ES2641882T3 - Manufacturing process of an emulsion of succinic alkenyl anhydride - Google Patents

Abstract

Continuous manufacturing process of an emulsion of succinic alkenyl anhydride, hereinafter referred to as ASA, in an aqueous solution of cationic amylaceous matter, performed by means of an emulsification unit (1) comprising an emulsification chamber (2) that receives a rotor torque (3) / stator (4), the process comprising the steps of: a) making an aqueous solution of cationic amylaceous material whose dry matter content is between 7% and 12% of its total weight, b) carrying Separately the ASA and the aqueous solution of cationic starch material from stage a), and feed the emulsification chamber in ASA and in the aqueous solution of cationic starch material from stage a), respectively thanks to two fluid inlets (E1, E2) different, so as not to mix them before their introduction into the emulsification chamber (2), c) mix the ASA and the aqueous solution of cation starch ica from stage a), in the emulsification chamber (2), in order to obtain a dry weight ratio of cationic amylaceous matter / ASA of less than 1, d) to carry out, in a single step, an emulsification unit ( 1), an emulsion from the mixture from stage b), and this without a recirculation loop, e) dilute the emulsion from stage d) in the immediate proximity of the outlet (So) of the emulsification unit (1), of tangential axis of the periphery of the rotor (3), the diameter of the outlet (So) of the emulsification chamber being between 3 mm and 10 mm, the dilution stage being carried out downstream of the outlet of emulsification unit, carrying the undiluted emulsion along a rectilinear path, from the outlet (So) of the emulsification unit (1), and to the dilution site, without change of direction, by a dilution device (8) comprising a straight section (80) of conduit whose proxy end badly it is connected to the outlet (So) of the emulsification unit (1) and whose distal end flows into an elbow (81) of a duct of greater diameter and that channels the dilution liquid, and in which the dilution factor of step e) is between 4 and 21, in order to obtain a minimum fluid velocity in a conduit, downstream to the dilution device, greater than 0.2 m / s.

Description

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DESCRIPTION

Manufacturing process of an emulsion of succinic alkenyl anhydride

The present invention aims at a process for manufacturing an emulsion of succinic alkenyl anhydride (ASA) in an aqueous solution of cationic amylaceous matter, it being understood that the oil phase is constituted by ASA, the solution performing amylacea supporting the function of said emulsion . By aqueous solution of cationic amylacea, a composition is understood which contains at least one cationic starch in aqueous solution.

The procedure described in the present application does not use the product's recirculation loop at the level of the emulsification unit, and makes a dilution of the emulsion once it is manufactured: a product is obtained that has a fine, monodispersed and stable granulometry at the same time over time, and that limits fouling in the ducts that carry the emulsion from the emulsion manufacturing facility to the paper machine. An efficient, simple to perform procedure is thus provided, at a paper production site, which is convenient for manufacturing flows compatible with the needs of paper machines.

The invention also relates to an installation for manufacturing an emulsion that is convenient for carrying out the process.

In the paper and other cardboard sector, the so-called sizing operations are intended to give these supports improved properties, in particular in terms of hydrophobicization, resistance to penetration of hydrophilic species such as water and aqueous inks. In this regard, compositions called "sizing" containing hydrophobic substances are used.

One of the compounds frequently used in sizing compositions is succinic alkenyl anhydride or "ASA" (according to the acronym Anglo-Saxon alkenyl succinic anhydrid). This chemical species that is not miscible in water must be emulsified in order to be used advantageously in the form of a liquid product: this allows a good contact between ASA and the cellulose fibers. The emulsion in question is an emulsion of ASA in an aqueous solution of cationic amylacea; then, in the application, this may also be designated under the simple term of emulsion.

In order to carry out this emulsion, the concomitant use of the aqueous solutions of cationic amylaceous materials of different natures is known, the amylacea material being eventually modified; The function of such compositions is to prevent the coalescence of the ASA particles by positive ionization of the surface of the particles, and to bring the ASA particles closer to the fibers by an ionic mechanism. Widely, a dry weight ratio of cationic amylacea / ASA material between 0.2 and 4 is used.

In addition to the ability to confer improved properties on the final product, the emulsion of ASA in the aqueous solution of cationic amylacea must have a certain number of characteristics. It must present, in particular, a great fineness of particle sizes, as well as a narrow spectrum of distribution of these sizes ("monodispersed" product). As explained in WO 97/35068 A1, these parameters condition the effectiveness of the glue composition against hydrophobic properties that are supposed to confer.

In this regard, it is well known that the presence of "coarse" particles is a source of fouling, in particular of the various materials in which the sizing composition passes, but also of the dryness of the paper machine, by dragging with Vapor from these coarse particles (which can sometimes lead to fires). Conversely, too "fine" particles of said composition will pass through the fibrous bed and will be transported in the process waters during draining. Therefore, it is necessary to have a sizing composition in the form of an emulsion that has a maximum of particles whose diameter is centered in an optimal size that the person skilled in the art estimates between 1 mm and 1.5 mm.

The applicant has recently developed a manufacturing process for an ASA emulsion in a composition of cationic amylacea, which leads to a distribution of particle sizes, narrow and centered over a range between 1 mm and 1.5 mm, and this without the temperature rise of the emulsion, phenomenon that accelerates the hydrolysis of ASA. On this occasion, it has shown that the resulting emulsions effectively confer excellent hydrophobicization properties on the papers in which they are intended to be used.

The key to this procedure is based on a step of emulsifying an ASA / aqueous solution of cationic amylacea in a single step (i.e. no recirculation loop as per prior art), while adjusting the content in dry matter of the initial aqueous solution of cationic amylacea matter between approximately 7% and 12% of its total weight. Such a procedure is taught by document WO2013 / 186491.

However, it seems that the emulsions thus manufactured do not have a stable particle size distribution of the particle sizes. Thus, it has been found that the average diameter of these particles evolved rapidly

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in time, towards values sometimes greater than 4 pm: it therefore departs substantially from the optimum value sought by the papermaker and as defined above, to obtain an effective gluing of the sheet of paper. However, it is not uncommon for the paper machine to stop for several minutes, even several hours, after technical problems, for cleaning or maintenance operations. In this regard, it is essential that the particle size distribution of the emulsion particle sizes does not vary.

Having carried out intensive work in this field, the applicant has managed to improve the procedure object of the aforementioned patent application, in order to alleviate the granulometric derivative observed above. He has found in particular that a stage of dilution of the emulsion substantially improved and very advantageously the stability of the granulometry of said emulsion: specifically, the average diameter of the particles does not evolve practically more in time, in periods that can reach 4 hours. This improvement is subject to the deposit of the application WO2014 / 053788A1.

