EP0956335A1 - Silices agglomerees - Google Patents

Silices agglomerees

Info

Publication number
EP0956335A1
EP0956335A1 EP97945973A EP97945973A EP0956335A1 EP 0956335 A1 EP0956335 A1 EP 0956335A1 EP 97945973 A EP97945973 A EP 97945973A EP 97945973 A EP97945973 A EP 97945973A EP 0956335 A1 EP0956335 A1 EP 0956335A1
Authority
EP
European Patent Office
Prior art keywords
weight
granular composition
particle size
less
micron
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.)
Withdrawn
Application number
EP97945973A
Other languages
German (de)
English (en)
Inventor
Ian Patrick Mckeown
Michael Thomas Gleaves
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.)
Ineos Silicas Ltd
Original Assignee
Joseph Crosfield and Sons Ltd
Crosfield Ltd
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 Joseph Crosfield and Sons Ltd, Crosfield Ltd filed Critical Joseph Crosfield and Sons Ltd
Publication of EP0956335A1 publication Critical patent/EP0956335A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • C12H1/0408—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of inorganic added material

Definitions

  • Alcoholic fermented beverages for example beers, have a tendency to produce haze which can be of biological or physico-chemical origin, and a number of products and processes are used for the removal of haze-forming constituents Whilst gross haze effects are resolved by filtration, flocculation, or centnfugation, secondary haze develops during storage due to interactions between certain polypeptides and polyphenols which coagulate and precipitate This haze therefore becomes apparent only at a stage when the beverage is being prepared for consumption and when removal is impractical
  • a number of organic and inorganic substances can be used to remove the polypeptide and polyphenol haze precursors prior to packaging and so stabilise the beverage, such as tannic acid, polyvinylpolypyrrohdone, bentonite, active carbon and silicas
  • Amorphous silica hydrogels are non-dusty, easy to handle powders
  • amorphous silica xerogels, while being effective beer stabilisers, are extremely dusty and pose difficult handling problems
  • the present invention is aimed at delivering low dusting, highly stabilising silica gels for use in stabilising beverages
  • the invention is directed to the treatment of beers, which term includes lager, Pilsner, Dortmund and Minato beer, as well as top fermented beers such as ale, porter and stout, it is applicable to other fermented liquids which are liable to generate haze on storage, as well as to non-fermented beverages that may form haze during storage, such as fruit juices and
  • the agglomerates, and their component particles, of the invention are defined in terms of their physico-chemical properties
  • the test methods used to determine these properties are - i) Surface Area and Pore Volume
  • the total moisture content was determined from the loss in weight of a silica when ignited in a furnace at 1000°C to constant weight iv) Weight Mean Particle Size
  • the weight mean particle size of the silicas before agglomeration was determined using a Malvern Mastersizer Model X, made by Malvern Instruments, Malvern, Worcestershire with MS15 sample presentation unit This instrument uses the principle of Fraunhoffer diffraction, utilising a low power He/Ne laser
  • the particulates are dispersed ultrasonically in water for 7 minutes to form an aqueous suspension and then mechanically stirred before they are subjected to the measurement procedure outlined in the instruction manual for the instrument, utilising a suitable lens in the system
  • the Malvern Particle Sizer measures the weight particle size of the particulate
  • the weight mean particle size (d50) or 50 percentile, the 10 percentile (d 10) and the 90 percentile (d90) are easily obtained from the date generated v) Beer Stabilisation
  • the proteins in beer which precipitate in the presence of tannic acid are considered to be important polypeptide haze precursors
  • the sensitive protein content of degassed beer was determined using a Tannometer supplied by Bearwell International Systems, 125 St Mary's Road, Market Harborough, Leicestershire, LE16 DT, England Measurement was made at 25°C using a 0 01 % w/v tannic acid solution (Brewtan
  • the Microson XL2020 Sonicator ultrasonic processor has a maximum of 550 watts output with a 20kHz convertor and is fitted with a % inch tapped horn
  • the processor has variable amplitude control and a microprocessor controlled digital timer integrated with a Pulsar cycle timer with power output and elapsed time displays
  • the piezoelectric convertor transforms electrical energy to mechanical energy at a frequency of 20KHz Oscillation of piezoelectric crystals is transmitted and focused by a titanium disruptor horn that radiates energy into the liquid being treated
  • the generator provides high voltage pulses of
  • the % inch probe is a medium intensity horn for processing volumes between 25 and 500ml
  • the maximum amplitude at the tip of the probe is 60 microns
  • sonicator processors operating at output control setting 10 have 60 microns of amplitude (peak to peak amplitude of the radiating face of the tip) at the tip of the probe Therefore, there is a linear relationship between the output control knob (or amplitude adjustment knob) and the amplitude at the tip of the probe, i e 6 microns of amplitude per control knob setting
