PRETREATMENT PROCEDURES TO IMPROVE THE FILLING OF A CHAMBER WITH SOLID PARTICLES

Description

FIELD OF INVENTION

[0001] The invention relates to the field of reactor filling with solid particles. More particularly, the invention relates to the loading of fixed-bed reactors of the chemical, electrochemical, petroleum, or petrochemical type with solid particles in a divided state. These particles may be in the form of spheres, grains, cylinders, pellets, rods, or any other shape, but are generally of relatively small dimensions. The particles may, in particular, be adsorbents, molecular sieves, or solid catalyst grains, generally extruded, manufactured either in an irregular shape or as single- or multi-lobed rods, the dimensions of which vary, depending on the case, from a few tenths of a millimeter to a few centimeters. EARLIER ART

[0002] Most industrial transformation or separation processes involve the use of a solid in a reactor. The performance of these processes is generally directly proportional to the number of active or adsorption sites present in the reactor. It is therefore desirable to load the reactor as densely as possible. Those skilled in the art are familiar, for example, with "sock loading," which consists of manually pouring the solid particles using a flexible conduit, called a "sleeve" or "sock" (from the English "sock loading"). High-density loading techniques also exist, such as the high-density loading technique described in French patent application FR2721900 A1 Catapac™, which allows for a loading density at least 10% higher than that of sock loading.

[0003] WO 2006 / 094766 A1 discloses a pretreatment process to improve the filling of a catalytic reactor with solid catalyst particles.

[0004] Solid lubricants have long been used in the pharmaceutical, cosmetic, food processing, and petrochemical industries (PVC, etc.) to improve the flowability of powder mixtures, a critical property for many processes. For example, in the pharmaceutical industry, granules must pass through a feed hopper before reaching the mold that will shape them into tablets. The flow through this hopper must be as smooth as possible to ensure tablets with homogeneous masses. To achieve this, almost all pharmaceutical processes incorporate a preliminary step of mixing the granules with a lubricant.

[0005] The increased flowability of the powders is made possible by the lubricant, which spreads across the surface of the granules. Due to the presence of a lubricant film formed on the surface, the distance between the granules increases, initially reducing the inter-particle adhesion forces.

[0006] However, when the amount of lubricant increases excessively, aggregates form on the surface, increasing surface roughness and creating friction between particles. The opposite effect to that desired is then observed: the adhesion force increases.

[0007] Therefore, there is an optimum which is a function of the size of the solid particles and their nature, because these parameters control the inter-particle adhesion forces.

[0008] Industrial lubricants are generally composed of long carbon chains (at least 14 carbon atoms) associated with a functional group at the end of the chain such as carboxylic acid (-COOH), their associated salts (-COO-Na+), alcohol (-OH) or ester (-COOR).

[0009] The most commonly used lubricant is magnesium stearate, the formula of which is explained by the figure 1 whose biocompatibility is useful in pharmaceutical tablets, food and cosmetics.

[0010] These lubricants are typically added to powder mixtures with a solid-solid mixing step. This type of mixing is far from trivial and is a crucial step in achieving the desired performance. The lubricant must be evenly distributed across the surface, without forming aggregates, to effectively reduce inter-particle adhesion forces.

[0011] For reactor filling, catalysts or adsorbents in solid particle form have so far been transported to the site in large bags or drums. As mentioned previously, there are several loading methods, the main ones being: Manual loading, of the Sock type, involves manually transferring solid particles, for example, using a sleeve or flexible conduit. Loading using a device internal to the chamber, such as Catapac™ described in patent FR2721900, allows for loading at least 10% denser and more homogeneous than Sock loading. This loading technique relies, in particular, on the insertion and / or removal of a functional device within the chamber during the loading process, thanks to the hollow configuration of a rotating shaft.The introduced device is a device comprising, at its upper part, a means for supplying particles and, at its base located inside the enclosure to be loaded, a dispersion system attached to a central shaft driven in rotation around a substantially vertical axis by a motor, and a supply conduit surrounding at least partially the central shaft, said central shaft being a tube of sufficient internal diameter to allow to be carried out in the area to be loaded, via this tube and during the loading period, a number of operations related or complementary to said loading operation, this device comprising a fixed tube attached to the supply conduit and placed inside said rotating central shaft, the fixed tube and said rotating central shaft being substantially coaxial.

