Europäisches Patentamt

(19) European Patent Office &  

Office européen des brevets (11) EP 1 470 202 B1
(12) EUROPEAN PATENT SPECIFICATION

(45) Date of publication and mention (51) Int Cl.:

of the grant of the patent: C09J 103/02 (2006.01)
10.05.2006 Bulletin 2006/19
(86) International application number:
(21) Application number: 02716704.8 PCT/EP2002/000975

(22) Date of filing: 30.01.2002 (87) International publication number:

WO 2003/064553 (07.08.2003 Gazette 2003/32)

(54) HIGH DRY SUBSTANCE STEIN HALL ADHESIVES AND METHOD FOR PREPARING HIGH DRY
SUBSTANCE STEIN HALL ADHESIVES
STEIN-HALL KLEBEMITTEL MIT HOHEM TROCKENSTOFFGEHALT UND VERFAHREN ZU DEREN
HERSTELLUNG
ADHESIFS STEIN HALL A TENEUR ELEVEE EN MATIERE SECHE ET PROCEDE DE FABRICATION

(84) Designated Contracting States: (74) Representative: Ostyn, Frans

AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU K.O.B. NV,
MC NL PT SE TR Kennedypark 31 c
Designated Extension States: 8500 Kortrijk (BE)
SI
(56) References cited:
(43) Date of publication of application: GB-A- 1 571 336 US-A- 4 917 870
27.10.2004 Bulletin 2004/44 US-A- 6 048 391

(73) Proprietor: Tate & Lyle Europe NV • CHEMICAL ABSTRACTS, vol. 76, no. 14, 3 April
9300 Aalst (BE) 1972 (1972-04-03) Columbus, Ohio, US; abstract
no. 74053k, SMID J. ET AL.: "Wheat starch
(72) Inventor: VANDEVELDE, Dani¬l adhesive" page 100; XP002214862 & DIE
B-9300 Aalst (BE) STÄRKE/STARCH, vol. 25, no. 11, 1973, page 384
EP 1 470 202 B1

Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give
notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in
a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art.
99(1) European Patent Convention).

Printed by Jouve, 75001 PARIS (FR)

 EP 1 470 202 B1

Description

[0001] The invention relates to a method for preparing a Stein Hall adhesive, comprising the steps:

5 - preparing a carrier portion by gelatinising at least a part of the total starch in the adhesive in an alkaline medium;
- diluting the carrier portion with a volume of water; and
- adding the remaining secundary starch,

