EP3292913A1 - Procede de forte reduction de la taille de materiau en granules - Google Patents

Procede de forte reduction de la taille de materiau en granules Download PDF

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Publication number
EP3292913A1
EP3292913A1 EP16188026.5A EP16188026A EP3292913A1 EP 3292913 A1 EP3292913 A1 EP 3292913A1 EP 16188026 A EP16188026 A EP 16188026A EP 3292913 A1 EP3292913 A1 EP 3292913A1
Authority
EP
European Patent Office
Prior art keywords
mixing vessel
high speed
rotor stator
granular material
stator mixer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP16188026.5A
Other languages
German (de)
English (en)
Other versions
EP3292913B1 (fr
Inventor
Maarten Hammink
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Polychimique Nv
Treatex NV
Ecochem International NV
Original Assignee
Polychimique Nv
Treatex NV
Ecochem International NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Polychimique Nv, Treatex NV, Ecochem International NV filed Critical Polychimique Nv
Priority to EP16188026.5A priority Critical patent/EP3292913B1/fr
Priority to PCT/EP2017/072597 priority patent/WO2018046669A1/fr
Publication of EP3292913A1 publication Critical patent/EP3292913A1/fr
Application granted granted Critical
Publication of EP3292913B1 publication Critical patent/EP3292913B1/fr
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C18/00—Disintegrating by knives or other cutting or tearing members which chop material into fragments
    • B02C18/06—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives
    • B02C18/08—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives within vertical containers
    • B02C18/083—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives within vertical containers with a disc rotor having generally radially extending slots or openings bordered with cutting knives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/06—Selection or use of additives to aid disintegrating