[0012] However, there remains a need for improvement in the techniques of filling reactors with solid particles in order to improve the performance of the processes implemented in these reactors.

[0013] Surprisingly, it has been discovered that, under certain conditions, adding a lubricant to solid particles leads to an increase in reactor filling densities. The invention thus proposes a pretreatment process that is applied upstream of loading, whether it be manual "Sock" loading or high-density loading, and which improves reactor filling. SUBJECT OF THE INVENTION

[0014] The invention relates to a pretreatment method for improving the filling of a chamber with solid particles. The chamber can be any adsorbent requiring a dense loading of solid particles of absorbents, known to those skilled in the art. SUMMARY OF THE INVENTION

[0015] The invention relates to a pretreatment process for zeolite X-type adsorbent particles for xylene separation, to improve the filling of a chamber with said solid particles, characterized in that said solid particles are mixed before loading said solid particles into the chamber with at least one lubricant which is solid at room temperature and selected from saturated fatty acids having 14 or more carbon atoms, metallic salts of saturated fatty acids having 14 or more carbon atoms, esters of fatty acids having 14 or more carbon atoms, fatty alcohols having 14 or more carbon atoms, linear N-alkanes having 16 or more carbon atoms in solid form, fumaric acid, talc, sodium stearoyl fumarate, the lubricant being introduced at a content of between 0.01 and 1% relative to the total weight of the mixture of solid particles and lubricant,loading is carried out manually using a flexible conduit or a functional device internal to the enclosure that can be inserted into and / or removed from said enclosure.

[0016] The invention relates to a pretreatment process for improving the filling of a chamber with solid particles, in which said solid particles are mixed before loading said solid particles into the chamber with at least one solid lubricant at room temperature selected from saturated fatty acids having 14 or more carbon atoms, metallic salts of saturated fatty acids having 14 or more carbon atoms, esters of fatty acids having 14 or more carbon atoms, fatty alcohols having 14 or more carbon atoms, linear N-alkanes having 16 or more carbon atoms in solid form, fumaric acid, talc, sodium stearoyl fumarate, the lubricant being introduced at a content of between 0.01 and 1% relative to the total weight of the mixture of solid particles and lubricant.

[0017] In one embodiment, the loading is done manually using a flexible conduit.

[0018] In another embodiment, the loading is carried out using a functional device internal to the enclosure which can be inserted into and / or removed from said enclosure.

[0019] Preferably, said internal functional device comprises, at its upper part, a means for feeding particles and, at its base located inside the enclosure to be loaded, a dispersion system attached to a central shaft driven in rotation around a substantially vertical axis by a motor means, and a feed duct surrounding at least partially the central shaft, said central shaft is a tube of sufficient internal diameter to allow to be carried out in the area to be loaded, via this tube and during the loading period, a number of operations related or complementary to said loading operation, this device comprising a fixed tube attached to the feed duct and placed inside said rotating central shaft, the fixed tube and said rotating central shaft being substantially coaxial.

[0020] Preferably, the lubricant content is between 0.01 and 0.5% by weight, most preferably between 0.05 and 0.25% by weight.

[0021] Preferably, the lubricant is a fatty acid selected from myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, lignoceric acid, cerotic acid, or a metallic salt of saturated fatty acids having 14 or more carbon atoms, selected from aluminum, calcium, magnesium, zinc, sodium, barium, or lithium salts; a fatty alcohol having 14 or more carbon atoms selected from myristyl alcohol, palmitic alcohol, or stearyl alcohol; a paraffin having 16 or more carbon atoms; or an ester of saturated fatty acids having 14 or more carbon atoms selected from the following compounds: glyceryl monostearate, glyceryl distearate, glyceryl monopalmitate, glyceryl dipalmitate, glycerol tristearate, or glyceryl tripalmitate. glycerol, glycerol trimyristate, glycerol tribenhenate.