wherein in a first step said carrier portion is prepared using part of the alkali, and in a second step the carrier portion is
10 diluted with a volume of water, followed by the addition of at least a portion of the secondary starch.
[0002] The invention further relates to a high dry substance Stein Hall adhesive (also called a high concentration Stein
Hall adhesive or glue), containing between 32 and 45 % dry weight starch solids, obtained by a such method.
[0003] Starch based adhesives are well known in the corrugated board industry. Among the adhesives used, Stein
Hall-type adhesives are the most popular.
15 [0004] Stein Hall adhesives are generally known as comprising a carrier portion of the adhesive that is obtained by
gelatinising about 10-20% of the total starch in the glue using caustic soda. The resultant paste is then cooled and diluted
with water and the remaining starch is then added as native granular starch. Also borax (1,5-2,5%) is added.
[0005] In US 4,917,870 for instance, an installation is described which is used for the preparation of starch glues. The
installation comprises a substantially vertical axis; that vessel is equipped with stirring means acting at its lower level; it
20 comprises furthermore pipes to supply the vessel with all the constituents of the glue to be manufactured, the starch
being introduced pneumatically in the form of powder through a pipe. The pipe passes through the wall of the vessel
from the outside to the inside of a level close to the lower portion of the vessel and in the vicinity of the stirring means.
The preparation of the starch glues comprises the steps of first introducing water in the vat, adding corn starch, heating
the starch - water mixture and then adding NaOH solution, and subsequently adding water again, adding the remaining
25 starch and finally adding borax.
[0006] Under these circumstances, the maximum total starch concentration in these Stein Hall-type formulations does
not surpass 25%, although values up to 30-37% on dry weight basis have been reported. These higher values were
obtained when viscosity of the carrier was reduced by means of an oxidation reaction or the like.
[0007] The disadvantage of these low-concentration adhesives is that they contain higher water contents, reduce
30 adhesion speed and retard drying of the adhesive layer in the adhesion step. In addition, higher dry substance adhesives
result in reduced energy consumption because smaller quantities of water need to be evaporated.
[0008] Subsequently, higher starch concentrations in the glue are desirable. But, it is also known that, when starch is
used as the binding agent, there is a limit to the highest amount of starch that can be used. At higher amounts of starch
the amount of water becomes insufficient to guarantee the desired adhesion, while the viscosity of the adhesive becomes
35 too high.
[0009] High concentration starch based adhesives have already been described in the prior art. In EP 0 038 627 a
starch based adhesive is described that is composed of a completely gelatinised starch fraction and a partly swollen
starch fraction, this in a ratio between 0,2:100 and 2:1. The adhesive may contain between 10% and 40% dry weight
starch solids. The gelatinised fraction is obtained by heat treatment at 95 °C or higher, and not via mixing with concentrated
40 alkali as in a classic Stein Hall formulation. In fact, it is a no-carrier type adhesive to which a gelatinised starch fraction
is added to improve wet tack of the adhesive.
[0010] In EP 0 576 221 adhesive compositions are disclosed comprising from 15 to 35% by weight starch solids. A
substantial quantity of the starch is partially swollen (preferably between 20 and 50%).
[0011] EP 0 376 301 describes an adhesive prepared by treating a starch slurry in a jet cooker at a temperature
45 between 120 and 200°C to obtain a gelatinised dispersion. The ungelatinised is then added to this gelatinised dispersion.
The total starch solids content in this formula, as illustrated in the examples, varied between 32 and 40%.
[0012] Also in GB 1 571 336, a method is described for the preparation of a starch-based aqueous adhesive. In this
method, a carrier portion is prepared of gelatinised molecularly dispersed starch at a solids content from 3 % to 40 %
by weight by cooking a starch slurry using a jet cooker. The carrier portion is ten mixed with a slurry of ungelatinized
50 starch. Alkali is provided in the resulting mixture.
[0013] The adhesives described in these applications are not typical Stein Hall compositions.
[0014] In EP 1 101 809, high dry substance starch-based adhesives are described containing at least 40%, preferably
at least 46% dry substance. This high dry substance content is realised by the addition of inorganic salts, preferably
calcium carbonate, to the starch-based adhesive. The starch/filler ratio is preferably at least 60:40. The adhesive can
55 be of the Stein-Hall, no-carrier or Minocar-type.
[0015] In EP 0 409 240, a high concentration starch slurry adhesive is described comprising between 20 and 60% by
weight of starch solids. This adhesive is stabilised through the addition of a gum such as xanthan or rhamsan gum and
some sodium hydroxide.

