Method for grinding waxes using grinding aids in a jet mill, using polyols as grinding aids and wax powder containing polyols

Abstract

Process for grinding waxes and producing wax powders - with an average particle size d 50 of less than 10 µm or - with an average particle size d 90 of less than 15 µm or - both comprising the step of bringing a wax as millbase into contact with at least one polyol as milling aid and milling in a jet mill, a) wherein the polyol is added at a concentration of 0.01 to 5.0 wt.% based on the sum of grinding aid and mill base during the milling process, b) wherein the wax powder contains the polyol in an amount of 0.01 to 5.0 wt.%, based on the total of wax powder including polyol in the wax powder, c) wherein the wax powder consists of more than 97.5% by weight exclusively of wax(es) and polyol(s), and d) wherein the polyol has 2 to 12 carbon atoms, optionally 1 ether group per molecule, and at least 2 free hydroxy groups per molecule.

Description

[0001] The present invention relates to a process for grinding waxes, in particular paraffin waxes, using a polyol as a grinding aid in a jet mill, in particular a fluidized bed counter-jet mill, to wax powders thus produced and to the use of the polyols as grinding aids for waxes.

[0002] It is known to grind waxes into powders using mills of various designs. Care must be taken to ensure that the amount of energy introduced into the material to be ground is as low as possible to avoid melting and thus clogging or sticking of the material to be ground in the grinding chamber or of the product particles to one another. Furthermore, the choice of mill type also depends on the desired fineness of the material to be ground. The coarser the grain size, the more flexibility there is in selecting the possible mill machine designs. Waxes with correspondingly high melting points can be ground at room temperature. If the wax to be ground cannot tolerate the energy input caused by the grinding process without clogging or even melting, the grinding temperature must be lowered by external cooling of the mill, the gas transport stream and / or the material to be ground, and possibly also the recycle stream, in order to achieve the desired grinding result.

[0003] US Pat. No. 3,615,785 A discloses a grinding aid for the production of Portland cement. The grinding aid comprises at least the following water-soluble components: a glycol, an alkali metal salt of a short-chain carboxylic acid, a salt of a sulfonated lignin, and optionally a hydroxyalkylamine.

[0004] US 2004 / 0 057 973 A1 describes a cosmetic composition comprising a micronized polyethylene wax produced by polymerizing ethylene under high pressure in the presence of aliphatic or alicyclic ketones as molecular weight regulator and subsequent micronization.

[0005] DE 40 32 619 A1 discloses a matting agent consisting of SiO 2 , polyol and wax for paints and varnishes, and a process for producing the matting agent, wherein SiO 2 in a jet mill or a mechanical mill, if necessary with subsequent screening, with the addition of SiO2 , polyol and wax is micronized.

[0006] EP 2 006 322 A1 discloses wax mixtures with reduced dust generation, containing, according to one embodiment, polyethylene glycols or polyethylene glycol derivatives and at least one wax selected from amide waxes, hydrocarbon waxes, or oxidized long-chain hydrocarbon waxes. Reducing dust generation is intended to reduce the risk of explosion during grinding.

[0007] The object of the present invention is to provide a process which enables the grinding of waxes, e.g. with solidification points (each ASTM D 938-05 / DIN ISO 2207:1983) of less than 115°C, in particular less than 110°C, and to wax powders with average particle sizes d 50 (number average) of less than 10 µm, especially less than 7 µm, especially without cooling. According to a further definition, the average particle sizes d 90(Number average) less than 15 µm, in particular less than 10 µm (each according to ISO 13320:2009), also in particular without cooling.

[0008] The object is achieved according to the invention by the subject matter of the independent claims. Advantageous developments of the invention are specified in the subclaims or described below.

[0009] The present invention makes it possible to grind waxes that were previously impossible to grind, or only with considerable effort for machine cleaning, or at very low process temperatures. These can include petroleum-based waxes, synthetic or natural waxes, and their modified forms, such as partially oxidized paraffin waxes, which are ground using a jet mill as the grinding tool.

[0010] Waxes are substances defined by their mechanical and physical properties. Their chemical composition and origin can vary greatly. A substance is referred to as a wax within the meaning of the present invention if it is malleable and solid at 20°C, melts without decomposition above 40°C, and becomes slightly liquid / is slightly viscous slightly above its melting point. Particularly suitable waxes are waxes with solidification points below 115°C, especially solidification points below 110°C or even below 80°C. In particular, the solidification point of waxes is above 40°C.

[0011] Particularly suitable are hydrocarbon waxes and their derivatives, such as partially oxidized hydrocarbon waxes, e.g., those with an acid number of less than 30 mg KOH / g. Hydrocarbon waxes include, for example, Fischer-Tropsch waxes or paraffin waxes. However, it is also possible to grind partially oxidized paraffin waxes or Fischer-Tropsch waxes into powders according to the invention. Examples of commercial products that are particularly suitable for grinding by the process according to the invention are Sasolwax C105, Sasolwax H1, Sasolwax C80, or Sasolwax 7040.

[0012] The grinding aid is added to the material to be ground either in solid form or in liquid form during the grinding process. It remains in the material after the grinding process or evaporates completely or partially during the grinding process. If desired, the grinding aid can also be subsequently removed, for example by stripping with a stripping gas.

[0013] Polyols are used as grinding aids, particularly polyols with 2 to 12, especially 3 to 7, carbon atoms and optionally 1 to 4 ether groups. Polyols in the sense of the present invention are alcohols with at least two free hydroxyl groups.