[0022] Preferably, the lubricant is chosen from magnesium stearate, calcium stearate, and barium stearate.

[0023] Preferably, the lubricant is magnesium stearate. Advantageously, the solid particles are catalyst particles or adsorbent particles.

[0024] Solid particles can be in the form of beads or extrudates.

[0025] Preferably, the equivalent diameter of the solid particles is less than 2 mm.

[0026] Advantageously, the lubricant particles used have a particle size such that at least 90% by mass of the lubricant particles pass through a 90 µm sieve. Preferably, the mixing is carried out at ambient temperature and atmospheric pressure in a drum-type mixer.

[0027] Preferably, the mixing is carried out with a rotation speed between 5 and 30 rpm, for a duration between 5 min and 20 min, and with a filling level in the mixer tank between 30% and 80%.

[0028] Preferably, the enclosure is a chemical or electrochemical, petroleum or petrochemical type reactor. LIST OF FIGURES

[0029] THE figures 1 to 6 illustrate the invention by way of non-limiting example. There figure 1 represents the expanded chemical formula of magnesium stearate. figure 2 represents an industrial drum mixer. The Figures 3A, 3B, 3C relate to example 1 and represent the evolution of the packed density in kg of dry adsorbent / m³ with respect to the lubricant content in % weight relative to the total weight of the mixture, for three types of lubricants: calcium stearate, magnesium stearate and barium stearate. Figures 4A and 4Brelate to example 1 and represent the evolution of the density added in kg of dry adsorbent / m³ with respect to the lubricant content in % weight relative to the total weight of the mixture, for two types of lubricants: magnesium stearate and barium stearate. figure 5 refers to example 1 and represents the water absorption in grams of a sample of adsorbent pretreated with magnesium stearate according to the invention, as a function of the lubricant content in % weight relative to the total weight of the mixture. Figures 6A (comparative) and 6B (according to the invention) relate to Example 1 and illustrate the anti-adherent properties of an adsorbent pretreated with the process according to the invention. DETAILED DESCRIPTION OF THE INVENTION

[0030] The ranges of values ​​are understood to include the limits unless otherwise stated.

[0031] The pretreatment process according to the invention consists of mixing the solid particles (for example, in the form of beads or extrudates) with a solid lubricant at room temperature before loading the particles into the reaction vessel in order to further densify the particle beds. Without being bound by any particular theory, it appears that the lubricant, if introduced under the appropriate conditions, reduces the inter-particle adhesion forces, leading to better filling. The observed effect is attributed to the fact that reactor filling is governed by the same physical phenomenon that increases flowability, namely the adhesion force between particles. Indeed, when the adhesion force is low compared to the gravitational force acting on the particle, the solid particle settles easily, and the filling is of good quality.Conversely, when the adhesion force is greater than gravity, the solid particle tends to agglomerate with its neighbors, creating empty spaces and poor quality filling.

[0032] According to the invention, the proposed pretreatment process improves the filling of a reactor with solid particles by mixing the solid particles (e.g., beads or extrudates) with a solid lubricant at ambient temperature before the loading step (manual or using a functional device). The lubricant surrounding the solid particles is then removed from the process during the start-up of the process implemented in the reactor.

[0033] On an industrial scale, the pretreatment process according to the invention can be carried out at two points: either on-site, just before loading into the reactor, or at the end of the solid adsorbent particle preparation process, once shaping is complete and before shipping the particles to the site. The second embodiment can reduce transport costs due to improved particle compaction in the bags and avoids complicating start-up procedures.

[0034] The lubricant used in the pretreatment process according to the invention is solid at room temperature and is selected from the following compounds: Saturated fatty acids having 14 or more carbon atoms; metallic salts of saturated fatty acids having 14 or more carbon atoms; esters of fatty acids having 14 or more carbon atoms; fatty alcohols having 14 or more carbon atoms; linear N-alkanes (paraffins) having 16 or more carbon atoms, in solid form. Other compounds such as fumaric acid, talc, and sodium stearoyl fumarate.