  • a 250ml Pyrex beaker is insulated and fitted with a lid with a 3/4 inch hole in the centre to accommodate the ultrasonic probe and a 1 /8 inch hole to the side to accommodate a temperature probe
  • Into the insulated beaker weigh the desired amount of deionised water, and the desired amount of inorganic granule to obtain a final weight of 200 g
  • a magnetic stirrer bar is introduced into the beaker and the beaker is placed on a magnetic stirrer hotplate equipped with a temperature sensor (Heidolph MR3003 magnetic stirrer hotplate with a stainless steel PT-100 temperature sensor and rpm stirrer speed, obtainable from Orme Scientific, Manchester)
  • the beaker contents are stirred on setting 3 (-300 rpm), the ultrasonic probe is immersed to a depth of 5/8 inch into the liquid and the temperature sensor is inserted into the liquid to continuously monitor temperature
  • the Sonicator ultrasonic processor is switched on and information on processing time and pulsed mode programmed, as
  • the inorganic particle dispersion is poured through a 45 micron sieve Any residue in the beaker is washed through the sieve, using half the amount of initial water The sieve is then dried to constant weight in an oven at 150°C The residue which remains on top of the 45 micron sieve is then weighed and expressed as a percentage of the initial weight of inorganic granule The greater the amount retained on the sieve, the stronger the agglomerate strength of the granule and the more difficult it is to breakdown An optimum product will have no residue remaining on the sieve
  • 100g of the sample is placed on the top sieve of a series of BS sieves, at approximately 50 micron intervals to cover the particle size range of the granule
  • the sieves are arranged in order with the finest at the bottom and the coarsest at the top of the stack
  • the sieves are placed in a mechanical vibrator e g Inclyno Mechanical Sieve Shaker by Pascall Engineering Co Ltd , covered with a lid and shaken for 10 minutes
  • % residue Wt Of residue * 100
  • a process for the treatment of a fermented alcoholic beverage which comprises contacting the beverage with a granular composition comprising 45 to 98 % w/w on dry basis of a water insoluble particulate wherein more than 75% by weight on dry basis, preferably more than 90% by weight on dry basis, of the water insoluble particulate is made from an amorphous silica, having a weight mean particle size of from 5 to 30 microns, preferably from 10 to 30 microns, a pore volume of more than 1 cc/g, and a mean pore diameter of more than 60 Angstroms, the granular composition having a particle size, as measured by dry sieve analysis, such that more than 75% by weight of the granular composition, preferably more than 95% by weight, has a particle size of more than 45 microns
  • the granular composition is sieved at 125 and 600 microns so that more than 90% w/w of the granular composition has a parcile size between 125 and 600 microns
  • the granular composition has a granular strength such that less than 5%, more preferably less than 2%, most preferably less than 1 % by weight, residue is left on a 45 micron wet sieve after ultrasonification on setting 10 (60 micron amplitide) for a period of 7 minutes
  • the granular composition has a total moisture content of less than 40%, preferably less than 30%, more preferably less than 20%
  • Amorphous silicas which can be used in the present invention may be prepared via an acid gel route or an alkaline precipitate route Specific Description of the Invention
  • Silica gels having the properties shown in Table 1 were agglomerated individually at 200g powder batch size (laboratory scale) with deionised water using a Sirmon CV6 mixer, supplied by Metcalfe Catering Equipment Ltd , Blaneau Ffestmiog, Wales The resulting wet agglomerates were then dried in an oven at 150°C for 4 hours, gently forced through a 600 micron screen and sieved at 125 microns to collect the greater than 125 micron fraction Each silica 1 to 5 was agglomerated this way to produce agglomerates A to E
  • the strength of the prepared agglomerates was determined as outlined earlier Table 2 records these strengths as the energy required to reduce 50% of the structure to less than 45 microns particle size The results of Table 2 show that a wide range of strengths is attainable, the strength being a function of the physical characteristics of the silica particles making up the structure, as well as pressure applied and number of passes made through the agglomerator Beer Stabilisation
  • Table 4 shows, on a beer different from the beer tested on Table 3, that an input of sufficient energy to reduce the agglomerates to small particle size (cf Table 2) is effective in delivering the beer stabilising performance of the pre-agglomerated particles
  • Example D (prepared from silica example 4 of table 1 ) is a poor stabiliser in both pre and de-agglomerated forms due to not having a suitable pore structure for beer stabilisation, i e having a mean pore diameter of less than 60 Angstroms and a pore volume of less than 1 cm 3 /g All of the remaining samples are good stabilisers and recover their performance following de-agglomeration Table 1 : Physical properties of the silicas prior to Agglomeration

