AU619242B2 - New sweetening food product based on saccharose and intense sweetener, and methods for its preparation - Google Patents

Abstract

New granular sweetening food product comprising saccharose and at least one intense sweetener, characterized in that it contains from 50 to 99 % by weight of saccharose and from 1 to 50 % of at least one intense or strong sweetener, in that its apparent density is between 0.4 and 0.7 g/cm<3>, preferably between 0.45 and 0.55 g/cm<3>, and in that the mean diameter of the grains is between 150 and 500 mu m, preferably equal to about 200 mu m. The new product of the invention is stable in storage conditions. It is easy to handle. It is also easy to dose accurately and has a sweetening power equal to that of saccharose and brings in a reduced, practically negligible number of calories. The sweetening product may be added to various food products such as beverages, ice creams, dairy products such as yaourts and white cheese, confectionery, as well as food products in the form of powders.

Description

i i ~ls OPI DATE 19/02/90 APPLN. ID 29120 89h tI Ai 5j*-D E J ATE 29/03/90 PCT NUMBER PCT/FR88/00648 MDE KNALt FU1IIULLt IN VtKIU UU IAIIIt Ut LUrLKA ILUIN YIN IviAiIcrAr DE BREVETS (PCT) ap (51) Classification internationale des brevets4 (11) Numro de publication internationale: WO 90/01070 C13F 3/00, A23L 1/236 Al (43) Date de publication internationale: 8 f6vrier 1990 (08.02.90) (21) Numro de la demande internationale: PCT/FR88/00648 (81) Etats dsign6s: AU, DK, FI, JP, NO, US.

(22) Date de d6p6t international: 30 d6cembre 1988 (30.12.88) Publibe Avec rapport de recherche internationale, Donn6es relatives g la priorit6: 88/10004 25 juillet 1988 (25.07.88) FR (71) D6posant (pour tous les Etats dsign&b sauif US): BEGHIN- SAY [FR/FR]; F-59239 Thumeries (FR).

(72) Inventeurs; et Inventeurs/D6posants (US seulement) GENERMONT, G6rard [FR/FR]; 17, rue Gagn6e, F-94200 Ivry LE- PIETRE, Guy [FR/FR]; 118, av. Jean-Jaurbs, F-75019 Paris (FR).

(74)Mandataire: DAVID, Daniel; B6ghin-Say, 54, avenue Hoche, F-75008 Paris (FR).

(54)Title: NEW SWEETENING FOOD PRODUCT BASED ON SACCHAROSE AND INTENSE SWEETENER, AND METHODS FOR ITS PREPARATION (54)Titre: NOUVEAU PRODUIT EDULCORANT ALIMENTAIRE A BASE DE SACCHAROSE ET D'EDULCORANT INTENSE ET PROCEDES POUR LE PREPARER (57) Abstract New granular sweetening food product comprising saccharose and at least one intense sweetener, characterized in that it contains from 50 to 99 by weight of saccharose and from I to 50 of at least one intense or strong sweetener, in that its apparent density is between 0.4 and 0.7 g/cm 3 preferably between 0.45 and 0.55 g/cm 3 and in that the mean diameter of the grains is between 150 and 500 ptm, preferably equal to about 200 p m. The new product of the invention is stable in storage conditions.

It is easy to handle. It is also easy to dose accurately and has a sweetening power equal to that of saccharose and brings in a reduced, practically negligible number of calories. The sweetening product may be added to various food products such as beverages, ice creams, dairy products such as yaourts and white cheese, confectionery, as well as food products in the form of powders.

(57) Abreg6 Nouveau produit dulcorant alimentaire granulaire comprenant du saccharose et au moins un 6dulcorant intense caractbris6 en ce qu'il contient de 50 A 99 en poids de saccharose et de 1 A 50 d'au moins un 6dulcorant intense en ce que sa densit& apparente est comprise entre 0,4 et 0,7 g/cm 3 de pr~f~rence entre 0,45 et 0,55 g/cm 3 et en ce que le diametre moyen des grains est compris entre 150 et 500 plm, de pref6rence 6gal a environ 200 pm. Le nouveau produit de l'invention est stable au stockage. Il est de manipulation aisbe. 11 est facile A doser de faqon pr6cise et A pouvoir sucrant 6gal a celui du saccharose, il n'apporte qu'un nombre de calories r6duit, voire n6gligeable. Le produit 6dulcorant peut 8tre ajout6 A des produits alimentaires divers, comme par exemple les boissons, les glaces, les produits laitiers tels les yaourts et le fromage blanc, la confiserie, ainsi qu'A des produits alimentaires sous forme de poudres.

