Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/128—Aluminium silicates, e.g. zeolites
  • C11D3/1286—Stabilised aqueous aluminosilicate suspensions
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/20—Silicates
  • C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates

Definitions

• the invention relates to a process for the removal of coarse particles in aqueous Alumos i 1 katsuspens i ons, which contain finely divided water-soluble Alumos i I kates with cations exchanging for calcium, by wet grinding.
• the present invention relates to a wet grinding process in continuous ball mills, which enables the crobante parts over 50 ⁇ m in Alumos i I, which are harmful to the specific application as detergent constituents, even in very low concentrations i katsuspens i onen to shred practically completely while maintaining the rest of the grain spectrum.
• the grit content is usually determined by a standardized wet sieving method.
• the prior art strives for grit contents of less than 0.05%, which, however, cannot always be complied with due to the synthesis.
• Small portions of Grit which are normally present in aluminum suspensions, usually remain undetected even with the help of modern grain analyzes.
• the use of low-grit zeolite in detergents also results in a tendency to deteriorate washing results. A reliable determination of such a disturbing oversize can be carried out with the stool device according to DIN 53 580.
• the principle of the grit determination with the stool device is the wet sieving of samples on a standard sieve sprayed with rotating nozzles.
• the fine parts are rinsed through the test sieve, while the coarse parts remain on the test sieve and are weighed out after drying.
• Grit values that are too high lead to deteriorated residue values on textiles washed with them.
• One way of reducing the excessively high grit values is to screen, grind the sieve residue and partially mix it back.
• Such processes are extremely complex, especially with a throughput of the order of 100,000 tons per year. Immediate grinding does not appear to be very promising for the average person skilled in the art, since experience has shown that, in the case of large throughput quantities, relative to the absolutely low content. Oversize also a lot of so-called "good grain", which has the desired grain size distribution, would be crushed.
• the aluminum silicates to be used here with cations which are capable of exchanging calcium ions are from DE-A 24 12 836 and in DE-A 2-4 12 838 known as phosphate substitutes in washing and cleaning agents.
• DE-A 24 12 837 states that one can grind AIumos i I i kate in the coarser state to the desired grain size.
• mills and / or air classifiers are suitable.
• the aiumosilicate residue is ground in a ball mill and separated into two fractions in a centrifugal separator, the finer of which does not contain any parts above 10 ⁇ m.
• DE-A 27 40 784 also relates to the production of Alumos i 1 i katen and in particular the production of Zeol ith A.
• the present one Can grind product to the desired grain size.
• certain particles can be obtained by grinding and reference is made to DE-A 12 18 415. Even if grain size distributions are specified in DE-A 27 44 784, no reference to the removal of oversize particles can be found in this document.
• DE-A 12 18 514 describes the fine grinding of crystalline zeolite in detail. This is a fine grinding down to average particle sizes below 3 ⁇ m, which requires a correspondingly long grinding time.
• EP-B 16 344 is a method for the production of alumos i 1 i katsuspens i onen, the storage stable, pumpable and are flowable, without the need for dispersants and stabilizers, by wet grinding of the aluminosilicates.
• Conventional apparatus such as ball mills, agitator mills or rotor mills are recommended for wet grinding, with particle sizes of on average 1 to 10 ⁇ m.
• DE-A 26 15 689 describes pourable, pumpable and storable suspensions with a content of at least 30% of aluminum silicate, as well as additional dispersing agents and stabilizing agents.
• the aluminum particles of the suspension can essentially have a particle size of between 1 and 30 ⁇ m.
• the object of the present invention is to practically completely reduce the proportion of so-called "oversize" of an alumosilicate suspension.
• the invention thus relates to a process for the removal of coarse particles in aqueous aluminum silicate ions which, based on the suspension, contain 20 to 60% by weight of finely divided water-insoluble aluminum silicates with cations which can be exchanged for calcium, and also dispersants and / or stabilizing agents, by wet grinding of the aluminum silicates, characterized in that the aluminum silicate suspension is passed through agitator ball mills to be operated continuously and in the course of less than