In WO2013 / 186491 or also in WO2014 / 053788A1, the process of manufacturing an ASA emulsion in an aqueous solution of cationic amylacea is carried out in an installation comprising:

1) a storage unit of an aqueous solution of cationic matter,

2) a mixing unit of ASA and aqueous solution of cationic amylacea, connected with unit 1),

3) an emulsification unit of the mixture of ASA and the aqueous solution of cationic amylacea, connected with unit 2), and without a recirculation loop.

These three units 1), 2) and 3) allow to obtain an emulsion of succinic anhydride (ASA) in an aqueous solution of cationic amylacea as taught by application WO 2013/186491, which has a maximum of particles whose diameter is focused on an optimal size that the expert in the field estimates between 1 pm and 1.5 pm.

The device of WO 2014 / 053788A1 also comprises a unit of dilution of the emulsion connected to the unit of emulsification 3) and which allows to dilute the emulsion, and thus stabilize the granulometry of the emulsion.

In document WO2013 / 186491 or also document WO2014 / 053788A1, the applicant has identified two devices ("emulsification unit") which allows the emulsion to be made from the mixture of ASA and the aqueous solution of cationic amylacea, advantageously without recirculation of the emulsion to the device. These are Process Pilot 2000/4 (IKA®) or Ytron Z (YTRON®) materials.

Industrial scale test:

Desiring to confirm the relevance of this manufacturing process on an industrial scale, the applicant has carried out continuous manufacturing tests of an emulsion of alkenyl succinic anhydride (ASA), in an aqueous solution of cationic amylacea, by means of an emulsification unit , and according to manufacturing flows adapted to the needs of paper machines.

To do this, the applicant has used the Ytron material (YTRON®), the only emulsifying device between the two identified adapted for this industrial application, online.

This test has been carried out on an industrial scale for an uninterrupted time of 27 hours, under the following conditions, substantially close to those of example 2 of FR1259423.

An aqueous solution of cationic amylacea is used, marketed by the ROQUETTE® company under the name of VECTO®SCA 2015. ASA is also used, which is the Chemsize® A180 product marketed by the CHEMEC® company.

The water supply is made from an existing distribution network. The transfers and determinations of ASA and the aqueous solution of cationic amylacea material to the emulsification unit are carried out from its container, by means of ducts and volumetric pumps, whose rotation speeds depend on the desired flow rate setpoints and the relation considered as amylacea material cationic (s) / ASA.

In this case, and in this test, the dry weight ratio of cationic amylacea / ASA is 0.3.

Prior to the mixture of “ASA / aqueous solution of cationic amylacea matter”, the aqueous solution marketed under the name of VECTOR® SCA 2015 is diluted in line in order to obtain an aqueous solution of amylacea material whose dry matter content is 8 % of its total weight.

This aqueous solution of amylacea, of dry matter content of 8%, is mixed in line with ASA to the mixing unit 2). This mixture "aqueous solution of amylacea / ASA" is then transported through a

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conduit to the emulsification unit 3).

It is the Ytron Z (YTRON®) material, previously identified, without a recirculation loop.

This device comprises a carter, whose internal volume forms a substantially cylindrical emulsification chamber, as well as a single rotor / stator pair. Each rotor and each stator have three rows of concentric toothed crowns: the stator and broken crowns are mutually entangled in order to allow a work in shearing of the toothed crowns, during the rotation of the rotor. During this test, the rotational speed of the rotor is adjusted in order to obtain a peripheral speed of the rotor, at the level of toothed crowns, of the order of 31 m / s.

The fluid flow rate to the emulsification unit is approximately 50 1 / h-

The carton of the emulsification unit comprises a single inlet, with a diameter of the order of 2-3 cm for the mixture "aqueous solution of amylacea / ASA material" to be homogenized, and located substantially on the rotor shaft, as well as a single outlet for emulsion of substantially tangential direction to the cylindrical chamber.

At the exit of the emulsification unit, an emulsion is obtained from which the distribution of the particle sizes is centered in a range between 1 pm and 1.5 pm. The peak of the curve is measured at 1.25 pm analyzed from a laser granulometer marketed by the MALVERN® company under the name of Mastersizer® and according to the conditions specified below for the examples.

The emulsion is then diluted in line with a factor 2, ie a diluted emulsion flow rate of approximately 90-100 l / h.

A diluted emulsion is obtained, whose distribution of particle sizes narrows and focuses on a range between 1 pm and 1.5 pm. There is talk of "narrow" distribution of particle sizes, when at least 80% by volume of said particles have a diameter less than 2 pm, and when the average diameter is between 1 pm and 1.5 pm. As taught by WO2014 / 053788 A1, the stability of the emulsion granulometry is improved compared to an undiluted emulsion.

The results are thus satisfactory with regard to the quality of the emulsion and in particular the distribution of the granulometry. The use of the emulsion as a sizing composition gives satisfactory yields in terms of hydrophobicity of the paper.

On the contrary, and unexpectedly, this test on an industrial scale has revealed the production of deposit in a very important quantity, only at the end of a day of production, fouling that clogged and cut the emulsion feed of the paper machine.

Figure 1 illustrates a schematic diagram of the test carried out accompanied by photos of the fouling of the rotor / stator pair, as well as at the exit of the emulsification unit 3).

Figure 2 represents two detail photos of the fouling at the level of the entrance of the emulsification unit,

Figure 3 is a detail photo of the fouling at the exit level of the emulsification unit 3).

In conclusion, the installation tested, and as taught in document WO2013 / 186491 or WO2014 / 053788A1, causes insurmountable fouling problems on an industrial scale, only at the end of a production day and for flows compatible with paper machines .

The method of manufacturing an emulsion, according to the invention, aims to alleviate the fouling problems identified above.

This procedure allows the realization of an emulsion whose distribution of particle sizes narrows and focuses on an interval between 1 gm and 1.5 pm, and this without consequent elevation of the emulsion temperature, a phenomenon that accelerates hydrolysis of ASA.

The manufacturing process according to the invention allows, according to one embodiment, the obtaining of such an emulsion whose granulometry is stabilized in comparison with an undiluted emulsion.