[0035] Preferably: Saturated fatty acids with 14 or more carbon atoms are selected from myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, lignoceric acid, and cerotic acid. Metallic salts of saturated fatty acids with 14 or more carbon atoms are selected from, among others, salts based on aluminum, calcium, magnesium, zinc, sodium, barium, lithium, etc. Fatty alcohols with 14 or more carbon atoms are selected from the following alcohols: myristyl alcohol, palmitic alcohol, and stearyl alcohol. Linear N-alkanes are paraffins with 16 or more carbon atoms, in solid form. Saturated fatty acid esters having 14 or more carbon atoms are selected from the following compounds: glycerol monostearate, glycerol distearate, glycerol monopalmitate, glycerol dipalmitate, glycerol tristearate, glycerol tripalmitate, glycerol trimyristate, glycerol tribenhenate.

[0036] Among the preferred lubricating compounds according to the invention, magnesium stearate, calcium stearate, and barium stearate salts are preferred. Magnesium stearate ( Figure 1 ).

[0037] The above lubricants can be used alone or in mixtures.

[0038] The lubricant used in the pretreatment process according to the invention advantageously has a fine particle size, and preferably at least 90% by mass of the sample must be able to pass through a 90 µm sieve. More specifically, the lubricant's particle size is such that the size of the lubricant particles is less than 90 µm. The chosen particle size allows for an optimal distance between the solid particles.

[0039] The solid adsorbent particles to be loaded into the chamber preferably have an equivalent diameter of less than 2mm.

[0040] Preferably, said solid particles are substantially spherical.

[0041] The mass concentration of lubricant in the mixture formed by the lubricant and solid particles must be appropriate to achieve the desired effect. In the case of an excessive lubricant concentration, the lubricant particles form aggregates on the surface of the particles, leading to excessively large distances and a loss of the desired effect. Scanning electron microscopy shows that the particle surface is completely coated with lubricant starting at 1% by mass, and that aggregates form beyond this concentration.

[0042] The mass content of lubricant in the mixture formed by the lubricant and the solid particles is between 0.01% and 1% by weight, preferably between 0.01% and 0.5% by weight, more preferably between 0.01% and 0.25% by weight, inclusive, relative to the total weight of the mixture formed by the lubricant and the solid particles.

[0043] The mixing is advantageously carried out at ambient temperature and atmospheric pressure in a drum-type mixer in order to maximize the diffusion mechanisms which consist of an individual movement of the particles so that the lubricant can move and distribute itself homogeneously on the surface of the balls.

[0044] As is known to those skilled in the art (see, in particular, H. Berthiaux, "Mixing and Homogenizing Divided Solids," Technique de l'ingénieur, J3397 V1 (2002)), in this type of mixing, rotation speeds of 5 to 30 rpm are preferred for a duration of 5 to 20 minutes, with filling levels in the mixer tank of 30% to 80%. An example of a suitable mixer is illustrated by the figure 2 The mixing is achieved by rotating the tank. The conical shape of the mixer shown on the figure 2 advantageously ensures radial homogenization.

[0045] The gains compared to loading using a high-density loading device, such as the Catapac™, are evaluated by measuring the packed fill densities (PSD). The analysis is performed by weighing the mass of solid particles introduced into a given volume after compaction (2400 blows). The packed fill density represents a "maximized" filling, which is generally not fully achieved by high-density industrial loading. However, the Catapac™ behavior remains close to the PSD results, and industrial densities are extrapolated from these PSD tests. This packed fill density method is therefore a consistent indicator of the performance of the Catapac™ loading system.

[0046] The gains compared to manual loading, such as sock loading, are evaluated by measuring the poured density. The analysis is performed by weighing the mass of solid particles introduced into a given volume (without compaction). The poured density is considered equivalent to that obtained after manual loading since it results from the same flow.

[0047] These two methods therefore allow for an estimation of the densities obtained on an industrial scale.

[0048] Also, when the conditions mentioned above are met, the pretreatment process according to the invention advantageously allows an increase in filling densities in manual loading using a flexible conduit of up to 4% and an increase in filling densities with an internal device, for example Catapac™, ranging from 0 to 4%.