2
 EP 1 470 202 B1

[0016] In WO 9850478 high dry substance adhesive compositions are that contain a substantive amount of water-
soluble alkaline silicate, together with starch, borax and sodium hydroxide. Adhesive compositions containing up to 45%
solids are disclosed in the examples.
[0017] Part of the above-cited prior-art documents are not related to Stein-Hall type adhesives, such as EP 0 O38
5 627, EP 0 576 221, EP 0 376 301 and EP 0 409 240.
[0018] The two other documents cited, i.e. EP 1 101 809 and WO 9850478, may comprise Stein Hall-type adhesives,
but they differ substantially from standard formulations in that they contain inorganic filler material that contributes to the
high dry substance of the glue.
[0019] In the state of the art, further high dry substance Stein Hall-type adhesives have been disclosed.
10 [0020] In US 3,912,531 high dry substance adhesives of the Stein Hall-type are disclosed containing up to 40% by
weight of starch solids.
[0021] However, the disadvantage of this kind of high dry substance Stein Hall adhesives is that this is realised by
using a fluidity starch having a fluidity between 25 and 90 as the carrier starch or as part of the carrier starch.
[0022] Also EP 0 049 009 discloses high dry substance glues of the Stein Hall-type. The problem underlying this
15 patent document is how to obtain a final high DS glue where the viscosity does not increase strongly and whereby the
mixture remains pumpable. In fact the glue must show some storage stability and workable viscosity.
[0023] In the patent document, it is stated that high dry substance glues can not be obtained with the conventional
technology for preparing Stein Hall-type adhesives (which have a low dry substance). As described above, the method
by which these kinds of Stein Hall-type glues are prepared comprises preparing the carrier and thereafter diluting it by
20 lowering the alkalinity. When the alkalinity would not be lowered, the addition of the secundary starch would be affected
and would result in granule swelling and viscosity instability.
However, if high dry substance glues have to be obtained, dilution is becoming insufficient to prevent undesirable swelling.
In addition to this, the combination of less diluted carrier and high secundary starch concentration will result in composition
that are no longer workable.
25 [0024] The solution to this problem that is proposed in the application EP 0 049 009 consists in oxidising the carrier
portion and then gelatinising the oxidised starch in presence of the necessary amount of sodium hydroxide, thereby
reducing the viscosity of the carrier to a value which makes it possible to add the required secundary starch. This
secundary starch is then added to reach a 40% d.s. glue. It should be emphasised that the carrier starch portion in the
glue represents more than 14% of the starch dry substance present in the glue.
30 [0025] The disadvantage of this method is that high dry substance glues are obtained with the necessity of using
reduced viscosity starches in the carrier fraction.
[0026] The reduced viscosity starches referred to in the patent documents of the state of the art typically are fluidity
starches or oxidised starches in which the fluidity starches are obtained via chemical or enzymatic degradation.
[0027] In US 6,048,391, a process is described for the preparation of a starch based glue for making corrugated board.
35 The process is carried out in a system which includes a first and relatively large mixing vessel containing a stirrer. A
second and smaller mixing vessel is connected to the first mixing vessel via a recirculation path. The second and smaller
mixing vessel contains means for exerting a shearing force which is greater than the shearing force exerted in the first
and larger mixing vessel. The process is carried out in two steps. In a first step, water and starch are supplied to form
a carrier in the first mixing vessel, and then the resulting carrier is transported to the second mixing vessel. Lye is first
40 added in a controlled manner in the second mixing vessel to prepare the carrier. A second step adds further amount of
starch, water, borax, and a second shot of lye to the carrier while in the small vessel.
[0028] The disadvantage of this system is that a supplementary mixing vessel is provided, wherein a circulation loop
is introduced. In this way, a technical more complex and more expensive system is provided. Furthermore, the Stein
Hall adhesives as obtained by this method do not have a high dry substance.
45 [0029] The purpose of the invention is to provide a method for preparing a Stein Hall adhesive which doesn’t show
the abovementioned disadvantages.
[0030] This purpose is achieved by providing a method for preparing a Stein Hall adhesive, comprising the steps:

- preparing a carrier portion by gelatinising at least a part of the total starch in the adhesive in an alkaline medium;
50 - diluting the carrier portion with a volume of water; and
- adding the remaining secondary starch;

wherein in a first step said carrier portion is prepared using part of the alkali, and in a second step the carrier portion is
diluted with a volume of water, followed by the addition of at least a portion of the secondary starch, wherein a high dry
55 substance Stein Hall adhesive, containing between 32 and 45 % dry weight starch solids, is prepared using a single
mixing vessel, wherein in the first step said carrier portion is prepared in the single mixing vessel, and in a third step the
remaining alkali is added in a diluted form together with the secondary starch.
[0031] In a preferred method according to the invention, the addition of the remaining secundary starch and alkali is