Likewise, a first object of the present invention consists in a continuous manufacturing process of an ASA emulsion in an aqueous solution of cationic amylacea material made by means of an emulsification unit comprising an emulsification chamber that receives a rotor torque / stator, the procedure comprising the following steps:

a) make an aqueous solution of cationic amylacea material whose dry matter content is between 7% and 12% of its total weight,

b) separately carry ASA and the aqueous solution of cationic amylacea material from stage a), and

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feed the emulsification chamber in ASA and in the aqueous solution of cationic amylacea material from stage a), respectively, thanks to two different fluid inlets, so as not to mix them before being introduced into the emulsification chamber,

c) mixing ASA and the aqueous solution of cationic amylacea material from stage a), in the emulsification chamber, in order to obtain a dry weight ratio of cationic amylacea / ASA material of less than 1, preferably between 0.2 and 0.6 and most preferably between 0.25 and 0.5.

d) perform, in a single step, in an emulsification unit, an emulsion from the mixture of step b), without recirculation loop,

e) dilute the emulsion from stage d) in the immediate proximity of the emulsification outlet, of the tangential axis of the periphery of the rotor, the diameter of the emulsification chamber outlet being between 3 mm and 10 mm, being the dilution stage carried out downstream of the emulsification unit outlet, carrying the undiluted emulsion according to a rectilinear path, from the exit of the emulsification unit, and to the dilution site, without change of direction, by means of a device of dilution comprising a straight section of duct whose proximal end is connected to the outlet of the emulsification unit and whose distal end flows into an elbow of a larger diameter duct and channels the dilution liquid,

and in which the dilution factor of step e) is between 4 and 21, in order to obtain a minimum fluid velocity in a conduit, downstream to the dilution device, greater than 0.2 m / s.

The invention also relates to an installation that is convenient for the continuous manufacture of an ASA emulsion in an aqueous solution of cationic amylacea, comprising:

- an emulsification unit comprising an emulsification chamber that receives a rotor / stator pair, without a recirculation loop,

- volumetric pumps and ducts, intended to drive respectively the ASA and an aqueous solution of cationic amylaceous matter according to a specific flow ratio, said ducts being separate and distinct and suitable for feeding the emulsification chamber in ASA and in the aqueous solution of amylacea material, respectively, thanks to two different fluid inlets, so as not to mix them before being introduced into the emulsification chamber,

- a continuous dilution device connected to the outlet of the emulsification unit, with a tangential axis to the periphery of the rotor, the diameter of the emulsification chamber being between 3 mm and 0 mm, said dilution device comprising a straight section of conduit whose proximal end is connected to the outlet of the emulsification unit and whose distal end flows into an elbow of a larger diameter conduit intended to channel the dilution liquid and to allow the routing of the undiluted emulsion according to a rectilinear trajectory, from the exit of the emulsification unit, to the dilution site, without change of direction.

The invention also relates to an assembly comprising a paper machine and an installation for the continuous manufacture of an ASA emulsion in an aqueous solution of cationic amylacea according to the invention and connected to the paper machine.

The invention also relates to a method of gluing a sheet of paper or cardboard in which:

a) an emulsion of succinic alkenyl anhydride, called ASA in an aqueous solution of cationic amylaceous matter is obtained by performing the process of the invention,

b) a sizing composition containing an emulsion manufactured in step a) is used in a sizing operation of a sheet of paper or cardboard.

The invention will be better understood from reading the following description accompanied by the attached drawings, among which:

- Figure 4 is a schematic view of the method according to the invention, according to an embodiment,

- Figure 5 is a view of the emulsification unit of the installation according to the invention, which has three different entrances, respectively for ASA and the aqueous solution of amylaceous cationic matter, as well as for the introduction of a washing solution, being the emulsification unit followed by the dilution device,

- Figure 6 is an exploded view of the emulsification unit / dilution device assembly illustrated in Figure 5,

- Figures 7a, 7b and 7c are, respectively, front perspective, section and rear perspective views of a rotor / stator pair that can be used in the process according to the invention, but which is known as such in the state of the technique,

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- Figures 8a, 8b and 8c are, respectively, front perspective, sectional and rear perspective views of a rotor / stator pair according to the invention, object of an improvement,

- Figure 9a is a schematic view of a pair of an emulsification unit of Ytron Z type (YTRON®) as is known from the state of the art and presenting a unique input for the emulsified mixture,

- Figure 9b is a sectional view of the emulsification unit according to the invention, equipped with the improved rotor / stator pair, the unit presenting two different entrances, for ASA and the aqueous solution of cationic amylaceous matter, of inclined axes with respect to to the rotor shaft (the input for the wash solution is not shown in this figure),

- Figure 10 is a view of an emulsion manufacturing plant comprising two emulsification units, in parallel.

The invention was born from the finding by the inventors that one of the causes of fouling results, according to the prior art of WO2013 / 186491, from the prior mixing, upstream of the emulsification unit, of ASA with the aqueous solution of cationic amylacea matter.

Likewise, and according to a characteristic of the invention (namely step b), the ASA and the aqueous solution of cationic amylaceous matter are not mixed before being introduced into the emulsification chamber 2. In other words, and according to the invention , the mixing of these two components is carried out directly in the emulsification chamber 2, and not in an upstream mixture, other than the emulsification unit as taught by WO 2013/186491.

For this purpose, the emulsification unit 1 has two different inputs E1, E2 for the ASA and the aqueous solution of cationic amylacea and different conduits for routing these two fluids.

According to an embodiment illustrated in Figure 9, these two inputs E1, E2 can be advantageously of inclined axes with respect to the axis A of the rotor 3 such that their jets intersect in the emulsification chamber 2.

The step a) of carrying out the aqueous solution of cationic amylaceous matter consists of either providing an aqueous solution of cationic amylaceous matter, as it is commercially available, or diluting it with water, to obtain the desired dry matter content. This dilution can be done online, in the installation, for example by means of a static mixture. The dilution water is preferably of a temperature between 5 ° C and 40 ° C, and more preferably between 5 ° C and 25 ° C.

For all purposes, it is required that the expression cationic amylacea material designates an amylacea material obtained by any known process of cationization in aqueous medium, in solvent medium or in dry phase, from the moment in which this procedure allows one or more Nitrogenous groups of electropositive nature to be fixed on said amylacea matter. Reference may in particular be made to document WO2005 / 014709 A1.