t -LI r ~rr~i--l i ii I -1- NEW FOODSTUFF SWEETENING PRODUCT BASED ON SACCHAROSE AND AN INTENSIVE SWEETENER, AND PREPARATION PROCESSES The present invention concerns a novel food sweetening product based on an intensive sweetener and saccharose, and processes for preparing the food sweetening product. More specifically, the present invention concerns a novel granular sweetening product containing saccharose and at least one intensive sweetener of which the quantity can be as high as 50% by weight of the sweetening product.

Intensive sweeteners, such as saccharine, saccharinates, acesulfame, and especially intensive sweeteners of the dipeptide type, the esters of phenylalanine aspartyl of which the most widely used is methylester, a-L-aspartyl-L-phenylalanine methylester, known as aspartame are widely used in the foodstuff industry because of their high sweetening powers at least 150 times that of saccharose.

However, some properties of intensive sweeteners may hamper their applications and, in particular, may generate problems when they are incorporated into foodstuffs.

These properties include their mediocre solubility and their low wetting, their becoming adhesive in a humid environment and tendency to agglomerate, their exceedingly high sweetening power which (when high accuracy is required) makes the sweeteners difficult to dose, -the presence of fines, thereby hampering their handling, and their storage instability.

Various solutions have been suggested to palliate the drawbacks entailed in using intensive sweeteners in the I I I M -2foodstuff industry. Recent research mainly has been aimed at aspartame which is an intensive sweetener very widely used.

European Patent No. A-0102032 describes a liquid sweetening product comprising aspartame and an aqueous dispersant, and preferably includes a sugar. Such a liquid product is neither easily stored nor easily dosed.

European Patent No. A-0106910 describes a solid sweetening product in the form of molded items, such as items in the shape of cubes. The solid sweetening product contains a dipeptide-based sweetener, preferably aspartame, and at least one excipient which can be saccharose. The quantity of dipeptide-based sweetener is 0.3 to 30% by weight relative to the excipient. However, when the excipient mainly comprises saccharose, the amount of dipeptidebased intensive sweetener must be from 2.0 to 10% by weight relative to the excipient. When the excipient proportion is less, solubility and wetting of the dipeptidebased sweetener will be improved only in a mediocre manner.

Moreover, the product so obtained is too fine and, accordingly, handling of the product is greatly hampered (page 3, line 21 through page 4, line 1; and page 5, line 19 through page 6, line In other words, when a composition contains a dipeptide-based sweetener, such as aspartame, and saccharose, the quantity of aspartame cannot exceed 9% by weight of the total composition. Accordingly, the molded and illustratively cube-shaped product of European Patent No. A-0106910 is thereby prevented from being incorporated as such in a homogeneous manner into foodstuffs such as ice cream, yogurt, or powdered products.

One object of the present invention is to provide a sweetening product with a sweetening power, substantially lleV f~obe h corpoo'-e higher than saccharosea and th io4 .porain--f... an ing prodtet in an accurate and homogeneous manner into various food products, whether these products be liquid, semi-liquid, pastes, or powders.

se e 0 00 0 06 00 a *5* S 5 Other objects and advantages of the invention will be elucidated in the description below.

The present invention provides a granular sweetening product comprising saccharose and at least one intensive sweetener, wherein the granular sweetening product has an alveolar structure and contains 50 to 99% by weight of saccharose and 1 to 50% by weight of at least one intensive sweetener, and its bulk density is between 0.4 3 3 and 0.7 g/cm preferably between 0.45 and 0.55 g/cm with the mean grain diameter being between 150 and 500 pm, preferably about 200pm.

For reasons of semantic simplification, the expression "intensive sweetener" as used herein will denote within the present description, as well as in the claims, one or more intensive sweetener(s). Furthermore, the expression "moderate conditions" as used herein means mixing at low rotational speeds.

The present invention also provides several processes for preparing this novel sweetening product.

