the event that the outgoing gases are not washed or cleaned in order to remove the fine particles transported indicated exit psimi gases. The purpose of the invention is to intensify the process by uniformly distributing the starting material in an inert liquid. This goal is achieved by the fact that according to the method of obtaining micro spheroids, tal particles of the addurts of magnesium dihalide with electrophorescent compounds containing: active hydrogen atoms, by dispersing the molten starting material in an inert, immiscible with it liquid to form a mixture , curing microcapsules and obtaining particles of adducts with a diameter of 1-100 rtKM with a bulk density of 0.4 g / cm and a sphericity factor of 0.8-1.0 and urea particles with a diameter of 10002000 microns, fluidity not more than 10 s, and bulk density 0.85 g / cm, a mixture with a surface tension between the melt and an immiscible liquid equal to 10-100 dyne / cm is additionally emulsified in a turbulent flow at a speed of 0.2-20 m / s to obtain an emulsion, followed by quenching. An adduct between magnesium dihalide and alcohol is used as the starting material, and a hydrocarbon liquid in an amount of 0.1-0.3 quantities of the starting material is used as the inert immiscible liquid. Urea is used as a starting material, and a hydrocarbon liquid with a surface tension between it and urea of at least 30 dyne / cm is used as an inert, immiscible liquid. The quenching is carried out in an inert, immiscible liquid. The proposed method serves to obtain solid products in spherical form, having a maximum diameter of between 1 and 5 thousand microns, based on a mixture of at least two immiscible liquids, one of which is in the form of a solid melt, and these liquids are inert relative to each other and are present in such a way that one forms a dispersed phase, and the other a continuous phase. Of these two fluids, at least one that forms the dispersed phase is cured by cooling. The liquid forming the dispersed phase is present in a ratio ranging between 0.5 and 50% vs relative to the dispersing liquid. The process is carried out in the formation of an emulsion between the immiscible liquid phases by passing the mixture through a pipe of appropriate length and internal diameter under turbulent flow conditions. 3 Under the turbulent flow, the movement of a fluid in a cylindrical tube with a Reynolds number greater than 3000 is considered. At the outlet of the tube the emulsion is quenched so that an immediate change in the dispersed phase is formed. Quenching is achieved by mixing with a liquid that is inert and does not dissolve the dispersed phase, maintained at a suitable temperature, and cooling is carried out either in the line extending the tube or in a stirred volume. Such fluid may be similar to that used with as a continuous phase. The length of the pipe in which the emulsion is formed must be 50100 times longer than the internal diameter of the pipe. The output power of the process for producing spheroidal particles, which are formed from an emulsion, does not depend on the maximum diameter, which is independent of this. At any rate, the internal diameter of the pipe must be at least 3-4 times larger than the maximum diameter of the spheroidal particles that must be obtained. Under production conditions, the maximum diameter of the spheroidal particles to be obtained is a function of the linear velocity of the emulsion during flow through the pipe, interfacial tension that occurs between liquids, the density and viscosity of the dispersed medium and the viscosity of the dispersed phase. Among these functions, the most important variables, however, are linear velocity and interfacial tension. With an equal inner tube diameter at which the emulsion is formed, and with an equal interfacial tension, with an increase in the linear velocity, the maximum diameter of solid particles obtained in spheroidal form decreases. While a constant linear velocity is maintained in a pipe having the same diameter, the maximum particle diameter decreases with decreasing interfacial tension. Only for simplicity and in order to achieve the formation of particles with a maximum diameter of less than 784 50 microns, it is necessary to operate with linear velocities ranging between 2 and 20 m / s with fluids having an interfacial tension between 100 and 10 dyn / cm In this case, the dispersed and continuous phases are present in weight ratios of 0.1-0.3. In order to achieve particles with a maximum diameter greater than 1000 µm, it is necessary to operate at lower linear velocities, generally between 0.2 and 2 m / s, and using fluids with interfacial tension greater than 30 dyn / cm Operating under these conditions, it is possible to obtain products with a narrow particle size distribution, in which the maximum diameter can be adjusted and maintained below a predetermined value. These products are formed in the form of individual spherical particles having a sphericity factor of about 1 but generally between 0.8 and 1. A high coefficient (The