• 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:
    The process for bleaching continuously prepared sodium hydrogensulfate which forms in a sodium hydrogensulfate melt flow reactor during the reaction of sodium chloride and concentrated sulfuric acid, the hydrochloric acid generated and the heating gases generated by an immersion burner being drawn off at different places and seed crystals being added for the rapid conversion of the metastable phases formed in a first step, consists of adding as seed crystals of 0.01 to 0.05% by weight of aluminum oxide and / or 0.5 to 1.5% by weight of magnesium and / or magnesium sulfate as well as in addition, where appropriate, of calcium sulfate.
    公开号:BE1019014A3
    申请号:E2004/0441
    申请日:2004-09-09
    公开日:2012-01-10
    发明作者:Klaus Driemel；Ingo Biertuempel；Kirsch Horst
    申请人:Grillo Werke Ag；
    IPC主号:
    专利说明:

    The object of the present invention is a process for bleaching continuously prepared sodium hydrogen sulphate which is formed in a circulating reactor in the sodium hydrogen sulphoxide melt during the production of sodium hydrogen sulphate. reaction of sodium chloride and concentrated sulfuric acid, the hydrochloric acid generated and the heating gases generated by an immersion burner being withdrawn at different locations and seed crystals being added for the rapid conversion of the metastable phases formed in first time.
    Such a process has been applied for many years in a Hoechst AG installation. The installation corresponds to DE-C-2810693. The process corresponds to Example 5 of DE-C-2619811. In practice, the sodium sulphate sodium melt flowing from the sulphate calcium reactor is thus added in amounts of up to 2.5% by weight.
    The product thus obtained has an impeccable quality and is also marketed in this quality for years. The preparation and marketing of this sodium hydrogen sulphate is carried out in the meantime by the applicant.
    In principle, this product can also be used in the food industry. The fact that this product has a touch of yellow, however, is considered embarrassing.
    Extensive analyzes of the applicant have shown that this yellow color is attributable to traces of ferrous salts of the order of 50 to 200 ppm.
    All attempts to eliminate this staining by the addition of oxidation means and reducing or complexing means have failed. The hue of the yellow color may be somewhat modified by such additions but this hue can not however be eliminated.
    Further in-depth analyzes have now come to the surprising result that according to the above-mentioned method, continuously prepared sodium hydrogen sulfate can be bleached when seed crystals of 0.01 to 0.05% are added as seed crystals. weight of aluminum oxide and / or 0.5 to 1.5% by weight of magnesium oxide and / or magnesium sulphate and, in addition, calcium sulphate, if appropriate.
    It is in fact mentioned in DE 26 19 811 that 0.1 to 5% by weight of magnesium sulphate can also be used as seed crystals. But it was apparently not observed at the time that with only 0.5 to 1.5% by weight of magnesium sulphate or by adding calcium sulphate, a product is formed which no longer has this color yellow junk.
    It has furthermore been found that similar results are obtained when seed crystals of 0.01 to 0.05% by weight of aluminum oxide and / or 0.5 to 1.5% are used. by weight of magnesium oxide. In these cases also, one can still, if necessary, use in addition to calcium sulfate.
    These results were initially quite surprising and can perhaps be explained a posteriori in that the seed crystals used in accordance with the invention are able to insert preferably in a crystalline lattice the impurities present only as traces with ferrous salts so that most of the prepared sodium hydrogen sulfate has a virtually colorless appearance. The calcium sulphate used so far on the technical scale is apparently not able to do this, but its presence does not disturb the bleaching according to the invention thanks to the aluminum oxide, the magnesium oxide or magnesium sulfate.
    The process according to the invention is explained in more detail in the examples which follow.
    Example 1 (state of the art),
    In a masonry circulation reactor which is heated directly by a submerged burner, 1770 liters of technical sulfuric acid (d = 1.84) and 1933 kg of refined salt in melted sodium hydrogen sulphate were introduced per hour. The temperature of the sodium hydrogen sulphate melt was maintained at 260 ° C by the combustion of 300 m3 / h of hydrogen and 1000 m3 / h of air in the submerged burner. To the melt withdrawn from the reactor to the pumping station of the spraying tower was added 1 kg of calcium sulphate after addition of 100 l / h of water. The sodium hydrogen sulphate which has been known hitherto is, however, colored yellow.
    Example 2 Instead of 1 kg of calcium sulfate, 1 kg of Al 2 O 3 (0.025% Al relative to NaHSO 4) was added. In the spraying tower, the melt is sprayed by air injection into drops which then solidify to substantially white beads. Example 3
    The procedure was as in Example 1, except that instead of 1 kg of calcium sulphate 20 kg of anhydrous magnesium sulphate (corresponding to 0.2% magnesium per compared to sodium hydrogen sulphate). Once again pearls were almost white.
    Example 4
    Example 3 was repeated, but the same amount of magnesium oxide was added instead of 20 kg of anhydrous magnesium sulfate. White pearls were again obtained.
    The products of Examples 2 to 4 meet the purity requirements for sodium hydrogen sulphate as an additive for foodstuffs. They are more acceptable to the consumer in the food industry because of the bleaching achieved.
    权利要求:
    Claims (2)
    [1]
    A process for bleaching continuously prepared sodium hydrogen sulphate which is formed in a circulating reactor in the sodium hydrogenosulfate melt during the reaction of sodium chloride and concentrated sulfuric acid, the acid generated hydrochloric acid and the heating gases generated by an immersion burner being withdrawn at different locations and seed crystals being added for the rapid conversion of the metastable phases formed in a first step, characterized in that it is added as crystals of inoculation of 0.01 to 0.05% by weight of aluminum oxide and / or 0.5 to 1.5% by weight of magnesium oxide and / or magnesium sulphate and, in addition, where appropriate, calcium sulphate.
    [2]
    2. Process according to claim 1, characterized in that 0.5 to 1.5% by weight of magnesium sulphate is added.
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    同族专利:
    公开号 | 公开日
    US7067094B2|2006-06-27|
    DE10341460A1|2005-04-07|
    DE10341460B4|2006-04-20|
    US20050089469A1|2005-04-28|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2893836A|1954-12-06|1959-07-07|Monsanto Chemicals|Process for producing substantially white sodium bisulfate|
    US2861868A|1956-10-18|1958-11-25|Monsanto Chemicals|Method of producing substantially white, globular sodium bisulfate|
    US3690825A|1970-10-30|1972-09-12|Du Pont|Process for the preparation of globular sodium bisulfate|
    DE2619811B1|1976-05-05|1977-09-15|Hoechst Ag|PROCESS FOR THE PRODUCTION OF SODIUM BISULFATE|
    DE2810693A1|1978-03-11|1979-09-13|Hoechst Ag|Continuous prodn. of sodium bi:sulphate - from sulphuric acid and sodium chloride with economical use of energy and reduced reactor corrosion|
    US1599996A|1926-09-14|Cleaning compound and process of preventing the deliquescence of a salt |
    US1104913A|1913-12-10|1914-07-28|Peter Loeffler|Process for the manufacture of sodium bisulfate in a directly-calcinable form.|
    GB110405A|1916-10-20|1917-10-22|Jacob Grossmann|Improvements in the Treatment of Nitre Cake.|
    US3919401A|1974-07-29|1975-11-11|Du Pont|Method of preventing formation of sodium-iron sulfate in the preparation of sodium bisulfate|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE10341460|2003-09-09|
    DE10341460A|DE10341460B4|2003-09-09|2003-09-09|Process for leaching sodium hydrogen sulfate|
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