The first process of the invention comprises the following stages: preparing saccharose particles having a mean diameter of between 150 and 500 pm by the following steps: (al) granulating saccharose in the moist phase in a continuous granulating device, with the granulating device receiving in its upper part crystallized saccharose having a mean diameter of between and 100 pm, with water being added substantially during the addition of the crystallized saccharose and 30 with hot air being blown in such a manner as to cause the hot air to rise into the granulating device so as to form saccharose particles having an alveolar structure; (a2) drying and cooling the saccharose particles formed in step (al) on a fluidized bed which is connected to the lower part of the granulating device; (a3) sifting the particles formed in step (a2) so as to obtain saccharose particles having a mean diameter between 150 and 500 pm; and SbC~~ 5.55.

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R4 1 0O 3 :lir.: i 1: r; mixing the saccharose particles obtained in step (a3) with an intensive sweetener present in powder form under moderate conditions and for a time sufficient to produce the desired product.

The second process of the invention comprises the following steps: (al) humid-phase granulation in a continuous granulating device which, in its upper part, receives a crystallized saccharose having a mean diameter of between 80 and 100 pm and a crystallized intensive sweetener having a mean diameter of less than about 500 pm, wherein the intensive sweetener is pre-mixed with the crystallized saccharose, water is added substantially during the addition of the crystallized initial products, and hot air is blown in a rising manner into the granulating device so as to form granular sweetener particles having an alveolar S: structure; 6O** (a2) drying and cooling the particles of granular sweetener formed in step (al) on a fluidized bed which is S 20 connected to the lower part of the granulating device; and (a3) sifting the particles formed in step (a2) in such a manner as to obtain particles of the desired granular sweetener having an average diameter of between 150 and 500 pm.

In a variation of the first described process, and constituting the third process of the invention, a portion of the intensive sweetener is added in the granulation step with the remaining portion being added during Sstage o oo o~o S2328Z -4- L_ I~l i; _EMIR- The addition of water as recited in step (al) of the processes of the invention can consist of steam injection, atomized water, or a granulation solution.

Illustratively, intensive sweeteners usable in the present invention can be saccharine, saccharinates, acesulfame and dipeptide sweeteners such as esters of aspartyl phenylalanine of which the most widely used is a-L-aspartyl- L-phenylalanine methylester, also known by the name aspartame This listing is not all inclusive of suitable intensive sweeteners.

The novel foodstuff of the present invention which is based on saccharose and an intensive sweetener can also include a complementary support consisting of one or more constituents such as gelling agents; texturizers; stabilizers, illustratively pectins; animal and vegetal proteins, in particular lactic proteins; fibers; carboxymethyl-cellulose; cyclodextrins; etc.

The sweetening product of the present invention when containing a complementary support can be prepared in a variety of ways. The complementary support can be added in the course of mixing stage under moderate conditions either with the totality of the intensive sweetener when using the first process described above, or with a portion of the intensive sweetener when using the third process described above, or else alone when using the second process described above in which case stage is part of the process.

In a variation of the preparation processes of the invention for the sweetening product containing a complementary support, part of the complementary support can be added during step with the remainder being added during stage As noted above, the addition of water in step (al) of the processes of the invention can consist of injecting steam, atomizing water, or using a granulation solution. I L -6- When using a granulation solution, the granulation solution, illustratively, can be a saccharose syrup or an aqueous solution of a complementary support, for example a gelling pectin solution. Accordingly, in some cases it is possible to introduce in part or in whole the complementary support when called for by atomizing, during the granulation process step or as a solution of the complementary support.

One mode of preparing the sweetening product of the invention is described for illustration purposes in detail below.

