Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
  • C01B15/04—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof
  • C01B15/043—Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof of alkali metals, alkaline earth metals or magnesium or beryllium or aluminium

Definitions

• the present invention relates to a process for producing agglomerates consisting of alkaline earth peroxide, in which primary alkaline earth peroxide particles are subjected to a compacting press agglomeration, and to the alkaline earth peroxide agglomerates obtainable by this process and alkaline earth peroxide granules obtainable therefrom.
• Alkaline earth metal peroxides essentially mean the products magnesium peroxide, calcium peroxide and barium peroxide and the zinc peroxide chemically related to the products listed.
• the production of these peroxides is known in the prior art.
• DE 29 18 137 and DE 196 50 686 describe the production of peroxides by spray drying the respective concentrated suspensions, which were obtained from the reaction of hydrogen peroxide with the corresponding oxides or hydroxides.
• alkaline earth peroxides are produced which correspond to a particle diameter of 1 -10 ⁇ m and thus have a high degree of fine particle size; Due to this high degree of fineness, the alkaline earth peroxides are very susceptible to dusting, which is associated with major disadvantages when the alkaline earth peroxides are processed in various applications.
• the object was therefore to produce a more or less low-dust alkaline earth oxide which, on the one hand, has the advantageous properties of the finely divided starting product in later applications, but on the other hand can also be adapted with regard to the chemical properties.
• the invention proposes a process for the production of alkaline earth peroxide agglomerates, which is characterized in that the finely divided alkaline earth peroxides prepared from known processes are used in the presence of compacting aids which have disintegrating or hydrophobic properties have, compressed by press agglomeration and optionally comminuted the alkaline earth peroxide thus obtained in the form of granules with the desired particle size.
• alkaline earth metal peroxides to which compacting aids have been added, are subjected to a pressing process and compressed under the action of the pressing pressure used for this purpose, with a simultaneous vacuum in the compression zone.
• Suitable additives can be added to the alkaline earth peroxides to be compressed with a view to later application.
• the compacting aid is used in an amount of 0.1 to 10% by weight, preferably 1 to 5% by weight (based on the finished product).
• compacting aids made from salts of long-chain fatty acids, preferably magnesium montanate, ie substances which have hydrophobic properties, are suitable.
• the compacted alkaline earth peroxides produced in these two ways can be used directly - whereby a significantly lower dust pollution is to be expected compared to the starting product - or as a slurry - whereby, due to the disintegration agents available, only a very low expenditure of energy is required for resuspending.
• the temperature range at which the press agglomeration process of the invention can be carried out preferably corresponds to the temperature range in which the alkaline earth metal peroxides used have high thermal stability and the process can be carried out without problems from a safety point of view.
• the press agglomeration of the very small alkaline earth peroxide particles are e.g. B. in an advantageous embodiment of the invention at temperatures between about 0 to 60 ° C, preferably 20 to 60 ° C.
• the process can be carried out without problems in this area with regard to the active oxygen content of the alkaline earth peroxide particles to be pressed; active oxygen losses that impair the product are not observed.
• the process is preferably carried out in a vacuum.
• the pressure is advantageously a maximum of 0.25 bar.
• the size of the pressing pressure to be used to achieve the advantages of the invention and the level of the negative pressure to be used can be freely selected within wide limits and can therefore be adapted to special wishes or requirements with regard to the product. According to the lower values, however, the pressing pressure is determined by two specifications: the minimum pressing pressure to be applied should be sufficient to give the agglomerate of the alkaline earth primary particles sufficient strength to avoid annoying dusting in the later application.