• the continuously operated agitator ball mills are commercially available vertically and / or horizontally working agitator ball mills that contain up to 90% of their volume with small diameter balls, in particular 0.5 to 3 mm made of glass, ceramics, corundum and others hard material or steel are filled. Particularly preferred in the sense of the present invention is a diameter of the balls of the agitator ball in the range of 2 to 3 mm.
• the rapidly rotating stirrer shaft with several attached stirrer disks brings the ball mass into motion.
• the grinding process takes place between the moving balls when pumping through the suspension.
• An essential characteristic of the present invention is therefore the extraordinarily high product throughput, which is set at the upper limit of the throughput capacity of the agitator ball mill.
• a single grit grain consists of an agglomerate of several thousand single crystals of 1 to 2 ⁇ m each.
• the cohesion of the individual criteria is so strong that the usual operations in manufacture, processing and application do not affect it.
• the aluminum is suspended to a grain size with a fraction of 0.01% with a grain size of 50 ⁇ m or more and 0.1% with a grain size of 25 ⁇ m or more.
• a further embodiment of the present invention consists in that the dwell time in the agitator ball is reduced to such an extent that a dwell time in the agitator ball mill of 10 to 20 seconds is particularly preferred.
• Alumosilicate suspensions to be used according to the invention contain dispersing agents and / or stabilizing aids in all embodiments of the present invention.
• Such dispersants and stabilizers are described in DE-A 26 15 698 and can essentially be selected from the following compounds:
• Stabilization I Not visible, organic or inorganic, water-soluble salts with a molecular weight below 1,000, free of additional phosphonic acids and organically bound phosphate groups.
• these are contained in the aluminum silicate suspensions in an amount of 0.2 to 7% by weight.
• REPLACEMENT LEAF The product flowing out of the mill is foam-free and has no detectable grit content on the 50 ⁇ m sieve.
• the grain size distribution between 1 and 20 ⁇ m changes only slightly through the mill passage, as can be seen from the following list.
• Zeolite A suspensions 48%, from production, served as the starting material for Example 2 and Comparative Examples 1 to 4.
• the Zeolite A suspension had the particle size range and the grit shown in the table - upgrade.
• the grain spectrum described in the table was achieved in an agitator sphere Imüh1 e according to Example 1, which was operated with a dwell time of 15 seconds in the initial concentration.
• Example 1 of EP-PS 16 344 in a laboratory mill, corresponding to PE 075 - volume 0.75_I, degree of filling 55% grinding media, grinding media glass 1 mm, 20 min
• Comparative example 2 represents a repetition of measures of comparative example 1.
• the grain analysis and grit values can be found in the table.
• Comparative example 3 was carried out in accordance with EP-PS 16 344, example 2, a 30% suspension being used.
• the table shows the grain analyzes and grit values obtained.
• the comparison example 4 describes' the repetition of the method equal to Example 3.
• the particle analysis obtained and Grit-Wer ⁇ te le are shown in the Tabel.
• grain size For example grain size
• the MahI results There are no significant differences to be registered in the MahI results, but the Mah I services are significantly improved when the method according to the invention is applied. Taking into account the effective dwell time and the performance-determining concentration, the performance according to the procedure according to the invention is almost 100 times that of Comparative Example 1 and almost 130 times that of Comparative Example 3.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Life Sciences & Earth Sciences (AREA)
• Wood Science & Technology (AREA)
• Silicates, Zeolites, And Molecular Sieves (AREA)
• Crushing And Grinding (AREA)
• Detergent Compositions (AREA)
• Soil Conditioners And Soil-Stabilizing Materials (AREA)
• Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

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• 1988
  • 1988-08-11 DE DE3827260A patent/DE3827260A1/de not_active Withdrawn
• 1989
  • 1989-08-03 ES ES89114340T patent/ES2053881T3/es not_active Expired - Lifetime
  • 1989-08-03 EP EP89114340A patent/EP0354473B1/de not_active Expired - Lifetime
  • 1989-08-03 JP JP1508461A patent/JPH04500060A/ja active Pending
  • 1989-08-03 WO PCT/EP1989/000918 patent/WO1990001458A1/de not_active Application Discontinuation
  • 1989-08-03 EP EP89908977A patent/EP0428576A1/de active Pending
  • 1989-08-03 DE DE8989114340T patent/DE58903437D1/de not_active Expired - Fee Related
  • 1989-08-03 KR KR1019900700678A patent/KR900701655A/ko not_active Application Discontinuation
  • 1989-08-09 YU YU157689A patent/YU46709B/sh unknown
  • 1989-08-09 DD DD89331618A patent/DD283983A5/de not_active IP Right Cessation

Non-Patent Citations (1)

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