E-qmMPe. Icing sugar, which is crystallized saccharose having a mean diameter between 80 and 100 Am, is supplied by a volumetric or gravimetric metering means for example a screw dosimeter to the upper part of a granulation chamber. The lower part of this granulation chamber communicates with a fluidized bed onto which is blown air. The temperature of the air decreases from upstream to downstream from a temperature 100°C (hot air) to a temperature of (cold air). Steam is injected into the granulation chamber essentially upon the incorporation of the icing sugar. At the same time, the hot air is blown upstream of the fluidized bed, causing turbulence whereby the particles of icing sugar agglomerate one to another and thereafter subsequently granulate. The agglomerated and granulated particles by their own weight drop into the lower part of the granulation chamber where they are picked up by the air flow of the fluidized bed. The particles then advance on the fluidized bed and are cooled by the cold air flow at 15-20°C before being evacuated from the fluidized bed. T1e particles then are moved to a sieve so as to provide saccharose particles having a suitable granulometry (average diameter being between 150 and 500 Mm). Thereafter, the saccharose particles are mixed with an intensive sweetener to form a powder by means of a "soft" mixer; for example, a ribbon or paddle mixer, at low rotational speeds. The required i,

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-7amount of intensive sweetener can be added in one or several batches.

Illustratively, for example, to manufacture 50 kg of the product of the invention containing 30 kg saccharose and 20 kg intensive sweetener, a ribbon mixer which holds 200 liters and operates at 30-40 rpm can be used. The 20 kg of intensive sweetener can be added in o e batch to the kg of sifted saccharose particles by mixing for 15 to minutes. Alternatively, 6.7 kg intensive sweetener can be added three times, with the interval between additions being minutes and the final mixing being set at 10 minutes. As a rule, the mixing time for the sifted saccharose particles following their exit from the fluidized bed jointly with the intensive sweetener is set so that the intensive sweetener is fully incorporated into the saccharose particles and full product homogeneity is achieved.

The product of the invention prepared in the manner illustrated above is not a mere mixture of saccharose and intensive sweetener. In this regard, ultrasonic sedimentation tests have been carried out on a product of the invention containing 40% by weight of AP and 60% by weight of saccharose. Dosages at different heights revealed no significant deviation of the components.

The novel sweetening product of the invention contains no fines and, therefore, is easily handled. The product is storage-stable and does not agglomerate. This product is easily dosed because of the simultaneity of its granular shape and low-bulk density. It dissolves well in water, and its wetting is excellent. For example, 2.5 g of the product of the invention cont-ining 1.5 g saccharose and 1 g AP dissolves in one liter of water at 20°C four times more rapidly than 1 g of AP alone.

Moreover, while having a sweetening power equal to that of saccharose, the product of the invention introduces only a minimal number of calories, even a negligible number.

For instance, a product of the invention containing 60% by -8weight saccharose and 40% by weight AP will be about times as sweet as saccharose. Accordingly, at a sweetening power equal to that of saccharose, this product will introduce a number of calories less than 1% of that which would have been present with saccharose, a negligible amount.

The novel sweetening product of the invention can be added to various foodstuffs, such as beverages, ice cream, dairy products such as yogurt and cream cheese, candies, foodstuffs present in powder form, etc.

The formulation of the present invention can be accommodated to each specific case, in particular by selecting the intensive sweetener(s) present and by adjusting the dosage or the intensive sweetener(s) present.

L tI

Claims (15)

1. A granular foodstuff sweetening product comprising saccharose and at least one intensive sweetener, wherein V% as cO<^ ove a\Cr sCVcAAe k-i said sweetening product4contains from 50 to 99% by weight of saccharose and from 1 to 50% by weight of at least one intensive sweetener, and has a bulk density of between 0.4 and 0.7 g/cm 3 and a mean grain diameter of between 150 and 500 pm.

2. The sweetening product defined in claim 1, wherein 3 15 the bulk density is between 0.45 and 0.55 g/cm.

3. The sweetening product defined by either of claims 1 and 2, wherein the mean grain diameter is approximately 200 pm. 20

4. The sweetening product defined in any one of claims S1 to 3, wherein said sweetening product further comprises a complementary support.

5. The sweetening product defined in claim 4, wherein said complementary support is made up of one or several constituents selected from among gelling agents, texturing agents and stabilizers such as pectins, animal and vegetal proteins, in particular lactic proteins, fibers, carboxymethyl-cellulose and cyclodextrins.