As examples of aqueous solution of cationic amylaceous materials that can be made according to the present invention, the products marketed under the VECTOR® SC and IC (ROQUETTE®), Raisabond® 15 (CHEMIGATE), Licocat® P ( SUEDSTAERKE®), Lyckeby® LP 2145 and LP 1140 (LYCKEBY®), Redisize® 205 and Redibond® 4000 (NATIONAL STARCH®) and Raifix® 25035 and 01035 (CIBA RAISIO®).

Step c) consists, directly in the emulsification chamber 2, in mixing the aqueous solution of cationic amylacea from stage a) and the ASA. The dry weight ratio of cationic amylacea / ASA is less than 1, preferably between 0.2 and 0.6, and most preferably between 0.25 and 0.5.

For this purpose, the manufacturing facility comprises volumetric pumps (not shown) and ducts, intended to drive the ASA and an aqueous solution of cationic amylacea material according to a given flow ratio in order to obtain the dry matter weight ratio. cationic amylacea / ASA.

Step d) consists in circulating in a single step the mixture that has been obtained in step c), in the emulsification unit 1. This unit comprises the emulsification chamber 2 that receives the rotor 3 / stator pair 4.

The rotor 3 and the stator 4 preferably each have concentric toothed crowns, the crowns of the stator and rotor being mutually entangled. Preferably, each rotor and each stator have several rows of concentric toothed crowns, for example a number of three, as illustrated in the examples in the figures.

In order to limit the heating, the emulsification unit preferably comprises a single rotor 3 / stator 4 pair. According to another alternative (not illustrated), the emulsification unit may comprise several successive levels (for example 3 levels), each presenting a rotor / stator torque

According to the procedure, the rotor 3 of the emulsification unit is preferably driven in rotation in order to

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obtain a peripheral rotor speed, in particular at the level of toothed crowns, between 30 m / s and 40 m / s.

Finally, the dilution stage e) is carried out in the immediate proximity of the So outlet of the emulsification unit 1, and not just upstream of the paper machine. The emulsion is preferably diluted with water.

This dilution step first allows the emulsion to cool at the outlet of the emulsification unit 1, and thus prevent the hydrolysis of the ASA. This dilution also reduces the deposits in the duct downstream of the dilution device, bringing the diluted emulsion from the manufacturing facility to the paper machine, substantially increasing the flow of fluid in the duct.

A minimum fluid velocity is thus sought in this downstream conduit, greater than 0.2 m / s, preferably greater than 0.8 m / s, even greater than or equal to 1 m / s.

On this subject, and to satisfy these speeds and thus the objective of limiting the deposits in the duct, it is necessary to dilute the emulsion of a dilution factor between 4 and 21, and even more preferably between 5 and 15, most preferably between 6 and 11.

Such dilution of a factor strictly greater than 3.5 may be necessary, in particular when the fluid flow rate is between 45 l / h and 300 l / h in the emulsification unit 1, in order to achieve such fluid velocities in the ducts

This dilution factor is higher than that shown in the application WO2014 / 053788A1, of the applicant. Where appropriate, and for strong dilutions, close to the upper limit (for example dilution factor 21), this strong dilution can be carried out to the detriment of the emulsion's stability over time. A dilution factor between 4 and 11 may be a good compromise between the stability of the emulsion and the objective of limiting fouling.

In order to limit the deposits between the emulsification chamber 2 and the dilution site of step e), the fluid outlet So of the emulsification chamber 2 is tangential to the rotor 3 and is of reduced diameter, comprised between 3 mm and 10 mm, such as, for example, 4 mm, 6 mm or 8 mm: an output diameter less than or equal to 10 mm is selected, well below the output diameter of the commercial version Ytron Z (YTRON® ), in order to limit deposits on this area.

In the case of variable flow rates during the manufacturing process, the emulsification unit may comprise a set of removable connectors 7, intended to allow the change of the diameter of the So output. Each connector 7 has its own internal diameter (for example 4 mm, 6 mm or 8 mm). Depending on the needs and operating flow rates, the change in the diameter of the So output is simply obtained by removing a connector 7 and replacing it, for example in a housing of the cylindrical wall 6 of the crankcase, by another connector of more adapted diameter.

For these same reasons of adaptability, the emulsification unit 1 can comprise a set of rotor / stator pairs, different, and which differ in the length of the teeth of the concentric toothed crowns.

For example, and for a fluid flow rate between 45 l / h and 150 l / h to the emulsification unit 1, a stator 4 and a rotor 3 can be selected whose length of the teeth of the toothed crowns is between 4 mm and 6 mm and whose separation between the teeth is between 1 mm and 2 mm. This rotor / stator pair is referred to below as a short-tooth rotor / stator pair.

For a fluid flow rate between 150 l / h and 300 l / h of the emulsification unit 1, a stator 4 and a rotor 3 can be selected, whose teeth length of the toothed crowns is between 9 mm and 12 mm and whose separation between teeth is between 1 mm and 2 mm. This rotor / stator pair is referred to below as the long-tooth rotor / stator pair.

In order to limit the deposits between the outlet So of the emulsification chamber 2 and the dilution stage e), the dilution downstream of the outlet So of the emulsification unit 1 is carried out by means of a dilution device 8 which preferably comprises a straight section 80 of conduit whose proximal end is connected to the outlet So of the emulsification unit 1 and whose distal end flows into an elbow 81 of a larger diameter conduit, channeling the dilution liquid.

The undiluted emulsion is thus directed according to a rectilinear trajectory, from the So output of the emulsification unit 1 and to the dilution site, without change of direction and thus without elbow capable of favoring the deposits. Such dilution device 8 works by venturi effect.

The applicant has also worked on the geometry of the emulsification chamber, in the same deposit limitation objective. In this regard, Figures 7a, 7b and 7c illustrate a rotor / stator pair, as is known from the state of the art, as such. For such a rotor / stator pair, the free interior volume of the emulsification chamber 2, upstream of the shear work (according to the direction of flow), is defined between the walls of the cover and the

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rotor / stator set. As can be seen in the sectional view of Figure 9a which represents an emulsification unit according to the state of the Ytron Z (YTRON®) technique of unique Em input, and due to the geometry of the stator S, it is understood that this volume Free interior is important and extends radially beyond the diameter of the toothed crowns of stator S and rotor R.

As shown in Figure 9b, downstream of the shearing work, according to the direction of flow, the free volume of the emulsification chamber 2 is defined between the rotor 3, the internal surface of the cylindrical wall 6 of the crankcase, and a 5 'cover of the crankcase (opposite to the cover 5 that carries the inputs E1, E2).