• the pressing pressure to be at least used to achieve the desired properties depends on the type of press machine used and can easily be determined by a person skilled in the art in a few preliminary tests with regard to the desired product properties.
• the upper limit of the pressing pressure to be applied is not critical and is only limited by the maximum technically achievable or permissible pressing pressure used in the press agglomeration.
• compression is carried out at pressures of 2.35 t per cm of roll length ( ⁇ 145 bar), with a (air) pressure of at most 0.25 bar being present in the compression zone of the press machine, that is to say working in a vacuum.
• the agglomerates produced according to the invention can be shaped products, such as. B. tablets or agglomerate, such. B. be granules that are less prone to caking or dusting in use and can therefore be metered well. Both the physical properties such as agglomerate shape or granule shape and size can be adapted according to the requirements as well as the application properties described above. The desired product properties determine the appropriate process.
• all conventional press agglomeration devices can be used for the method of the invention. Suitable press agglomeration devices are e.g. B. molding presses, punch presses or roller presses. Depending on the press agglomeration device used, the primary particles are under pressure, with simultaneous negative pressure in the compression zone in defined shapes, for. B. tablets or pressed into tight slugs. The slugs are crushed into granules of the desired size.
• alkaline earth peroxide granules according to the invention are distinguished by the fact that they can be metered well and are low in dust and, depending on the compacting aid, are very easily resuspendable or are difficult to resuspend in granule form due to the hydrophobic properties and thus have an extended oxygen release.
• the invention provides a simple method for producing dust-free alkaline earth peroxide granules.
• alkaline earth peroxides produced according to the teaching of DE 29 18 137 and DE 196 50 686 were mixed after admixing additives such as magnesium montanate (manufacturer: Clariant, D-86368 Gersthofen), Arbocell (type TF 0406, a fibrous cellulose, manufacturer: Fa. J. Rettenmaier and Sons, D-73494 Rosenberg) or sodium bicarbonate for press granulation in a lightly structured roller press.
• magnesium montanate manufactured by Clariant, D-86368 Gersthofen
• Arbocell type TF 0406, a fibrous cellulose, manufacturer: Fa. J. Rettenmaier and Sons, D-73494 Rosenberg
• sodium bicarbonate sodium bicarbonate for press granulation in a lightly structured roller press.
• the primary particles were added with a press pressure of 2 t / cm roll length (-130 bar) to 2.35 t / cm roll length (-145 bar) and a vacuum of 0.75 bar (ie at a pressure of 0.25 bar) pressed into flakes with a thickness of 1 mm and then adjusted to the target grain size with the aid of a crusher using granulating screens.
• abrasion index 70 g of sample were manually separated from fine fractions on a sieve. Then exactly 50 g were placed on the appropriate sieve (1.0 mm) for 3 min. shaken with the laboratory sieve machine JEL. The resulting fine fraction ⁇ 0.425 mm in [%] indicated the abrasion.
• IXPER® 75C is a product of Solvay Interox GmbH with at least 75% by weight calcium peroxide.
• IXPER® 35M is a product of Solvay Interox GmbH with at least 35% by weight magnesium peroxide.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• General Life Sciences & Earth Sciences (AREA)
• Geology (AREA)
• Inorganic Chemistry (AREA)
• Glanulating (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Press-Shaping Or Shaping Using Conveyers (AREA)

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• 2002
  • 2002-10-18 DE DE10248652A patent/DE10248652A1/de not_active Withdrawn
• 2003
  • 2003-09-24 CA CA2502652A patent/CA2502652C/en not_active Expired - Fee Related
  • 2003-09-24 JP JP2004544040A patent/JP4478575B2/ja not_active Expired - Fee Related
  • 2003-09-24 EP EP03788917A patent/EP1565401A2/de not_active Withdrawn
  • 2003-09-24 AU AU2003293317A patent/AU2003293317A1/en not_active Abandoned
  • 2003-09-24 BR BRPI0315321-5A patent/BR0315321B1/pt not_active IP Right Cessation
  • 2003-09-24 CN CNB03823565XA patent/CN1299972C/zh not_active Expired - Fee Related
  • 2003-09-24 WO PCT/EP2003/010618 patent/WO2004035470A2/de active Application Filing
• 2005
  • 2005-04-18 US US11/107,784 patent/US7488439B2/en not_active Expired - Fee Related
• 2006
  • 2006-02-17 HK HK06102090A patent/HK1081937A1/xx not_active IP Right Cessation

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