6. A process for preparing the sweetening product defined in any one of claims 1 to 5 and comprising the following steps: preparing saccharose particles having a mean diameter between 150 and 500 pm and including the steps: (al) granulating the saccharose in the moist phase in a continuous granulation device which at its upper 1761Z T L. ~~~PISU~PX part receives the crystallized saccharose having a mean diameter of between 80 and 100 pm and adding water essen- tially during the addition of said crystallized saccharose, hot air being blown in a rising manner into said granulating device so as .o ?orm sacc'ro.ose. horl o- o\veo\o.r s -ruckuve. (a2) drying and cooling the saccharose pprticles formed in step (al) on a fluidized bed connected to the lower part of said granulating device, (a3) sifting the particles from step (a2) in such a manner as to obtain saccharose particles having a mean diameter of between 150 and 500 /m, mixing the saccharose particles from step (a3) with the intensive sweetener in the form of a powder and, where called for, the complementary support under moderate conditions and over a time sufficient to obtain the desired product.

7. Process for preparing a sweetening product defined in one of the claims 1 through 5 and comprising the steps: (al) moist-phase granulation in a continuous granulating device receiving at its upper part the crystall- ized saccharose having a mean diameter of between 80 and 100 pm together with the crystallized intensive sweetner having a mean diameter less than about 500 pm and, where called for the complementary support, which where called for are pre-mixed to said crystallized saccharose, and then adding water essentially during the addition of the crystal- lized initial products, hot air being blown in a rising manner into said granulation device so a h t orm Qan\or (a2) drying and cooling of the granular sweetener particles formed in step (al) on a fluidized bed connected to the lower part of said granulating device, (a3) sifting the particles from step (a2) in such a manner as to obtain particles of the desired granular sweetener having a mean diameter between 150 and 500 pm. L -11-

8. Process for preparing a sweetening product defined in one of claims 1 through 5 and comprising the fol- lowing stages: preparing sweetener particles having a mean diam- eter between 150 and 500 Am and including the following steps: (al) moist-phase granulation in a continuous granulation device which is supplied at its upper part with the crystallized saccharose having a mean diameter between and 100 gm together with a part or the whole of the intensive sweetener having a mean dianmeter less than about 500 Am and where called for a part or the whole of the com- plementary support possibly pre-mixed to said crystallized saccharose, followed by adding water essentially during the addition of the crystallized initial products, hot air being blown in a rising manner into said granulating device SO Q% o (a2) drying and cooling the granular sweetener particles formed in step (al) on a fluidized bed connected to the lower part of said granulating device, (a3) sifting the particles from step (a2) in such a manner as to obtain granular sweetener particles having a mean diameter between 150 and 500 Am, mixing the granular sweetener particles from step (a3) with the remainder of the intensive sweetener in the form of powder and the remainder of any complementary sup- port under moderate conditions and over a time sufficient to obtain the desired product.

9. Process defined in claim 8 wherein all the intensive sweetener is added during stage or ca vy. 9 Process defined in claim 8 A wherein all the complementary support, if any, is added in the course of stage -12-

11. Process defined in any one of claims 6 through wherein said water addition of step (al) consists in in- jecting steam.

12. Process defined in any one of claims 6 through wherein said water addition of step (al) consists of atomizing water or a granulation solution.

13. Process defined in claim 12, wherein sasd granulation solution is a saccharose syrup.

14. Process defined in claim 12, wherein said granulation solution iF a complementary-support solution, for instance a gelling-agent solution. a s

