• 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:
    57 Silica spheres are prepared in a process comprising: a) preparing a silica hydrosol by mixing an aqueous solution of an alkali metal silicate with an aqueous solution of an acid; b) converting the hydrosol into droplet form; c) ageing the droplets in a fluid to produce hydrogel particles; d) partially drying the hydrogel particles at 10 to 60 °C in air having a relative humidity in the range of from 45 to 95%, to a water content in the range of from 0.3 to 1.3 kg/kg solids; e) decreasing the cation content of the hydrogel particles by ion-exchange in an aqueous medium to less than 10 %w, calculated on dry material; and f) finally drying the hydrogel particles to obtain silica spheres.
    公开号:SU1577691A3
    申请号:SU853933054
    申请日:1985-08-01
    公开日:1990-07-07
    发明作者:Афгхан Маджид；Ирардус Спонселии Жозефус
    申请人:Шелл Интернэшнл Рисерч Маатсхаппий Б.В. (Фирма)；
    IPC主号:
    专利说明:

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    with
    The invention relates to methods for producing silica beads.
    The aim of the invention is to obtain silica with a narrow particle size distribution and pore volume.
    Example 1. A solution of liquid glass in water, containing 12 wt.% Silica and having a molar ratio of Na O / SiO of -0.3, is continuously stirred in a mixer with 1.2 n. an aqueous solution of sulfuric acid at a volume ratio of acid solution:: liquid glass solution 0.65. You get a hydrosol. A few seconds after being in the mixing chamber, the hydrosol is converted into a drop form, for which it is passed through a nozzle with a diameter of 5 mm. The drops are allowed to fall through a tube filled with paraffin oil at ambient temperature, during which time gelation takes place. The gel time is 5 s. To carry out this procedure, the apparatus described in European Patent No. 58441 is used. The hydrogel particles obtained are separated from the oil by precipitation and washed with water.
    Next, separate weights of the hydrogel are subjected to partial drying under the conditions specified in Table. 1, using blowing air having different humidity. In experiments 1 and 2, the hydrogel particles are partially dried with wet and dry air, respectively. In experiment 3, the hydrogel particles are first dried with relatively dry air and then at the second stage of drying with moist air. After incomplete drying, the size distribution of silica particles is determined by sieve analysis.
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    about with

    with
    From the experiments performed, it is recommended that a short period is required for drying with dry air at elevated temperature, but particles with a wide size distribution are obtained. When drying with moist air, excellent results are achieved with respect to particle size distribution, although drying takes considerable time. Sugaki time can be significantly reduced by first drying with dry air (10 minutes) and then wet (30 minutes), while, as follows from experiment 3, the results are superior to those achieved with dry air drying. .
    EXAMPLE 2 Hydrogel particles are prepared as in Example 1, but are dried according to the conditions given in Table 2. 2. After partial drying, the hydrogel particles are subjected to hydrothermal treatment, for which the particles are immersed in water and heated under their own pressure to 120 ° C.
    The resulting hydrogel particles are treated with 0.4 n. sulfuric acid solution to remove sodium ions to their content less than 0.2 wt.% calculated on the dry material. The particles are dried for 2 hours at 150 ° C and get silica beads, which are then calcined at 850 ° C for 45 minutes in air.
    The particle size distribution is determined after partial drying, and the pore volumes of the particles of the desired size after the final calcination, for which use the method of mercury porometry. It should be noted that after partial drying, the particle size does not actually change in the future.
    The results of the experiment are given in table. 3
    Thus, silica, prepared in the form of balls by the proposed method, has a narrow size distribution and pore volume (experiment 5). At the same time, when using dry air, as in the known method, the particle size distribution is much wider.
    When comparing the moisture content in the fractions and pore volumes of these fractions, it can be seen that the pore volume is substantially proportional to the humidity.
    The average crushing strength for all particles is quite high and is 40-50 N.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    A method for producing spherical silica, comprising mixing a solution of sodium silicate with sulfuric acid to form hydrosol, converting it into drops, aging drops in oil to produce a hydrogel, treating with an aqueous solution of acid to reduce the cation content to less than 0.2 wt.%, Drying and calcining at 850-UOO ° C, characterized in that, in order to narrow the distribution of silica particles by size and pore volume, after aging, the hydrogel particles are dried at 29-53 ° C with air with a relative humidity of 55-72% to their water content 0.33-0.62 kg / kg solids.
    Table 1
    Continuation of table 1
    类似技术:
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    US3716493A|1973-02-13|Process for making fine sized low density silica
    US2768145A|1956-10-23|Method of manufacturing silica alumina catalyst
    US3655580A|1972-04-11|Agglomerated silica bodies and method
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    US3146076A|1964-08-25|Preparing sorptive siliceous particles
    CN100469437C|2009-03-18|Process for preparing molecular sieve filter core for drying new refrigerant
    JPH0764543B2|1995-07-12|Spherical silica and its manufacturing method
    US3669624A|1972-06-13|Process for producing high average pore volume silica
    同族专利:
    公开号 | 公开日
    EP0170334A3|1987-04-22|
    DE3567845D1|1989-03-02|
    EP0170334B1|1989-01-25|
    JPH053412B2|1993-01-14|
    ZA855817B|1986-03-26|
    JPS6140810A|1986-02-27|
    EP0170334A2|1986-02-05|
    US4640807A|1987-02-03|
    CA1259473A|1989-09-19|
    GB8419708D0|1984-09-05|
    AU4569585A|1986-02-06|
    AU569168B2|1988-01-21|
    引用文献:
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    GB735146A|1953-06-09|1955-08-17|Ernest Baldwin Miller|Silica gel and method of making the same|
    DE1567805C3|1965-02-24|1974-07-25|Mobil Oil Corp., New York, N.Y. |Process for the production of silica gel beads of high density and resistance to abrasion|
    DE2103243C3|1971-01-25|1979-01-11|Basf Ag, 6700 Ludwigshafen|Process and device for the production of largely spherical, silica-containing hydrogels|
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    GB1525386A|1974-11-06|1978-09-20|Shell Int Research|Process for the preparation of globular silica particles|
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    US4872895A|1986-12-11|1989-10-10|American Telephone And Telegraph Company, At&T Bell Laboratories|Method for fabricating articles which include high silica glass bodies|
    JPH0699135B2|1989-02-20|1994-12-07|富士デヴィソン株式会社|Manufacturing method of spherical silica gel|
    BE1004675A3|1991-03-11|1993-01-12|Solvay|METHOD FOR OBTAINING PARTICLE microspheroidal HOMODISPERSES, microspheroidal SILICA PARTICLE SPECIFIC SURFACE HIGH, CATALYSTS SUPPORTED ON THESE PARTICLES AND METHOD FOR POLYMERIZATION OF ALPHA-OLEFINS IN THE PRESENCE OF THESE CATALYSTS.|
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    CA2087911C|1992-01-24|1999-06-29|Kiyoshi Abe|Spherical granules of porous silica or silicate, process for the production thereof, and applications thereof|
    US5312571A|1993-01-07|1994-05-17|Norton Company|Shaped bodies and the production thereof|
    US5571494A|1995-01-20|1996-11-05|J. M. Huber Corporation|Temperature-activated polysilicic acids|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB848419708A|GB8419708D0|1984-08-02|1984-08-02|Preparation of silica spheres|
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