3
 EP 1 470 202 B1

performed stepwise.
[0032] This has the advantage that the secundary starch is not directly submitted to excessively high alkaline con-
centrations, thus preventing premature swelling of the secundary starch.
[0033] In a more preferred method according to the invention, the addition of alkali and starch is done in at least two
5 steps.
[0034] In a specific method according to the invention, during the first step, a carrier portion is prepared containing
between 2 and 9 % of the total starch content by mixing the starch together with water and alkali until all the starch has
gelatinised.
[0035] In a more specific method according the invention, in the first step, the alkali content in the carrier portion is
10 typically less than 2/3 of the total amount needed in the adhesive formulation.
[0036] In another specific method according the invention, in the second step the carrier portion is diluted with a volume
of water corresponding to 60 to 85 % of the carrier volume.
[0037] In a more specific method according the invention, in the second step 50 to 75 % of the secundary starch is added.
[0038] In a preferred method according to the invention, after the third step borax is added.
15 [0039] The advantage of this is that initial tacking is improved and both water retention and penetration ability of the
adhesive is regulated.
[0040] The purpose of the invention is further achieved by providing a high dry substance Stein Hall adhesive obtained
by a method as described above, whereby

20 - it contains between 32 to 45 % native or stabilised starch;

- the ratio carrier starch to secundary starch is between 1:50 and 1:11;
- it shows a Bauer-viscosity between 21s and 60s; and
- the alkali concentration in the glue is sufficient to provide a SGP of between 45 °C and 53 °C.

25 [0041] In a preferred high dry substance Stein Hall adhesive according the invention, the native or stabilised starch
is obtained from cereal, tuber or root starches.
[0042] The method for preparing the glues of the invention comprises several consecutive steps:

• during a first step a carrier portion is prepared containing between 2 to 9 % of the total starch content, by mixing
30 the starch together with water and alkali until all the starch has gelatinised. The alkali content in the carrier portion
is typically less than 2/3 of the total amount needed in the glue formulation;
• during the next step the carrier portion is diluted with a volume of water corresponding to 60 to 85% of the carrier
volume, followed by the addition of at least half, and at most 75% of the secundary starch.
• in a further step the remaining alkali is then added in a diluted form together with the remaining secundary starch.
35
[0043] The addition of remaining starch and alkali can be performed simultaneously or stepwise. When addition is
performed simultaneously, care must be taken that starch is not submitted directly to alkali.
During the stepwise addition, alkali is first added to the mixture of the first and the next step, followed by the addition of
the remaining secundary starch. Stepwise addition of alkali and starch is preferably done in two or more steps.
40 Finally borax is added to finish the glue.
[0044] The high dry substance Stein Hall type adhesives according to the invention have the following properties:

• they contain between 32 to 45% native or stabilised starch,

• the ratio carrier starch to secundary starch is between 1:50 to 1:11,
45 • they show a Bauer-viscosity between 21 s and 60 s,
• and the alkali concentration in the glue is sufficient to provide a SGP of between 45 and 53°C.

[0045] The native or stabilised starch can be obtained from cereal, tuber or root starches. Typical examples thereof
are e.g. starches obtained from maize, wheat, barley, potato, tapioca or arrowroot, including the waxy and high amylose
50 type starches.
The stabilised starches referred to in the application correspond with starches that have been physically and/or chemically
treated in view of obtaining starches that are less sensitive to alkali at ambient or slightly higher temperatures. As a
result thereof they are not subject to uncontrolled premature swelling and/or gelatinisation.
[0046] The advantage of the high dry substance Stein Hall adhesives according to the invention and produced by the
55 method by the invention is that there is no necessity to use reduced viscosity starches in the carrier fraction, while the
corresponding adhesives still do show excellent storage stability, and workable viscosities. They only contain native or
stabilised starches. Furthermore, a final pumpable high dry substance glue is obtained.
[0047] This invention will now be illustrated by the following examples which should be considered as being not limiting

4
 EP 1 470 202 B1

to the scope of the invention as such and as expressed in the following claims.