The new rotor / stator pair illustrated in Figures 8a, 8b and 8c aims to significantly reduce this free volume of the emulsification chamber, upstream of the shearing work between the toothed crowns. The stator 4 is always positioned between the rotor 3 and said fluid inlets E1, E2 in said emulsification chamber 2.

As shown in FIG. 9b, the geometry of the stator thus modified comprises a reduced central opening 40, of a diameter smaller than the average diameter of the toothed crowns, as well as a wall 41 extending from the central opening 40 to the toothed crowns. from stator 4, widening. This reduced central opening 40 is intended to be traversed by the fluid inlet jets E1, E2.

As can be seen in the sectional view of Figure 9b, this new geometry of the stator 4 makes it possible to substantially reduce the free internal volume of the emulsification chamber 2, upstream of the shearing work, and thus the deposit surfaces. Thus, it can be seen from figure 9b that this free internal volume, upstream, is defined between the widened wall 41 and the rotor 3, and is thus contained, of a diameter smaller than the diameter of the stator crowns of the stator 4.

The emulsification unit 1 may comprise a third fluid inlet, marked as En, other than the inputs E1 and E2, and which allow the completion of a cleaning cycle of the emulsification unit 1, including also the dilution device 8 located downstream of the emulsification unit.

Cleaning is carried out by feeding the inlet of a cleaning fluid such as water, with or without adjuvant, and preferably by driving the rotor from a rotational movement.

In order not to stop the paper machine during the maintenance and cleaning periods of the emulsification unit, the emulsion manufacturing facility can advantageously comprise, as illustrated in Figure 10, two emulsification units 1 , 1 ", the emulsion being produced from the same source of ASA and from the same solution of cationic amylacea, to one of the two emulsification units 1, 1", while the other emulsification unit performs a cycle of cleaning, or undergoes maintenance.

The solenoid valve 9 is a three-way solenoid valve that allows the cationic solution of amylacea to be driven either to the E2 inlet of the first emulsification unit 1, or to the inlet E2 "of the second emulsification unit 1". The solenoid valve 10, is a three-way solenoid valve that allows the ASA to be driven either to the input E1 of the first emulsification unit 1, or to the input E1 "of the second emulsification unit 1".

In operation, these two solenoid valves 9 and 10 lead the ASA and the solution of cationic amylaceous matter either to the entrances of the first emulsification unit 1, or to the entrances of the second emulsification unit 1 ”.

The solenoid valve 11 is a three-way solenoid valve that allows the diluted emulsion from stage e) to be driven to the paper machine through a tube, or from the output of the dilution device 8 associated with the first unit of emulsification 1, or from the output of the dilution device 8 "associated with the second emulsification unit 1".

An automatic device allows to control these three solenoid valves 9, 10 and 11, and synchronize them in order to connect either the first emulsification unit 1, or the second emulsification unit 1 ”.

The method according to the present invention is also characterized in that ASA is a product preferably of synthetic origin; these are modified oils that result from pairs of C16-C18. Among the commercially available and usable ASAs in the present invention, one may cite the Chemsizer® A 180 (CHEMEC®) product or the PENTASIZE® 8A product by the PENTAGON® company which is an equivalent product.

This procedure is also characterized in that the aqueous solution of cationic amylacea has a nitrogen percentage of less than 3.5%, preferably between 0.3% and 3.5%, most preferably between 0.7% and 2% dry weight of nitrogen with respect to the total weight of cationic amylacea.

This cationic amylaceous matter may eventually be modified from an operation selected from hydrolysis, chemical and physical, mechanical, thermomechanical or thermal transformations. A hydrolysis operation, which directly targets the reduction of molecular mass and, in most cases,

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The reduction of viscosity can be carried out by various means such as chemicals, usually by the action of an acid, a base or an oxidizing agent or by an enzymatic action, most commonly by amylase. The usual chemical modifications are of different natures such as oxidation, in particular with hypochlorite, esterification, such as acetylation, etherification, for example by cationization, carboxymethylation or hydroxypropylation. The physical treatments can be carried out by means of thermomechanical means, such as extrusion or pre-gelatinization, or thermal, such as those known to those skilled in the art under the name of Hot Moisture Treatment (HMT) or Annealing.

The following examples allow a better appreciation of the nature of the present invention, without limiting its scope.

Examples

In the tests, the granulometry of the emulsions is analyzed from a laser granulometer marketed by the company MALVERN® under the name of Mastersizer®, with the following parameters:

- 800 ml of demineralized water

- 1900 rpm agitation

- Measurement "background": 10 s

- 3 consecutive measurements per sample (time between measurements: 0 s)

- duration of each measurement 10 s

- laser dimming: between 8% and 13%

- refractive index: 1.5

- dispersant (water) refractive index: 1.33

- Absorption: 0.01

- Particle shape model = spherical Test No. 1 on an industrial scale (reference):

The first reference test is the one that has allowed us to verify the fouling problem, already described here in the introduction, and illustrated schematically in Figure 1.

This is carried out continuously in a duration of 27 hours, under the following conditions, substantially close to those of example 2 of document FR1259423.

An aqueous solution of cationic amylacea is used, marketed by the ROQUETTE® company under the name of VECTOR® SCA 2015. ASA is also used, which is the Chemsize® A 180 product marketed by the CHEMEC® company.

The water supply is made from an existing distribution network. The transfers and dosing of the ASA and the aqueous solution of cationic amylacea material to the emulsification unit are carried out, from its container, by means of a duct and volumetric pumps, whose rotation speeds depend on the desired flow rate setpoints and the proportion considered of cationic (dry) amylacea / ASA.

The dry weight ratio of cationic amylacea / ASA is 0.3.

Prior to the mixture of “ASA / aqueous solution of cationic amylacea matter”, the aqueous solution sold under the name of VECTOR® SCA 2015 is diluted in line in order to obtain an aqueous solution of amylacea material whose dry matter content is 8 % of its total weight.

This aqueous solution of amylacea material, with a dry matter content of 8%, is mixed in line with the ASA in a mixing unit. This mixture "aqueous solution of ASA amylacea" is then transported through a conduit to the emulsification unit.

It is the Ytron Z (YTRON®) material, previously identified, without a recirculation loop.

This device comprises a carter, whose internal volume forms a substantially cylindrical emulsification chamber, as well as a single rotor / stator pair. Each rotor and each stator has three rows of concentric toothed crowns: the stator and rotor crowns are mutually entangled in order to allow shearing work. During this test, the rotational speed of the rotor is adjusted in order to obtain a peripheral speed of the rotor, at the level of toothed crowns, of the order of 31 m / s.