sphericity of the particles gives them considerable fluidity and high bulk density. By the term sphericity is meant the ratio between surface area a sphere having the same volume as the particles and the external surface area of the particles determined experimentally. The proposed method is applicable to organic or inorganic compounds, have melting points in the range of 20400 s, such as, for example, urea, thermoplastic polymer products, waxes, organic or inorganic salt adducts. More specifically, the process is applicable to the preparation of microspheres of adducts between magnesium halides, especially magnesium chloride, and alcohols or water, and in general electron-containing compounds containing active hydrogen atoms, used as carriers for catalysts. The preparation of catalysts based on these microspheroidal particles is carried out, for example, in accordance with the method described in UK patent No. 1485234. Moreover, the process is suitable for the preparation of urea in spheroidal form. When the dispersed medium is used at high temperatures (e.g., 300 ° C), it can also use substances that are solid at room; temperature In this case, it receives a dispersion of the dispersed phase in the form of a solid spheroidal part ,. connected in a similar tzerduto continuous phase. Dispersing liquids can be generally aliphatic, aromatic, cycloparaffinic hydrocarbons, water, silicone oil (methylpolisis-poxane), organic phthalate-type ethers, liquid polymers. Example 1.48 g of anhydrous magnesium dichloride, 77 g of anhydrous ethyl alcohol and 830 ml of kerosene are loaded in an inert gas atmosphere and at room temperature into a two-liter autoclave equipped with a turbine agitator and a carrier tube. The mixture is then heated until stirred. Formed a, pnc between magnesium chloride and alcohol. The specified adduct is then melted and left mixed with a dispersing liquid. Inside the autoclave, maintain a nitrogen pressure of 15 kg / cm. The pipe of the autoclave is connected through the edges to a pipe heated by external heating to 120 ° C and having an internal diameter of 1 mm and a length of 3 m. The shut off valve is open to allow the mixture to flow along the pipe. The linear flow rate is set at about 7 m / s. At the outlet of the pipe, the dispersion is collected in a 5-liter flask5 equipped with a stirrer and containing 2.5 liters of kerosene. The flask is cooled from the outside and maintained at the initial temperature - The final temperature after collecting the outgoing emulsion the autoclave is a spheroidal solid product, which is formed from the dispersed phase of the emulsion, separated by decantation and filtration, washed with heptane and dried. All these operations are carried out in an inert gas atmosphere. 130 g of MgCl.sub.- are obtained, containing about 20% of a solvent and in the form of solid spheroid particles having a maximum diameter of less than 50 μm and a basic weight diameter of 19 microns. Solid gfoduktz dried under vacuum for 2 4. weighs 105 g. Bulk density of the product is Odz3 g / cm. Example 2 Conducted under conditions of npPiMepa 1 ,, with the difference that petroleum jelly is used as dispersed liquid. FU, and a linear flow rate of the mixture in the pipe is set at 4.5 m / s at an autoclave pressure of 10 g / cm. Anhydrous heptane is used as a quenching fluid. 130 g of solid spherical product MgCIaZS IeON5 containing about 17% solvent make it easier, which corresponds to 108 g of product dried under vacuum for 2 hours. The product has the following characteristics: Maximum diameter 50 μm Bulk weight 21 μm Bulk density 0.64 g / cm - Example 3, is carried out in the conditions of unit 2 except for the fact that the autoclave is loaded: 116 g of ethyl alcohol: 77 g, and the temperature is maintained. About 164 g of MgC 12 5C2Hj40H5 product containing about 18% solvent are obtained. This product, dried under vacuum for 2 hours, weighs 135 g :. He was a spherically solid particles having the following characteristics: Max y; pl15; diameter 50 mgsm; Osnswiy weight diameter: 7 microns; Volume density: 0., 62 g / cm; and p and measure 4 a. Under conditions of example 2, except that 130 g of solid magnesium chloride hexahydrate are loaded into the autoclave at room temperature and 830 cm of the FU vaseic mask. Then everything is heated to 140C. . About 130 g of the spherical MgCl2 product containing 12% solvent are obtained, which corresponds to 114 g of the cjxoro product of the 5th following gallant. Characteristics: Maximum diameter 50 microns Main weight di-meter 15 microns Bulk density 0547 g / cm
    71111678
    Example 5. It is carried out in the conditions of example 1. except that technical urea is used as the dispersed base, the internal diameter of the pipe is taken as 5 mm in size and dodecane is used as the dispersing medium.
    135 g of solid urea are loaded into the autoclave at room temperature. The autoclave, heated to 134 ° C, is pressurized with an inert gas of 2 kg / cm. A linear flow rate of the mixture in the pipe is set at 2.2 m / s.