15. The sweetening product according to claim 1, substantially as herein described with reference to.the Example.

16. A process for preparing the sweetening product defined in claim 1, substantially as herein described with reference to.the g Example. DATED 15 AUGUST, 1991 PHILLIPS ORMONDE FITZPATRICK Attorneys For: BEGHIN-SAY I V© 0 [Y .11 I- -13- ABSTRACT The invention concerns a ncvel foodstuff sweeten- ing product comprising saccharose and at least one intensive sweetener. The sweetening product contains from 50 to 99% by weight saccharose and 1 to 50% by weight of at least one intensive sweetener. The bulk density of the product is between 0.4 and 0.7 g/cm 3 and preferably between 0.45 and 0.55 g/cm 3 The mean grain diameter of the product is be- tween 150 and 500 Am, preferably being about 200 Am. The novel product of the invention is storage-stable, easily handled, and easily dosed in a precise manner. The product has a sweetening power equal to that of saccharose, while having only a reduced, even negligible, number of calories. The sweetening product can be added to diverse foodstuffs, such as beverages, ice cream, dairy products such as yogurt and cream cheese, candy, and powdered foodstuffs. INTERNATIONAL SEARCH REPORT International Application No PCT/FR8 8 00 6 4 8 I. CLASSIFICATION OF SUBJECT MATTER (if several classification symbols apply, Indicate all) According to International Patent Classification (IPC) or to both National Classification and IPC Int.Cl.4 C13F 3/00 A23L 1/236 II. FIELDS SEARCHED Minimum Documentation Searched 7 Classification System Classification Symbols Int.Cl.4 C13F A23L Documentation Searched other than Minimum Documentation to the Extent that such Documents are Included in the Fields Searched III. DOCUMENTS CONSIDERED TO BE RELEVANT' Category Citation of Document, with indication, where appropriate, of the relevant passages 12 Relevant to Claim No.1 3 A EP,A, 0218570 (RAFFINERIE TIRLEMONTOISE) 1-4 April 1987 see claims 1-3,6,9 A EP,A, 0219150 (RAFFINERIE TIRLEMONTOISE) 1-4 22 April 1987 see claims 1,2,11-13 A EP,A, 0052919 (AMSTAR CORP.) 2 June 1982 1-4 see claims 1,2,6; example 13 A EP,A, 0102032 (AJINOMOTO CO.) 7 March 1984 1-4 see claims 1-3 cited in the application A EP,A, 0106910 (AJINOMOTO CO.) 2 May 1984 1-4 see claims 1,4 example 1 cited in the application SSpecial categories of cited documents: 1t later document published after the international filing date document defining the general state of the art which is not r priority date and not in conflict with the application but condered to be o particular reevance cited to understand the principle or theory underlying the invention earlier document but published on or after the international document of particular relevance: the claimed invention filing date cannot be considered novel or cannot be considered to document which may throw doubts on priority claim(s) or involve an inventive step which Is cited to establish the publication date of another document ot particular relevance; the claimed invention citation or other special reason (as specified) cannot be considered to involve an inventive step when the document referring to an oral disclosure, use, exhibition or document is combined with one or more other such docu- other means ments, such combination being obvious to a person skilled document published prior to the international filing date but in the art. later than the priority date claimed document member of the same patent family IV. CERTIFICATION Date of the Actual Completion of the international Search Date of Mailing of this International Search Report 12 April 1989 (12.04.89) 3 May 1989 (03.05.89) International Searching Authority Signature of Authorized Officer European Patent Office Form PCT/ISA/210 (second sheet) (January 1985) Mn, r ANNEX TO THE INTERNATIONAL SEARCH REPORT ON INTERNATIONAL PATENT APPLICATION NO. FR 8800648 SA 26199 This annex lists the patent family members relating to the patent documents cited in the above-mentioned international search report, The members are as contained in the European Patent Office ED)P file on 261(04/89 The European Patent Office is in no Aay liable for these particulars hich are merely given for the purpose of information. Patent document Publication Patent family Publication cited in search report date member(s) date EP-A- 0218570 15-04-87 BE-A- 902356 02-09-85 US-A- 4746520 24-05-88 EP-A- 0219150 22-04-87 