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Genetics & Genomics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Food Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
  • Silicon Compounds (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

L'invention a pour objet des agglomérats de silice non poudreux pouvant être utilisés dans la stabilisation de la bière.
EP97945973A 1996-12-20 1997-11-28 Silices agglomerees Withdrawn EP0956335A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GBGB9626611.9A GB9626611D0 (en) 1996-12-20 1996-12-20 Agglomerated silicas
GB9626611 1996-12-20
PCT/GB1997/003281 WO1998028401A1 (fr) 1996-12-20 1997-11-28 Silices agglomerees

Publications (1)

Publication Number Publication Date
EP0956335A1 true EP0956335A1 (fr) 1999-11-17

Family

ID=10804834

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97945973A Withdrawn EP0956335A1 (fr) 1996-12-20 1997-11-28 Silices agglomerees

Country Status (7)

Country Link
EP (1) EP0956335A1 (fr)
JP (1) JP2001506860A (fr)
AU (1) AU5129298A (fr)
BR (1) BR9714058A (fr)
CA (1) CA2274242A1 (fr)
GB (1) GB9626611D0 (fr)
WO (1) WO1998028401A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SG99853A1 (en) * 1996-02-22 2003-11-27 Neurosearch As Tropane-derivatives, their preparation and use
US6013187A (en) * 1998-08-31 2000-01-11 Dow Corning Corporation Method for removing metal contaminants from solution using mercapto-functional silica xerogels

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL7014811A (fr) * 1970-10-09 1972-04-11
US4457900A (en) * 1982-04-30 1984-07-03 Akzona Incorporated Silicic acid for the filtration of beverages, particularly beer
GB8707526D0 (en) * 1987-03-30 1987-05-07 Unilever Plc Amorphous silicas
US5232724A (en) * 1988-12-22 1993-08-03 Unilever Patent Holdings B.V. Method for stabilizing alcoholic beverages using an aqueous suspension containing amorphous silica
DE19516253A1 (de) * 1995-04-26 1996-10-31 Grace Gmbh Mattierungsmittel auf Basis von aggregiertem Siliciumdioxid mit verbesserter Effizienz

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9828401A1 *

Also Published As

Publication number Publication date
WO1998028401A1 (fr) 1998-07-02
GB9626611D0 (en) 1997-02-05
CA2274242A1 (fr) 1998-07-02
JP2001506860A (ja) 2001-05-29
AU5129298A (en) 1998-07-17
BR9714058A (pt) 2000-05-09

Similar Documents

Publication Publication Date Title
EP0235352B1 (fr) Gel de silice hydraté pour la stabilisation de la bière
US20100021601A1 (en) Stabilising Beverages
AU2002217323A1 (en) Stabilising beverages
EP0683222A2 (fr) Agent stabilisateur pour la bière
CA1305694C (fr) Silices amorphes
EP0377301B2 (fr) Suspensions stables de silice
EP0956335A1 (fr) Silices agglomerees
US5232724A (en) Method for stabilizing alcoholic beverages using an aqueous suspension containing amorphous silica
MX2009001405A (es) Auxiliar para la clarificacion de la cerveza, basado en zerogel de silice, con elevada capacidad de filtracion.
US4457900A (en) Silicic acid for the filtration of beverages, particularly beer
NZ201648A (en) A composition and method for stabilizing beverages against haze formation
JP2003190781A (ja) 濾過助剤用シリカゲル
WO2004091318A1 (fr) Procede de production d'aliments ou de boissons a partir de racine de malt
JP4537857B2 (ja) カンラン石からシリカを製造する方法
USRE32503E (en) Silicic acid for the filtration of beverages particularly beer
CA2013970C (fr) Traitement de boissons alcooliques
JP3719686B2 (ja) 濾過剤用シリカゲル
USH89H (en) Apple juice clarification by using silica hydrogels
JPH07138018A (ja) 炭酸カルシウム分散体の製造方法及び食品組成物
EP1744989B1 (fr) Suspensions stabilisees d'aluminosilicate
RU2221860C1 (ru) Водка и способ ее производства
WO1991019780A1 (fr) Elimination de proteine au moyen de dioxyde de silicium precipite
RU2221861C1 (ru) Водка и способ ее производства
US4758633A (en) Insoluble vinyl lactam clarifiers
JPH0870827A (ja) 飲料用消泡剤とそれを添加した缶入り飲料およびその製造方法

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19990521

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: INEOS SILICAS LIMITED

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20020601