[0049] In addition to the gain provided on the application process (adsorption process) inherent in increasing the number of adsorption sites in the reactor, we observe: A reduction in the re-settling effect. Re-settling is often observed a few hours after unit start-up, corresponding to a density increase of 1 to 2%. This effect creates empty spaces above the beds after loading, which can impair performance. The pretreatment step according to the invention reduces, or even completely eliminates, this settling effect after unit start-up. Improved hydrodynamics in the reactor. The increased filling density results in more homogeneous filling, which reduces hydrodynamic dispersion. Easier operation of the loading device, particularly for internal devices such as Catapac™™, thanks to the increased flowability of the solid induced by the pretreatment step.

[0050] It was also observed that pre-treated solid particles exhibit reduced water absorption in the case of hygroscopic solid particles. The hydrophobic film on their surface protects them from moisture and reduces static electricity generated during flow. EXAMPLES Example 1: Adsorbent loading for xylene separation

[0051] Xylene separation is achieved using a zeolite X-type adsorbent in the form of 0.54 mm nominal diameter beads, which are loaded into the adsorber using a Catapac™-type loading system. Industrial densities are extrapolated from packed densities (DRT).

[0052] Three types of lubricants were tested: magnesium stearate, calcium stearate and barium stearate. Pretreatment

[0053] In the laboratory, the adsorbent was mixed with the lubricant by rotating a drum-type mixer.

[0054] The drum is slightly inclined to ensure radial homogenization.

[0055] The procedure followed is as follows: The adsorbent is introduced into the drum, with a quantity of approximately 50 g. The lubricant is then introduced into the drum in the appropriate proportions (between 0 and 1% by weight relative to the weight of the adsorbent). The drum is rotated at a speed of 10 rpm for 10 minutes. The packed density is measured as described previously. The poured density is measured as described previously.

[0056] The water content is initially determined by measuring the loss on ignition (LOI) as a percentage by weight at 900 °C. The sample mass is then measured between each step to determine the exact mass of water reabsorbed during the pretreatment test. The tests are conducted in a laboratory with controlled humidity of 55%. The results are expressed as the mass of dry adsorbent per unit volume, which is the relevant value for the process, after correcting for the mass of lubricated adsorbents introduced during the density measurement, as well as their water and lubricant content.

[0057] The results in packed density for three different lubricants (Magnesium Stearate, Calcium Stearate and Barium Stearate) are described by the Figures 3A, 3B and 3C The composition of the mixture is expressed as a mass percentage. The points at 0% constitute the reference (comparative), i.e. the packed filling density of the adsorbent alone, and therefore without mixing with the lubricant.

[0058] The results obtained with Calcium Stearate ( Figure 3A ) show satisfactory reproducibility and prove that pretreatment allows for a significant improvement in packed density.

[0059] Tests conducted with barium and magnesium stearate show an increase in packed density for all lubricant contents between 0.01 and 1% by weight of the mixture, and reveal an optimum for lubricant contents between 0.05 and 0.25% by weight of the mixture. This behavior is consistent with the theory presented earlier, which predicts an initial decrease in adhesion force followed by a reversal of this phenomenon as the lubricant begins to aggregate on the surface, creating roughness rather than a reduction in interaction forces.

[0060] Under optimal conditions, the pretreatment process according to the invention thus allows a gain in compacted density of 2.2% compared to the reference.

[0061] The results of the poured density are expressed in the same way and are presented by the Figures 4A (with magnesium stearate) and 4B (with barium stearate).

[0062] The effect of the lubricant on the poured density is identical to that observed on the compacted density, with an increase in poured density of up to 3.7% compared to the reference.

[0063] This result confirms that the pretreatment process improves both a classic manual loading of the Sock type (loose density) and a high density loading of the Catapac ™ type (compacted density).

[0064] Furthermore, the water measurements taken during the tests show a protective role of the lubricant against moisture, as represented by the figure 5which shows the mass of water in grams taken up by the pre-treated adsorbent sample as a function of the lubricant content by weight relative to the total mass of the mixture.

[0065] When a unit is started up, in the absence of an adsorbent pretreatment process, the transport bags are weighed on-site, and those exhibiting excessive water absorption are declared "out of specification" and are not loaded. Therefore, using a pretreatment according to the invention prior to transport can also limit the effect of water absorption and thus prevent loss before loading.