Example 1:

5 [0048] A high dry substance glue was prepared as follows:

[0049] In a 2000 1 vessel, first the carrier fraction was prepared. Therefore, 16 l of a 30% w/w NaOH-solution was
mixed into a dispersion containing 28 kg stabilised wheat starch and 650 l water. The mixture was stirred with a high
shear mixer at 1500 rpm for 10 minutes, allowing the starch to gelatinise. The starch in the carrier fraction corresponds
with 3,25% of the total starch content in the glue (1:30 ratio).
10 [0050] In a next step 550 1 tap water was added to the carrier together with 500 kg stabilised wheat starch and 3 kg
borax. The whole was mixed at 1500 rpm for an additional 5 minutes.
Before addition of the remaining alkali and starch, the remaining 12 l 30% w/w NaOH solution was first diluted with 100
l of water.
Then 37 l diluted alkali, followed by 200 kg of stabilised wheat starch was added into the vessel. This mixture was stirred
15 for 5 minutes before a second quantity of 37 1 of alkali and 138 kg of starch was added. Again the mixture was stirred
intensively. Finally the remaining 38 1 alkali and 6,5 kg borax was added while stirring the glue.
[0051] The thus prepared glue formulation comprises 40% by weight starch solids and is composed of:

Water: 13001
20 Starch: 866 kg
Volume: 1820 1
NaOH : 6,25 g/l
Borax : 5,21 g/l

25
[0052] The thus prepared glue did show the following properties:

Direct after preparation After 30 minutes After 6 hours

Bauer (seconds) 22 25 27
30
Brookfield (mPas,20rpm) 480 500 710

SGP: 47°C

35
Example 2:

[0053] In this example a glue is described containing 40% by weight maize starch solids. In a 1500 l recipient, 24 kg
maize starch is dispersed in 440 l water. To this dispersion, 12 kg of 33% w/w NaOH was added and the mixture was
stirred with a high shear mixer for 12 minutes at 1500 rpm. The starch in the carrier fraction corresponds with 4,2% of
40
the total starch content in the glue (1:24 ratio).
In a next step 320 1 water followed by 4,5 kg borax was added and intensively stirred for 3 minutes. Then 300 kg starch
were added to the carrier fraction and homogeneously dispersed therein by mixing at 1500 rpm for an additional
3 minutes. Before addition of the remaining alkali and starch, this additional alkali fraction (10 kg 33% NaOH) was diluted
with 1001 of water.
45
Thus 37 1 diluted alkali, followed by 151 kg of stabilised maize starch was added to the recipient, and stirred at 1500
rpm for 3 minutes. Then a second quantity of alkali, followed by 100 kg of starch was added and dispersed. Finally the
remaining 35 l alkali together with 4 kg of borax was added while stirring.
[0054] The thus prepared glue formulation comprises 40% by weight starch solids and is composed of:

50 Water : 8601
Starch : 575 kg
Volume : 12001 1
NaOH : 6,25 g/l
55
Borax : 6,25 g/l

[0055] The thus prepared glue did show the following properties:

5
 EP 1 470 202 B1

Direct after preparation

Bauer viscosity (seconds) 48
5 Brookfield (mPas, 20rpm) 1600

SGP: 48,5°C

10
Claims

1. Method for preparing a Stein Hall adhesive, comprising the steps:

15 - preparing a carrier portion by gelatinising at least a part of the total starch in the adhesive in an alkaline medium;
- diluting the carrier portion with a volume of water; and
- adding the remaining secondary starch;

wherein in a first step said carrier portion is prepared using part of the alkali, and in a second step the carrier portion
20 is diluted with a volume of water, followed by the addition of at least a portion of the secondary starch,
characterised in that a high dry substance Stein Hall adhesive, containing between 32 and 45 % dry weight starch
solids, is prepared using a single mixing vessel, wherein in the first step said carrier portion is prepared in the single
mixing vessel, and in a third step the remaining alkali is added in a diluted form together with the secondary starch.

25 2. Method according to claim 1, characterised in that the addition of the remaining secondary starch and alkali is
performed stepwise.

3. Method according to claim 2, characterised in that the addition of alkali and starch is done in at least two steps.

30 4. Method according to any one of the claims 1 to 3, characterised in that during the first step, a carrier portion is
prepared containing between 2 and 9 % of the total starch content by mixing the starch together with water and
alkali until all the starch has gelatinised.