Definitions

  • the present invention relates to aqueous systems. More specifically the present invention relates to that can be safely manufactured while using equipment standard in the art of dispersion technology.
  • EP 2 586 849 discloses reducing the particle size of a granular mono-ammonium phosphate (MAP), by means of a method comprising the steps of:
  • the inline rotor stator mixer receives an input of a too much granule concentration and will block.
  • the rotor will aspire the granules and gets blocked because the distribution of the granules is not homogenous.
  • a combination of a rotor stator system inline or batch type
  • any type of high speed disperser having a disk preferably having tooth shapes at the edge of the disk, whether with a closed disk or an open disk, whether with 1, 2 or 3 levels or teeth
  • the process of the present invention is as defined in claim 1, i.e. a process for reducing the average particle size of a granular material by a factor of at least 20, said process comprising the steps of:
  • the process in accordance with the present invention may comprise the use of one or more thickeners, which may be of different types, e.g. thickeners that are able to swell in water during the initial stage of the process, and/or thickeners which are able to control and adjust the desired viscosity in the final stage of the process.
  • the process in accordance with the present invention may also comprise the use of one or more dispersing agents for aqueous systems.
  • rotor stator mixer refers to an equipment substantially as described in EP 2 586 849 .
  • high speed disperser having a mixing disk refers to a so-called high speed disperser (or dissolver) having a mixing disk, either closed or open, preferably having 1, 2 or 3 levels of tooth shapes at the edge of the disk. Examples of such, or funcionally equivalent, are available from various suppliers, including but without limitation:
  • the granular material may be mineral, e.g. selected from the group consisting of phosphates, sulfates (for instance aluminum sulfate), borates, hydrates (for instance aluminum hydrate), zeolites, hypophosphites, alkaline earth carbonates (for instance calcium carbonate), and alkaline earth oxides and hydroxides (for instance magnesium oxide, magnesium hydroxide).
  • the granular material may be organic such as, but not limited to, peroxydicarbonic acid, bis[4-(1,1-dimethylethyl)cyclohexyl] ester (commercially available under the trade name Perkadox® 16).
  • the rotor stator mixer (B) is either an internal batch-type rotor stator mixer (B1) or an inline rotor stator mixer (B2) externally connected to the mixing vessel (A).
  • the high speed disperser (A) is one of the type of a single shaft high speed disperser having a closed or open disk and having at least one set of teeth at the edge of said disk.
  • the liquid medium (or vehicle) provided to the mixing vessel may be selected from various chemical groups, especially from the group consisting of:
  • the process may further comprise the step of providing to the mixing vessel a first type thickening agent prior to, or simultaneously with, providing the liquid medium (or vehicle) to the mixing vessel.
  • the first type thickening agent is preferably one acting as a swelling agent in an aqueous system, and may be an organic material such as, but not limited to, xanthane gum or carboxymethylcellulose.
  • the type and useful amount of thickening/swelling agents may depend upon the granular material chemical and upon the solids content of the dispersion, but are well known to the person skilled in dispersion technology.
  • the process may further comprise the step of providing to the mixing vessel a dispersing agent such as an alkali neutralized acrylic polymer.
  • a dispersing agent such as an alkali neutralized acrylic polymer.
  • the type and useful amount of dispersing agents may depend upon the granular material chemical and upon the solids content of the dispersion, but are well known to the person skilled in dispersion technology.
  • the process may further comprise the step of providing to the mixing vessel a second type thickening agent after operation of the high speed dispenser (A) and/or during operation of the rotor stator mixer (B).
  • a second type thickening agent may be a mineral material such as, but not limited to, fumed silica or a phyllosilicate such as sepiolite (a complex magnesium silicate which can be found in fibrous or fine particulate solid forms from various commercial sources), or any other inorganic material capable to adjust the final viscosity of the dispersion to a predefined or desirable viscosity target.
  • the type and useful amount of such mineral thickening agents may depend upon the granular material chemical and upon the solids content of the dispersion, but are well known to the person skilled in dispersion technology.
  • the proper selection of the amount of thickener added at this step is also based on its capacity to afford the target final viscosity of the liquid (aqueous) aqueous system without negatively interfering with the other physical and chemical characteristics of the fine particles produced in the final stage.
  • an amount of thickener from 0.2% to 1% by weight, is well sufficient for meeting this requirement.
  • the liquid medium (or vehicle) provided to the mixing vessel may further include, dissolved or suspended therein, a grinding aid chemical.
  • the grinding aid chemical may be, but without limitation, selected from the group consisting of sand, silicate powder, phosphoric acid, sulfuric acid, nitric acid, and other weak or strong acids.
  • the medium (vehicle) may be brought back to normal by the addition of a suitable alkaline chemical, in a manner well known to the person skilled in the art. Consequently also, a salt may then be formed be formed by the acid, the partially dissolved granular/medium blend and the added alkaline chemical. This salt should be considered as a co-product, usually present in an amount limited to 1% - 5% mole/mole, and in such limited amount is normally not detrimental to the main product quality.
  • the process may thus be performed at a temperature between about 15°C and 50°C, for instance between about 20°C and 40°C.
  • the amount of granular material added to the mixing vessel may be such that the solid contents of the dispersion comprising the liquid medium and the granular material ranges between about 20% and 70% by weight, for instance between about 35% and 65% by weight, or between about 40% and 50% by weight.
  • the period of time of operating the high speed disperser (A) may range from about 5 to 60 minutes, preferably from about 10 to 30 minutes.
  • the period of time of operating the rotor stator mixer (B) may range from about 10 to 60 minutes, preferably from about 15 to 30 minutes.
  • Determination of the average particle size throughout the sequence of process steps can be made by the skilled person by reference to the current limits and precision of optical methods for determining the presence and size of particles present in a liquid medium (or vehicle), preferably an aqueous or water-based medium.
  • the standard reference in this respect is currently laser diffraction particle size analysis.
  • a laser diffraction particle size analyzer currently does not easily detect or quantifies with reasonable accurateness particles which are in aqueous solution, i.e. particles with a size below 0.1 ⁇ m. If need be, in particular for product quality control and regulations, the quantification of the amount of non-optically detectable particles present in the dispersed aqueous medium of the present invention can thus be carried out by indirect methods.
  • a suitable determination method includes the steps of:
  • the skilled person will readily select an appropriate dilution ratio X. It has thus been found that the above determination method can be carried out within a reasonable period of time (say not more than a few hours) by selecting a dilution ratio X ranging from about 5 to about 20.
  • Laser diffraction particle size analysis is herein given as a non limiting example of an easy-to-use method suitable for performing step (i) of the above determination method.
  • Gravimetric infrared moisture analysis is herein given as a non limiting example of an easy-to-use method suitable for determining the presence and amount of particles with a size below 0.1 ⁇ m within an aqueous liquid solution. Such a method may be performed for instance by using a precision weighing balance from the company Sartorius (Germany).
  • the process is performed, in contrast with the teaching of EP 2 586 849 , in the absence of a defoamer.
  • the present invention produces significant advantages over the traditional processes for finely comminuting granular materials.
  • the present invention produces significant advantages over the traditional processes for finely comminuting granular materials.
  • aluminium trihydrate_(ATH) with an average particle size of 5 microns is suitable to make stable dispersions with standard mixing equipment.
  • a 5 micron ATH grade can be 2-3 times more expensive than a coarse grade with average particle size above 50 microns. The latter particle size is too high to make stable dispersions with low viscosity by standard mixing equipment.
  • the 2 stage refining process of described herein is used with an acid grinding aid.
  • the process provides a mixing tank equipped with a high speed disperser having a mixing disk, and with a rotor atstor mixer.
  • the sequence of process steps is as follows:
  • Aluminium sulfate is available in the form granules, with a particle size ranging from 1 to 3 mm. It can be dissolved using hot water, but after cooling, crystallization will occur.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
EP16188026.5A 2016-09-09 2016-09-09 Procede de forte reduction de la taille de materiau en granules Active EP3292913B1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP16188026.5A EP3292913B1 (fr) 2016-09-09 2016-09-09 Procede de forte reduction de la taille de materiau en granules
PCT/EP2017/072597 WO2018046669A1 (fr) 2016-09-09 2017-09-08 Procédé pour réduire fortement la dimension de matériaux granulaires