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Four. Five

The fluid flow rate of the emulsification unit is approximately 50 1 / h.

The carton of the emulsification unit comprises a single inlet, with a diameter of the order of 3-4 cm for the mixture "aqueous solution of amylacea / ASA material" to be homogenized, located substantially on the rotor shaft, as well as a single outlet for the emulsion of substantially tangential direction to the cylindrical chamber and of the diameter of the order of 2-3 cm.

The emulsion is then diluted in line with a factor 2, ie a diluted emulsion flow rate of approximately 100 l / h. The dilute water temperature is 382C.

At the exit of the emulsification unit, an emulsion is obtained, whose distribution of particle sizes narrows and focuses on a range between 1 pm and 1.5 pm. The peak of the curve (volume of the particles in% / diameter in pm) measured by the granulometer is at 1.25 pm.

At the end of a production day, however, important fouling is found in:

- the feeding duct of the emulsification unit,

- the entry of the ASA emulsification unit and the solution of cationic amylacea, as illustrated in Figure 2,

- the emulsion chamber and in particular on the rotor, as illustrated in figure 1 (visible in the photo on the left),

- the output of the emulsification unit as illustrated in figure 1 (visible in the photo in the center) and in figure 3,

- the conduit downstream of the device that carries out the dilution and routes the diluted emulsion to the paper machine, as illustrated in figure 1 (visible in the photo on the right).

Test n ° 2 on an industrial scale (invention):

In order to alleviate these fouling problems, modifications have been made to the manufacturing process and the installation that allows its use.

A first substantial modification consists, according to steps b) and c) of the process according to the invention, mixing the ASA and the amyloaceous cationic solution from stage a) directly in the emulsification chamber of the emulsification unit, and not in a upstream mixing unit. The modified installation thus comprises separate ducts and different inlets for ASA and the solution of amylacea cationic matter.

A second substantial modification consists, according to step e) of the process, in diluting the emulsion more strongly, in order to increase the fluid velocity in the duct downstream of the dilution device. In this test, the dilution factor goes from 2 to 6.

On the other hand, an outlet for the smallest diameter emulsification unit (8 mm) and a dilution device 8 as described above are used.

A rotor / stator pair of short teeth is used as defined above.

The products used are the same as for test n ° 1: an aqueous solution of cationic amylacea is used, marketed by the ROQUETTE® company under the name of VECTOR® SCA 2015. ASA is also used, which is the Chemsize® product A180 marketed by the CHEMEC® company.

Thus, the conditions of this test n ° 2 are the following:

- dry matter content of the aqueous solution of cationic amylacea, according to step a) of the procedure: 8%

- relation in dry weight cationic amylacea / ASA matter, according to step c) of the procedure: 0.25

- flow rate in the emulsification unit: 49.5 l / h

- dilution factor according to step e) of the procedure: 6 (5 x the volume of the emulsion),

- peripheral rotor speed: approximately 31 m / s (4600 rpm),

- diluted emulsion temperature: 29 ° C

After the modifications made, there is a very clear improvement in terms of fouling, in the end

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of a production day, namely:

- no fouling at the level of the feeding ducts and the inlets of the emulsification unit,

- no fouling at the level of the emulsification chamber,

- no fouling at the level of the output of the emulsification unit,

- no fouling after stage e), in the downstream duct.

Diluted emulsion extraction is performed: the peak of the particle distribution curve (particle volume in% / diameter in pm) measured by the granulometer is at 1.30 pm.

Test n ° 3 on an industrial scale (invention):

The conditions of test n ° 3 differ from those of test n ° 2 by the flow rate to the emulsion unit which is 190 l / h, as well as by the dry weight ratio of cationic amylacea / ASA material that is slightly different, equal to 0.3.

The installation is the modified test No. 2: the "short teeth" rotor / stator pair is replaced by a "long teeth" rotor / stator.

The conditions of this test n ° 3 are the following:

- dry matter content of the aqueous solution of cationic amylacea, according to step a) of the procedure: 8%

- relation in dry weight cationic amylacea / ASA matter, according to step c) of the procedure: 0.3

- flow rate in the emulsification unit: 190 l / h

- dilution factor according to step e) of the procedure: 6 (5 x the volume of the emulsion),

- peripheral rotor speed: approximately 31 m / s (4600 rpm)

- diluted emulsion temperature: 24 ° C

As in trial 2, the fouling problems are solved.

Diluted emulsion extraction is performed: the peak of the particle distribution curve (particle volume in% / diameter in pm) measured by the particle size meter is at 1.38 pm.

Test No. 4 on an industrial scale (Invention):

The conditions of test No. 4 differ from those of test No. 3 only by the flow rate of the emulsification unit which is 300 l / h.

The conditions of this test n ° 4 are the following:

- dry matter content of the aqueous solution of cationic amylacea, according to step a) of the procedure: 8%

- relation in dry weight cationic amylacea / ASA matter, according to step c) of the procedure: 0.3

- flow rate in the emulsification unit: 300 l / h

- dilution factor according to step e) of the procedure: 6 (5 x the volume of the emulsion)

- peripheral rotor speed: approximately 31 m / s (4600 rpm)

- diluted emulsion temperature: 26 ° C

As in test n ° 2 and test n ° 3, the fouling problems are solved.

Diluted emulsion extraction is performed: the peak of the distribution curve of the particle sizes (in volume of the particles in% / diameter in pm) measured by the granulometer is at 1.49 pm.

Test No. 5 on an industrial scale (Invention):

The conditions of test # 5 differ from those of test # 4 only by the rotor speed of the emulsification unit which is 5700 rpm.

The conditions of this test n ° 5 are the following:

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- dry matter content of the aqueous solution of cationic amylacea, according to step a) of the procedure: 8%

- relation in dry weight cationic amylacea / ASA matter, according to step c) of the procedure: 0.3

- flow rate in the emulsification unit: 300 l / h

- dilution factor according to step e) of the procedure: 6 (5 x the volume of the emulsion)

- peripheral rotor speed: approximately 38 m / s (5700 rpm)

- diluted emulsion temperature: 21 ° C.

As in trials n ° 2, n ° 3 and n ° 4, the fouling problems are solved.

Diluted emulsion extraction is performed: the peak of the distribution curve of the particle sizes (in volume of the particles in% / diameter in pm) measured by the granulometer is at 1.39 pm.