[0066] Finally, it was noted that the lubricant possesses anti-adhesive properties and significantly reduces the generation of static electricity. The passage of an untreated adsorbent through the drum results in the adhesion of particles to the wall: the Figures 6A and 6B, illustrate this phenomenon and show the contents of the drum after 10 minutes of rotation at 10 rpm, respectively for the untreated adsorbent and for the adsorbent-lubricant mixture with a content of 1% magnesium stearate.

[0067] The presence of the lubricant inhibits this phenomenon of static electricity generation and allows for easier handling of the solid. Example 2 : Drilling test

[0068] The absence of interaction between the pretreatment process according to the invention and the performance of a xylene separation process was verified by penetration tests (frontal chromatography) as described in patent FR2903978, carried out on a reference column comprising an adsorbent (comparative) and a pretreated column comprising an adsorbent pretreated with 0.8% Calcium Stearate by weight relative to the total weight of the mixture (according to the invention). The quantity of adsorbent used for these tests was approximately 75 g.

[0069] The procedure is as follows: In the case of the pre-treated column, mix with 0.8% calcium stearate, according to the methodology described in Example A. Fill the column with the adsorbent, pre-treated or untreated, and place it in the test bench. Fill with the solvent (paradiethylbenzene at room temperature). Gradually raise the adsorption temperature under a solvent flow rate (5 cm³ / min). In the case of the pre-treated column, paradiethylbenzene samples are taken every 2 minutes during the temperature ramp-up. Inject solvent when the adsorption temperature is reached. Switch the solvent / feed mixture to inject the feed. The feed injection is then maintained for a sufficient time to reach thermodynamic equilibrium. Collect and analyze the effluent from the drilling.

[0070] The operation is carried out at a charge flow rate of 10 cm³ / min.

[0071] The pressure is sufficient to keep the charge in the liquid phase, i.e., 1 MPa. The adsorption temperature is 175 °C. The composition of the charge is as follows: Meta-xylene 45 wt% Para-xylene 45 wt% Isoo-octane 10 wt% (this is used as a tracer for estimating non-selective volumes and does not participate in the separation)

[0072] During the heating of the pretreated column, samples taken at around 120-130 °C become biphasic. This phenomenon is attributed to the melting of the lubricant (its melting point is 130 °C), which is then carried away by the paradiethylbenzene.

[0073] The results from the analysis of the drilling curves are summarized in Table 1. Table 1: Drilling curve results Reference column (comparative) Pre-treated column (according to the invention) Loss on ignition at 900°C 5,5% 5,5% Selectivity Para-xylene / Meta-xylene (1) 1 1,003 Capacity (1) 1 0,995 Theoretical platform height (1) 1 1,011 (1) The results are expressed in relation to the reference column, that is, by dividing the value obtained by the value obtained with the reference column.

[0074] It was observed that the pretreatment had no impact on the raw performance of the adsorbent. These results confirm the absence of interactions with process performance and confirm the removal of the lubricant with the solvent (here, paradiethylbenzene) during the start-up of the xylene adsorption unit.

[0075] Therefore, the example shows that applying the pretreatment process according to the invention to the loading of an adsorbent in a xylene separation process makes it possible to improve the Catapac™ type dense loading density by 2.2%, without altering the performance of the adsorbent, which leads to an increase in the productivity of the process of 2.2% (proportional to the mass of adsorbent present in the reactor).