    About 135 g of spheroidal solid urea containing about 15% of solvent was obtained, which corresponds to 115 g of dry product, Hivie following particle size distribution (ASTM D-1921/63). µmW.%
    100-15078.9
    75-10014.6
    50-75-4.4
    30-502.1
    Bulk density 0,865 fluidity of about 8 s (ASTM I-1895/69, method A).
    Example 6. It is carried out similarly to Example 5, except that a linear flow rate of 0.3 m / s is used.
    An analysis of the particle size of the spherical product gave the following results:
    wt.% 29.2 31.8 34.0 5.0
    from
    0.85 9 s
    J Example 7. Carried out under the conditions of Example 1, except that the dispersed phase contains polypropylene with a basic molecular weight of 1500, while the continuous phase is a mixture of ethylene glycol and water, in an amount of 50 wt.% 5 and internal pipe diameter is 3 mm.
    75 g of solid polypropylene are then loaded into the autoclave at room temperature in a gravitational relation to the continuous phase. Then everything is heated to t25C with stirring for 1 hour, after which the mixture is discharged through a pipe under a nitrogen pressure of 2 kg / cm. The product is collected in a flask equipped with a stirrer and containing a mixture of 50% ethylene glycol and water cooled to -20 ° C. The solid spheroidal polymer is then separated and dried. Thus, approximately 70 g of polymer in spheroidal form with a maximum particle diameter of lower 500 is obtained. um
    权利要求:
    Claims (4)
    [1]
    1. METHOD FOR PRODUCING MICROSPHEROIDAL PARTICLES of adducts of magnesium dihalo with electron-donating compounds containing active hydrogen atoms by dispersing the molten starting material in an inert immiscible liquid to obtain a mixture, curing microcapsules and obtaining adduct particles with a diameter of 1-100 microns with a volume of 1 to 100 microns in volume at a volume of 4 g / cm 3 and a sphericity coefficient of 0.8-
    1.0 and urea particles with a diameter of 1000-2000 μm, a fluidity of not more than 10 s and a bulk density of 0.85 g / cm 3 , characterized in that, in order to intensify the process due to the uniform distribution of the starting material in an inert liquid, the mixture with a surface tension between the melt and immiscible liquid of 10-100 dyne / cm, additionally emulsify in a turbulent flow with a speed of 0.2-20 m / s to obtain an emulsion with its subsequent hardening.
    [2]
    2. The method according to p. ^ Characterized in that the adduct between the magnesium dihaloide and alcohol is used as the starting material, and a hydrocarbon liquid in an amount of 0.1-0.3 of the amount of the starting material is used as an inert immiscible liquid.
    [3]
    3. The method according to p. Characterized in that urea is used as a starting material, and a hydrocarbon liquid with a surface tension between it and urea of at least 30 dyne / cm is used as an inert immiscible liquid.
    [4]
    4. The method according to PP. 1-3, characterized in that the hardening is carried out in an inert immiscible liquid.
    4 w
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    同族专利:
    公开号 | 公开日
    ZA792937B|1980-06-25|
    AU530494B2|1983-07-21|
    NO791967L|1979-12-14|
    JPS5518294A|1980-02-08|
    IN151519B|1983-05-14|
    PT69758A|1979-07-01|
    MX152552A|1985-08-23|
    DK150784C|1988-01-11|
    DK150784B|1987-06-22|
    US4469648A|1984-09-04|
    FR2428464B1|1983-05-06|
    FI67788C|1985-06-10|
    NO148283C|1983-09-14|
    GB2056987A|1981-03-25|
    BE876920A|1979-12-12|
    CH641686A5|1984-03-15|
    FI67788B|1985-02-28|
    DE2924029C2|1987-06-25|
    NO148283B|1983-06-06|
    SE437476B|1985-03-04|
    CA1130518A|1982-08-31|
    FI791840A|1979-12-14|
    DK239779A|1979-12-14|
    GB2024215B|1982-10-27|
    ATA416379A|1981-05-15|
    IT1096661B|1985-08-26|
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    AR220395A1|1980-10-31|
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    AT365096B|1981-12-10|
    BR7903724A|1980-02-05|
    FR2428464A1|1980-01-11|
    NL191381B|1995-02-01|
    GR72467B|1983-11-10|
    NL191381C|1995-07-03|
    PH18077A|1985-03-18|
    DE2924029A1|1979-12-20|
    IT7824509D0|1978-06-13|
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    申请号 | 申请日 | 专利标题
    IT24509/78A|IT1096661B|1978-06-13|1978-06-13|PROCEDURE FOR THE PREPARATION OF SOLID SPHEROIDAL PRODUCTS AT AMBIENT TEMPERATURE|
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