5. Method according to any one of the claims 1 to 4, characterised in that in the first step, the alkali content in the
35 carrier portion is typically less than 2/3 of the total amount needed in the adhesive formulation.

6. Method according to any one of the claims 1 to 5, characterised in that in the second step the carrier portion is
diluted with a volume of water corresponding to 60 to 85 % of the carrier volume.

40 7. Method according to any one of the claims 1 to 6, characterised in that in the second step 50 to 75 % of the
secondary starch is added.

8. Method according to any one of the preceding claims, characterised in that after the third step borax is added.

45 9. High dry substance Stein Hall adhesive, obtained by a method according to any one of the preceding claims,
characterised in that it contains

- between 32 to 45 % native or stabilised starch;

- the ratio carrier starch to secondary starch is between 1:50 and 1:11;
50 - it shows a Bauer-viscosity between 21s and 60s; and
- the alkali concentration in the glue is sufficient to provide a SGP (starting gel point) of between 45 °C and 53 °C.

10. High dry substance Stein Hall adhesive according to claim 9, characterised in that the native or stabilised starch
is obtained from cereal, tuber or root starches.
55

6
 EP 1 470 202 B1

Patentansprüche

1. Verfahren zur Herstellung eines Stein-Hall Klebstoffes, wobei das Verfahren die folgenden Schritte umfaßt:

5 - Zubereitung eines Trägeranteils durch Gelieren von zumindest einem Anteil der gesamten Stärke im Klebstoff
in einem alkalischen Medium;
- Verdünnen des Trägeranteils mit einer Wassermenge;
- Zugabe der verbliebenen zusätzlichen Stärke;

10 wobei in einem ersten Schritt der Trägeranteil unter Verwendung eines Teils des Alkalis hergestellt wird, und in
einem zweiten Schritt der Trägeranteil mit einer Wassermenge verdünnt wird, gefolgt von der Zugabe zumindest
eines Teils der zusätzlichen Stärke, dadurch gekennzeichnet daß ein Stein-Hall Klebstoff mit hoher Trockensub-
stanz, der zwischen 32 % und 45 % Trockengewicht Stärkefeststoffe enthält, unter Verwendung nur eines Misch-
gefäßes dargestellt wird, wobei im ersten Schritt der Trägeranteil in dem einen Mischgefäß hergestellt wird, und in
15 einem dritten Schritt das verbliebene Alkali in verdünnter Form zusammen mit der zusätzlichen Stärke zugegeben
wird.

2. Verfahren nach Anspruch 1, dadurch gekennzeichnet daß die Zugabe der verbliebenen zusätzlichen Stärke und
des Alkalis schrittweise erfolgt.
20
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet daß die Zugabe von Alkali und Stärke in mindestens zwei
Schritten erfolgt.

4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet daß im ersten Schritt ein Trägeranteil,
25 der zwischen 2 % und 9 % des gesamten Stärkegehalts enthält, hergestellt wird durch Vermischen der Stärke
zusammen mit Wasser und Alkali, bis die Stärke vollständig geliert ist.

5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet daß im ersten Schritt der Alkaligehalt des
Trägeranteils üblicherweise geringer als 2/3 der gesamten in der Klebstofformulierung erforderlichen Menge ist.
30
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet daß im zweiten Schritt der Trägeranteil
mit einer Wassermenge verdünnt wird, die 60 % bis 85 % des Volumens des Trägeranteils entspricht.

7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet daß im zweiten Schritt 50 % bis 75 % der
35 zusätzlichen Stärke zugegeben werden.

8. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet daß nach dem dritten Schritt
Borax zugegeben wird.