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP16188026.5A EP3292913B1 (fr) 2016-09-09 2016-09-09 Procede de forte reduction de la taille de materiau en granules

Publications (2)

Publication Number Publication Date
EP3292913A1 true EP3292913A1 (fr) 2018-03-14
EP3292913B1 EP3292913B1 (fr) 2024-07-10

Family

ID=57103779

Family Applications (1)

Application Number Title Priority Date Filing Date
EP16188026.5A Active EP3292913B1 (fr) 2016-09-09 2016-09-09 Procede de forte reduction de la taille de materiau en granules

Country Status (2)

Country Link
EP (1) EP3292913B1 (fr)
WO (1) WO2018046669A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030215639A1 (en) * 2002-02-05 2003-11-20 Degussa Ag Aqueous dispersion containing cerium oxide-coated silicon powder, process for the production thereof and use thereof
US20090005589A1 (en) * 2007-06-27 2009-01-01 H R D Corporation System and process for production of toluene diisocyanate
US20120040168A1 (en) * 2007-02-12 2012-02-16 United States Gypsum Company Water resistant cementitious article and method for preparing same
EP2586849A2 (fr) 2011-10-28 2013-05-01 FR-Master bvba Systèmes aqueux de phosphate d'ammonium appropriés pour une utilisation en tant qu'additifs retardateurs de flamme

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030215639A1 (en) * 2002-02-05 2003-11-20 Degussa Ag Aqueous dispersion containing cerium oxide-coated silicon powder, process for the production thereof and use thereof
US20120040168A1 (en) * 2007-02-12 2012-02-16 United States Gypsum Company Water resistant cementitious article and method for preparing same
US20090005589A1 (en) * 2007-06-27 2009-01-01 H R D Corporation System and process for production of toluene diisocyanate
EP2586849A2 (fr) 2011-10-28 2013-05-01 FR-Master bvba Systèmes aqueux de phosphate d'ammonium appropriés pour une utilisation en tant qu'additifs retardateurs de flamme

Also Published As

Publication number Publication date
EP3292913B1 (fr) 2024-07-10
WO2018046669A1 (fr) 2018-03-15

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