The three tests n ° 2, 3, 4 and 5, on an industrial scale, confirm the relevance of the emulsion manufacturing process. The granulometries of the emulsions obtained are satisfactory, advantageously free of any disastrous phenomenon of hydrolysis of the ASA, and obtained without the problems of fouling of the installation found for test No. 1.

Table 1

 Test No.

 1 2 3 4 5

 % of dry matter from stage a)

 8 8 8 8 8

 Relationship of stage c)

 0.3 0.25 0.3 0.3 0.3

 Emulsification unit flow rate (l / h)

 50 49.5 190 300 300

 Dilution factor of stage e)

 2 6 6 6 6

 Rotor speed (rpm)

 4600 4600 4600 4600 5700

 Peripheral rotor speed (m / s)

 31 31 31 31 38

 Peak distribution curve (pm)

 1.25 1.30 1.38 1.49 1.39

 Dirting (at 24h)

 yes no no no no

The results of the different tests on an industrial scale are gathered in Table 1, above. The modifications made have allowed to solve the problems of fouling while preserving the qualities of the emulsion, as a sizing agent. It should be noted that for these tests on an industrial scale, a single value for the dilution factor (equal to 6) has been tested. No stronger dilutions have been tested, mainly in order to avoid the creation of an excessively large volume of effluents to be treated.

The applicant knows, however, that a stronger dilution would be even more favorable, in regard to the problems of fouling in the downstream conduit, directing the emulsion to the paper machine, because even more fluid velocities would be obtained. important in this duct.

The following laboratory tests demonstrate on the other hand that a stronger dilution, at least up to a dilution factor equal to 21, does not affect the quality of the emulsion as a sizing agent.

Laboratory tests:

In this example, an ASA emulsion is performed in the laboratory in an aqueous solution of cationic amylaceous matter and the emulsion is diluted according to three different dilution factors, namely 6, 11 and 21, in order to obtain three diluted emulsions, called "emulsion 1", "emulsion 2" and "emulsion 3".

The yields of these three diluted emulsions are then tested as a sizing agent to determine the influence of the dilution factor.

An aqueous solution of cationic amylacea is used, marketed by the ROQUETTE® company under the name of VECTOR® SCA 2015. ASA is also used, which is the Chemsize® A 180 product marketed by the CHEMEC® company.

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The aqueous solution marketed under the name of VECTOR® SCA 2015 is diluted in order to obtain an aqueous solution of amylacea material whose dry matter content is 8% of its total weight.

This aqueous solution is mixed with the ASA. The dry weight ratio of cationic amylacea / ASA is 0.3. This mixture is then transferred into a device that allows an emulsion to be obtained.

Three samples of this emulsion are diluted with water, respectively in ratios (emulsion / water) of 1/5, 1/10 and 1/20. The diluted emulsion of a 1/5 ratio (of a dilution factor 6) is called "emulsion 1". The diluted emulsion of a 1/10 ratio (of a dilution factor 11) is called "emulsion 2". The diluted emulsion of a 1/20 ratio (of a dilution factor 21) is called "emulsion 3-.

Afterwards, some sheets of laboratory paper are made from these three emulsions and the degree of hydrophobicity is measured (Cobb 60).

Specifically, these sheets of laboratory paper, also called test sheets, are manufactured from a FRET device (retention test sheets) marketed by the TECHPAP company. Such test sheets have characteristics similar to those of the client industrial paper, in particular as regards flocculation and retention.

The test sheet manufacturing process uses a paper pulp that is a virgin fiber pulp (50% resinous, 50% leafy) with a refining level of 35 ° Shopper (° SR). 35% (in dry weight with respect to the total weight of the paste) of natural calcium carbonate sold by the OMYA® company under the name of Omyalite® 50 are added. The charged fibrous suspension has a concentration of 2.5 g / l. Then 0.3% (dry equivalent / paper) of a HICAT® 5163 AM (ROQUETTE®) glue is added. Three samples of pasta thus extracted are extracted.

0.35% (with respect to paper) of the emulsion 1 is added to the first paste sample. Thus, a first test sheet having a grammage of 70 g / m2 is made.

0.35% (with respect to paper) of the emulsion 2 is added to the second paste sample. Thus, a first test sheet having a weight of 70 g / m2 is made.

0.35% (with respect to paper) of the emulsion 3 is added to the third paste sample. Thus, a first test sheet having a weight of 70 g / m2 is made.

After the manufacture of the test sheets, these are placed between 2 blotting papers and the assembly is passed twice through a TECHPAP® brand roller press. Each test sheet is separated after the drying papers and placed in a TECHPAP® brand dryer, for 5 minutes at 100 ° C. Then, the test sheets are matured, placing them for 30 minutes in an oven at 110 ° C, to allow the sizing agent to fully confer on the paper its hydrophobic character. The test sheets are placed after a minimum of 24 hours in a room set at 23 ° C (+/- 1 ° C) and 50% relative humidity (+/- 2%) (ISO 187: 1990 and Tappi standards T402 sp-08).

A measurement of Cobb 60 (ISO 535: 1991 and Tappi T441 om-04) is then carried out for each test sheet, which is relative to the hydrophobicity of the paper: the lower the amount of water absorbed, the more hydrophobic the paper will be .

Table 2 summarizes the Cobb 60 (g / m2) values measured on test sheets prepared with these three emulsions.

Table 2

 Emulsion No.

 Dilution factor Cobb 60 (g / m2)

 one

 6 20

 2

 11 20

 3

 21 18.5

This table shows that a dilution factor of up to 21 does not lead to a significant loss of the degree of hydrophobicity.

Nomenclature

Invention (Figures 4, 5, 6, 8a, 8b, 8c, 9b and 10):

eleven". Emulsification units,

2. Emulsification chamber,

3. Rotor,

4. Stator,

5 5. Inlet cover (Carter),

5'. Back cover (Carter),

6. Cylindrical wall (Carter),

7. Removable connector,

8. 8 ”. Dilution devices,

10 9, 10, 11. Solenoid valves,

40. Central opening (Stator 4),

41. Widened wall (Stator 4),

80. Straight section duct (Dilution device),

81. Elbow (Dilution device),

15 A. Rotor shaft,

E1, E2, E1 ”, E2”. Different inputs (emulsification unit),

In in". Inputs for cleaning fluid (emulsification unit), So. Output (emulsification chamber 2).