40 9. Stein-Hall Klebstoff mit hoher Trockensubstanz, hergestellt nach einem Verfahren gemäß einem der vorhergehenden
Ansprüche, dadurch gekennzeichnet daß er umfaßt

- zwischen 32 % und 45 % native oder stabilisierte Stärke;

- ein Verhältnis von Träger-Stärke zu zusätzlicher Stärke zwischen 1:50 und 1:11;
45 - er eine Bauer-Viskosität zwischen 21 s und 60 s zeigt; und
- die Alkalikonzentration im Klebstoff hinreichend ist, um einen SGP (starting gel point, Start-Gelpunkt) zwischen
45°C und 53°C zu liefern.

10. Stein-Hall Klebstoff mit hoher Trockensubstanz nach Anspruch 9, dadurch gekennzeichnet daß die native oder
50 stabilisierte Stärke aus Getreide-, Knollengewächs- oder Wurzelstärke erhalten worden ist.

Revendications

55 1. Procédé pour préparer un adhésif Stein-Hall, comprenant les étapes consistant à:

- préparer une partie primaire en gélatinant au moins une partie de la totalité de l’amidon dans l’adhésif dans
un milieu alcalin;

7
 EP 1 470 202 B1

- diluer la partie primaire avec un volume d’eau; et

- ajouter l’amidon secondaire restant;

dans lequel, au cours d’une première étape, ladite partie primaire est préparée en utilisant une partie des alcalis,
5 et au cours d’une deuxième étape, la partie primaire est diluée avec un volume d’eau, suivie par l’ajout d’au moins
une partie de l’amidon secondaire,
caractérisé en ce qu’un adhésif Stein-Hall à teneur élevée en matière sèche, contenant entre 32 % et 45 % en
poids à sec de particules solides d’amidon, est préparé en utilisant un récipient de mélange unique, dans lequel,
au cours de la première étape, ladite partie primaire est préparée dans le récipient de mélange unique, et au cours
10 d’une troisième étape, les alcalis restants sont ajoutés sous une forme diluée en même temps que l’amidon secon-
daire.

2. Procédé selon la revendication 1, caractérisé en ce que l’ajout de l’amidon secondaire restant et des alcalis est
effectué par étapes.
15
3. Procédé selon la revendication 2, caractérisé en ce que l’ajout des alcalis et de l’amidon est effectué en au moins
deux étapes.

4. Procédé selon l’une quelconque des revendications 1 à 3, caractérisé en ce que au cours de la première étape,
20 on prépare une partie primaire contenant entre 2 % et 9 % de la teneur totale en amidon en mélangeant l’amidon
avec de l’eau et des alcalis jusqu’à ce que la totalité de l’amidon soit gélatinisée.

5. Procédé selon l’une quelconque des revendications 1 à 4, caractérisé en ce que au cours de la première étape,
la teneur en alcalis dans la partie primaire est typiquement inférieure à 2/3 de la quantité totale nécessaire dans la
25 formulation de l’adhésif.

6. Procédé selon l’une quelconque des revendications 1 à 5, caractérisé en ce que au cours de la deuxième étape,
la partie primaire est diluée avec un volume d’eau correspondant à 60 % à 85 % du volume de la partie primaire.

30 7. Procédé selon l’une quelconque des revendications 1 à 6, caractérisé en ce que 50 % à 75 % de l’amidon secondaire
sont ajoutés au cours de la deuxième étape.

8. Procédé selon l’une quelconque des revendications précédentes, caractérisé en ce que du borax est ajouté après
la troisième étape.
35
9. Adhésif Stein-Hall à teneur élevée en matière sèche obtenu par un procédé selon l’une quelconque des revendi-
cations précédentes, caractérisé en ce que

- il contient entre 32 % et 45 % d’amidon natif ou stabilisé;

40 - le rapport de l’amidon primaire avec l’amidon secondaire est compris entre 1:50 et 1:11;
- il présente une viscosité Bauer comprise entre 21 s et 60 s ; et
- la concentration en alcalis dans la colle est suffisante pour obtenir un SGP (point de début de gélatinisation)
compris entre 45°C et 53°C.

45 10. Adhésif Stein-Hall à teneur élevée en matière sèche selon la revendication 9, caractérisé en ce que l’amidon natif
ou stabilisé est obtenu à partir d’amidons de céréales, de tubercules ou de racines.

50

55