LU-A- 86076 02-04-87 EP-A- 0052919 02-06-82 US-A- 4338350 06-07-82 JP-A- 57122759 30-07-82 CA-A- 1154628 04-10-83 EP-A- 0102032 07-03-84 JP-A- 59031669 20-02-84 US-A- 4722844 02-02-88 JP-A- 59031656 20-02-84 EP-A- 0106910 02-05-84 For more details about this annex :see Official Journal of the European Patent Office, No. 12/82 L~ .i I t 1 RAPPORT DE RECHERCHE INTERNATIONALE Demands lniernatlonale N, PCT/FR 88/00648 1. CLASSEMENT DIE LINVENTION (si plusieura symboles de classification sont applicable., ins indliquer tous)I Solon I& classification internstlonalo des brevets (CIB) ou 4k Ia Ibis sIna classification niationalte et& CIB CIB 4:C 13 F 3/00; A 23 L 1/236 It. DOMAINES SUR LESQUELS LA RECHERCHE A PORTE Documentation mlnimale consute I Systimo de classification Symbol., do clasuification 4 C 13 F; A 23 L CIB Documentation consuitde autre quo Ia documentation minlmale dans Ia meaure oOj de tel. documents font peris des domaines sur tesquels a& recherchie a portA 1 11l. DOCUMENTS CONSIDI!R9S COMME PERTINENTS CtgreIdentification des documents cit~s,U avec indication, ai niceasaire, N* des rovendicetiona Catgoiedes passages pertinents 12 visiies 12 A EP, A, 0218570 (RAFFINERIE TIRLEMONTOISE) 1-4 avril 1987 voir revendications 1-3,6,9 A EP, A, 0219150 (RAFFINERIE TIRLEMONTOISE) 1-4 22 avril 1987 voir revendications 1,2,11-13 A EP, A, 0052919 (AMSTAR CORP.) 1-4 2 juin 1982 voir revendications 1,2,6; exemple 13 A EP, A, 0102032 (AJINOMOTO CO.) 1-4 7 mars 1984 voir revendications 1-3 cite dans la demande A EP, A, 0106910 (AJINOMOTO CO.) 1-4 2 mai 1984 voir revendications 1,4; exemple 1 cit6 dans !a demande *Cat~oories sp~ciales de documents cit~s:' aT is document ulttriour pubIA posteriourement h Ia date do d~p~t ot xdoumntd~inssntI'ta gn~aldoIstechnique, non International ou A Ia date do priorito et nappartonant pas sAa ocnt om d pfin icuiesatpetnnt ALta P~~a d aaint de Ia technique pertinent. mais citt Pour comprendre conad~r com prticti~emen petinetIt principe ou Is thilorie constituent I& base do l'invention Eai document ant~rieur, main publid A Ia date do ddp6t Interna- aX a document particulikrement pertinent: l'invontion roendi- tional ou apris cette date qu~e no pout 6tre conaidirie comma nouvelle ou comme L document Pouvant laer un doute aur une revendicatlon do Impliquant une activiti inventive prioritt ou cit6j pour diterminer t& date os publication d'une it Y a document particulirroent pertinent; linvention reven- autre citation ou pour une raison ap~clale (totle qu'indiqu~e) diqu~e no pout 6tro conaidkrA. comme Implipuant une 0 as document so rdt~rant A une divulgatlon orate, A un usage, A activitt inventive tarsoue ts document eat associ6A un ou une exposition ou tous autran moyons plusioursa utroa documents do mhme nature, corto combi- P document publit avant In date do d~p6t International, mali naisan *tant dvidonte pour une personne du mitier, post~riourement A Ia date do prioritik revendiqute e& a document qul fatt partia do to m~in. famille do brovets IV. CERTIFICATION Date A taquelle to recherche Internationale a efloctivoment Date d'exp~dition du present rapport do recherch~e internationati' achevke 12 avril 1989 03. O5. 89 Administration charg~e do to recherche Internationale Signature di iqhtocn mire autorisd OFFICE EUROPEEN DES BREVETS L OS Formulaire PCTIISA121D (douxibme leuilit) (janvier 1985) ANNEXE AU RAPPORT DE RECHERCHE INTERNATIONALE RELATIF A LA DEMANDE INTERNATIONALE NO. FR 8800648 SA 26199 La pr sente annexe indique Ics mcmhres de la famille dc brevets reiatifs aux documents bre-sets citk~ dang le rapport de recherche intcrnationale %is6 ci-dessits. Lesdits nicmbres sont contenus au fichier informatiquc de I'Office cturop~en des brevets ii la date du 26/04/89 Les renseignements fournis sent donncs i tre indicatif et n'cngagcnt pa,; la responsabilite de I'001ce europcen des brescts. Document brevet c6tt Date de Memrbre(s) de la P~ate de au rapport de recherche publication fatnille de brevet(s) publication EP-A- 0218570 15-04-87 BE-A- 902356 02-09-85 US-A- 4746520 24-05-88 EP-A- 0219150 22-04-87 LU-A- 86076 02-04-87 EP-A- 0052919 02-06-82 US-A- 4338350 06-07-82 JP-A- 57122759 30-07-82 CA-A- 1154628 04-10-83 EP-A- 0102032 07-03-84 JP-A- 59031669 20-02-84 US-A- 4722844 02-02-88 JP-A- 59031656 20-02-84 EP-A- 0106910 02-05-84 Aucun Pour tout renseignement concernant cette annexe -voir JournaL Officiel de I'Office europeen des brevets, No.12/82