State of the art (figure 9a):

20 Em. Mix input,

R. Rotor,

5. Stator

Claims (15)

5 10 fifteen twenty 25 30 35 40 Four. Five fifty 1. Continuous manufacturing process of an emulsion of succinic alkenyl anhydride, hereinafter referred to as ASA, in an aqueous solution of cationic amylacea, carried out by means of an emulsification unit (1) comprising an emulsification chamber (2) that receives a rotor (3) / stator (4) pair, the process comprising the steps of: a) make an aqueous solution of cationic amylacea material whose dry matter content is between 7% and 12% of its total weight, b) separately carry the ASA and the aqueous solution of cationic amylacea material from stage a), and feed the emulsification chamber in ASA and in the aqueous solution of cationic amylacea material from stage a), respectively thanks to two different fluid inlets (E1, E2), so as not to mix them before they are introduced into the emulsification chamber (2), c) mixing the ASA and the aqueous solution of cationic amylacea material from stage a), in the emulsification chamber (2), in order to obtain a dry weight ratio of cationic amylacea / ASA material less than 1, d) perform, in a single step, in an emulsification unit (1), an emulsion from the mixture from stage b), and this without a recirculation loop, e) dilute the emulsion from stage d) in the immediate proximity of the outlet (So) of the emulsification unit (1), with a tangential axis of the periphery of the rotor (3), with the outlet diameter (So ) of the emulsification chamber between 3 mm and 10 mm, the dilution stage being carried out downstream of the emulsification unit outlet, carrying the undiluted emulsion according to a rectilinear path, from the outlet (So) of the unit of emulsification (1), and until the dilution site, without change of direction, by means of a dilution device (8) comprising a straight section (80) of conduit whose proximal end is connected to the output (So) of the unit of emulsification (1) and whose distal end flows into an elbow (81) of a duct of greater diameter and which channels the dilution liquid, and in which the dilution factor of step e) is between 4 and 21, in order to obtain a minimum fluid velocity in a conduit, downstream to the dilution device, greater than 0.2 m / s. 2. The method according to claim 1, wherein the flow rates of the ASA and the aqueous solution of amylacea material from step a) are determined in order to obtain a fluid flow rate between 45 l / h and 300 l / h in the emulsification unit (1). 3. Method according to claim 1 or 2, wherein the dilution factor of step e) is between 5 and 15. Method according to one of claims 1 to 3, in which, for the emulsification unit (1), an emulsification unit having a single rotor (3) / stator pair (4) is selected and wherein select, for the rotor (3) / stator (4) pair, a rotor (3) and a stator (4) each having concentric serrated crowns, the stator and rotor crowns being mutually entangled. 5. Procedure according to claim 4, wherein: - for a fluid flow rate between 45 l / h and 150 l / h of the emulsification unit, a stator (4) and a rotor (3) are selected whose teeth length of the toothed crowns is between 4 mm and 6 mm and whose spacing between teeth is between 1 mm and 2 mm, - for a fluid flow rate between 150 l / h and 300 l / h of the emulsification unit, a stator (4) and a rotor (3) are selected whose teeth length of the toothed crowns is between 9 mm and 12 mm and whose separation between teeth is between 1 mm and 2 mm. 6. Method according to one of claims 1 to 5, wherein the dilution factor of step e) is comprised between 4 and 21, in order to obtain a minimum fluid velocity in the conduit downstream of the dilution device, greater than 1 m / s. 7. Method according to one of claims 1 to 6, wherein the dilution factor of step e) is between 4 and 11. 8. Installation which is suitable for the continuous manufacture of an emulsion of succinic alkenyl anhydride referred to below as ASA in an aqueous solution of cationic amylacea, comprising: - an emulsification unit (1) comprising an emulsification chamber (2) that receives a rotor (3) / stator pair (4), without a recirculation loop, - volumetric pumps and ducts, intended to drive the ASA and a solution respectively 5 10 fifteen twenty 25 30 35 aqueous of cationic amylaceous matter according to a determined flow ratio, said ducts being separate and distinct and suitable for feeding the emulsification chamber in ASA and in the aqueous solution of amylacea material, respectively thanks to two fluid inlets (E1, E2), different, so as not to mix them before their introduction into the emulsification chamber (2), - a continuous dilution device (8) connected to the outlet (So) of the emulsification unit (1), the tangential shaft output being to the periphery of the rotor (3), the output diameter (So) being of the emulsification chamber between 3 mm and 0 mm, said dilution device comprising a straight section (80) of conduit whose proximal end is connected to the outlet (So) of the emulsification unit (1) and whose distal end flows in an elbow (81) of a larger diameter conduit intended to channel the dilution liquid and to allow the routing of the undiluted emulsion according to a rectilinear path, from the outlet (So) of the emulsification unit (1), to the dilution site, without change of address. 9. Manufacturing installation according to claim 8, wherein the emulsification unit (1) has a single rotor (3) / stator (4) pair and in which the rotor (3) and stator (4) each have one is a concentric toothed crowns, the crowns of the stator and rotor being mutually entangled. 10. Installation according to claim 9, wherein the stator (4) is positioned between the rotor (3) and said fluid inlets (E1, E2) in said emulsification chamber, the stator (4) comprising a central opening (4) 40), of a diameter smaller than the average diameter of the toothed crowns, the central opening (40) being intended to be crossed by the jets of the fluid inlets (E1, E2), as well as a wall (41) extending from the central opening (40) to the stator crowns, widening. 11. Installation according to one of claims 8 to 10, wherein the axes of the fluid inlets (E1, E2) are inclined with respect to the axis (A) of the rotor, such that their jets cross, in the emulsification chamber (2). 12. Installation according to one of claims 8 to 11, wherein the emulsification unit comprises a set of removable connectors 7, intended to allow the change in diameter of the So. 13. Installation of manufacture of the emulsion according to one of claims 8 to 12, comprising two emulsification units (1, 1 "), in parallel, as well as a set of solenoid valves (9, 10, 11) that allows the emulsion, from the same source of ASA and from the same solution of cationic amylacea, to one of the two emulsification units (1, 1 ”) while the other emulsification unit performs a cleaning cycle. 14. An assembly comprising a paper machine and a continuous manufacturing installation of an ASA emulsion in an aqueous solution of cationic amylacea according to one of claims 8 to 13 and connected to the paper machine. 15. Method of gluing a sheet of paper or cardboard in which: a) an emulsion of succinic alkenyl anhydride, called ASA in an aqueous solution of cationic amylaceous matter is obtained by performing the process according to one of claims 1 to 7, b) a sizing composition containing an emulsion manufactured in step a) is used in a sizing operation of a sheet of paper or cardboard.