[0076] The pretreatment process tested in the context of xylene separation allows for an increase in packed and poured densities of 2 to 4%, without altering the performance of the adsorbent. Since industrial densities are extrapolated from packed densities and performance is proportional to the mass of adsorbent present in the reactor, the pretreatment process according to the invention alone enables a 2 to 4% increase in the productivity of the xylene separation process. ADVANTAGES OF THE METHOD ACCORDING TO THE INVENTION

[0077] In addition to increasing the loading density of solid particles, the solid particle pretreatment process according to the invention also allows: A reduction in bed settling after start-up; a reduction in hydrodynamic dispersion; easier loading due to improved flowability; a reduction in water reabsorption of solid particles; a reduction in static electricity generated during flow

[0078] The pretreatment process according to the invention is particularly applicable to the loading of adsorbents for the implementation of a xylene separation process, for example, the ELUXYL™ process. Regardless of the type of loading, the pretreatment process tested in the context of xylene separation allows for a net increase in loading density without altering the intrinsic performance of the adsorbent. Since the performance of the xylene separation process is proportional to the mass of adsorbent present in the reactor, the pretreatment process according to the invention alone enables an increase in the productivity of the xylene separation process.

Claims

1. Process for pretreatment of X zeolite type adsorbent particles for the separation of xylenes, for improving the filling of a chamber with said solid particles, characterized in that said solid particles are mixed before loading of said solid particles into the chamber with at least one lubricant that is solid at ambient temperature and chosen from saturated fatty acids having 14 or more carbon atoms, metal salts of saturated fatty acids having 14 or more carbon atoms, esters of fatty acids having 14 or more carbon atoms, fatty alcohols having 14 or more carbon atoms, linear N-alkanes having 16 or more carbon atoms in solid form, fumaric acid, talc, sodium stearoyl fumarate, the lubricant being introduced at a content of between 0.01% and 1% relative to the total weight of the mixture of solid particles and lubricant, the loading being carried out manually with the aid of a flexible hose or with the aid of a functional device internal to the chamber which may be introduced into and / or withdrawn from said chamber.

2. Process according to Claim 1, in which said internal functional device comprises, in its upper part, a means for feeding with particles and, in its base located inside the chamber to be loaded, a dispersion system attached to a central shaft rotated about a substantially vertical axis by a motor means, and a feed pipe at least partially surrounding the central shaft, said central shaft is a tube having an internal diameter sufficient to make it possible to carry out, in the zone to be loaded, by means of this tube and during the loading period, a certain number of operations connected or complementary to said loading operation, this device comprising a stationary tube attached to the feed pipe and placed inside said rotary central shaft, the stationary tube and said rotary central shaft being substantially coaxial.

3. Process according to one of the preceding claims, in which the lubricant content is between 0.01% and 0.5% by weight.

4. Process according to Claim 3, in which the lubricant content is between 0.05% and 0.25% by weight.

5. Process according to one of the preceding claims, in which the lubricant is a fatty acid chosen from myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, lignoceric acid or cerotic acid, or a metal salt of saturated fatty acids having 14 or more carbon atoms, chosen from salts based on aluminium, calcium, magnesium, zinc, sodium, barium or lithium, a fatty alcohol having 14 or more carbon atoms chosen from myristyl alcohol, palmityl alcohol or stearyl alcohol, a paraffin having 16 or more carbon atoms, an ester of saturated fatty acids having 14 or more carbon atoms chosen from the following compounds: glyceryl monostearate, glyceryl distearate, glyceryl monopalmitate, glyceryl dipalmitate, glyceryl tristearate, glyceryl tripalmitate, glyceryl trimyristate or glyceryl tribenhenate.

6. Process according to one of the preceding claims, in which the lubricant is chosen from magnesium stearate, calcium stearate and barium stearate.

7. Process according to Claim 6, in which the lubricant is magnesium stearate.

8. Process according to one of the preceding claims, in which the solid particles are in the form of beads or extrudates.

9. Process according to one of the preceding claims, in which the equivalent diameter of the solid particles is less than 2 mm.

10. Process according to one of the preceding claims, in which the particles of lubricant used have a particle size such that at least 90% by weight of the particles of lubricant pass through a 90 µm screen.

11. Process according to one of the preceding claims, in which the mixing is carried out at ambient temperature and atmospheric pressure in a drum-type mixer.

12. Process according to Claim 11, in which the mixing is carried out with a speed of rotation of between 5 and 30 rpm, for a time of between 5 min and 20 min, and with a degree of filling in the tank of the mixer of between 30% and 80%.

13. Process according to one of the preceding claims, in which the chamber is a chemical or electrochemical, petroleum or petrochemical type reactor.