[0014] Particularly preferred are trimethylolpropane, ethylene glycol, diethylene glycol, propylene glycol, trimethylene glycol (1,3-propanediol), or neopentyl glycol. These prevent the grinding material from adhering to the walls of the machine and the particles from sticking to one another after the grinding process. Depending on the wax to be ground, the added amount of the grinding aid ranges from 0.01 to 5.0 wt.% or 0.1 to 3.0 wt.%, and in particular 0.2 to 2.5 wt.%.

[0015] Comminution is preferably carried out using a jet mill, preferably a counter-jet mill, and in particular a fluidized-bed counter-jet mill. The grinding process preferably takes place at temperatures of, for example, 10 to 40°C, in particular at typical ambient temperatures of 20 to 30°C.

[0016] Jet mills are long-established comminution machines in which the particles to be crushed are accelerated by gas streams and crushed by impact. There are a number of different jet mill designs. They differ in the type of gas flow, the way the particles impact each other or an impact surface, and whether the particles to be crushed are carried along in the gas jet or whether the gas jet impacts the particles and entrains them. Air is usually used as the grinding gas. Opposed jet mills, and especially fluidized-bed opposed jet mills, are preferred.

[0017] In the fluidized-bed counter-jet mill, as known, for example, from EP 0 139 279 A2, gas jets collide in a grinding chamber containing the material to be ground in the form of a fluidized bed. Grinding occurs through the collision of the material particles against each other, preferably almost exclusively through this collision. The fluidized-bed counter-jet mill is usually equipped with a separator, in which the resulting fine material is separated from the insufficiently ground coarse material. The coarse material is returned to the grinding chamber.

[0018] The fluidized-bed jet mill used according to the invention preferably has a grinding chamber free of internals, with one or more nozzles arranged in the bottom area. However, internals in the form of impact surfaces can also be provided.

[0019] The grinding chamber is preferably completely filled with the material to be ground up to this height. The material to be ground and the gas emerge from the material bed as a low-velocity fountain. This fountain serves to feed a classifier located above the surface of the material bed and operated independently of the momentum of the jet emerging from the bottom nozzle. During grinding, several additional jet nozzles can be arranged in a circle, approximately at the height of the upper edge of the filling bed, with their axes intersecting at a single point.

[0020] The invention is explained by means of examples, without being limited to them.

[0021] Fig. Figure 1 shows the particle size distribution of a powder of a Fischer-Tropsch paraffin wax containing trimethylolpropane obtained using a fluidized bed counter-jet mill. Experiment description:

[0022] In a Hosokawa fluidized bed opposed jet mill (AFG 400), trimethylolpropane was introduced as a solid grinding aid together with a Fischer-Tropsch paraffin wax (Sasolwax® C80), consisting of saturated hydrocarbons and having a congealing point of 78 to 83°C, in particular around 80°C, as the millbase. The millbase and the grinding aid were each pre-dosed using a dosing screw, so that 1 wt.% trimethylolpropane, based on the mixture of millbase and grinding aid, was milled. This arrangement allowed the millbase, which otherwise tends to clump and clog the mill, to be ground well at room temperature. Finenesses down to d 90 of 7.5 µm was achieved. Clogging of the machine was greatly reduced. The achieved particle size distribution is in Fig. 1 shown.

Claims

[1] Process for grinding waxes and producing wax powders - with an average particle size d 50 of less than 10 µm or - with an average particle size d 90 of less than 15 µm or - both comprising the step of bringing a wax as millbase into contact with at least one polyol as milling aid and milling in a jet mill, a) wherein the polyol is added at a concentration of 0.01 to 5.0 wt.% based on the sum of grinding aid and mill base during the milling process, b) wherein the wax powder contains the polyol in an amount of 0.01 to 5.0 wt.%, based on the total of wax powder including polyol in the wax powder, c) wherein the wax powder consists of more than 97.5% by weight exclusively of wax(es) and polyol(s), and d) wherein the polyol has 2 to 12 carbon atoms, optionally 1 ether group per molecule, and at least 2 free hydroxy groups per molecule. [2] Method according to claim 1, characterized by that the jet mill is a counter-jet mill, in particular a fluidized bed counter-jet mill. [3] Method according to claim 1 or 2, characterized by that the grinding process takes place at 10 to 40°C. [4] Method according to at least one of the preceding claims, characterized by that the wax is a paraffin wax or Fischer-Tropsch wax. [5] Method according to at least one of the preceding claims, characterized by that the grinding aid is added to the material to be ground either in solid form or in liquid or liquefied form during the grinding process. [6] Method according to at least one of the preceding claims, characterized bythat the polyol is added at 0.1 to 3.0 wt.%, in particular 0.2 to 2.5 wt.%, based on the sum of grinding aid and mill base during the grinding process. [7] Method according to claim 1, characterized by that the mean particle size d 50 of the wax powder is less than 7 µm. [8] Method according to claim 1, characterized by that the mean particle size d 90 of the wax powder is less than 10 µm. [9] Wax powder - with an average particle size d 50 of less than 10 µm or - with an average particle size d 90 of less than 15 µm or - both, and a solidification point of below 115 °C, further comprising 0.01 up to 5.0 wt.%, in particular 0.1 up to 3.0 wt.% and particularly preferably 0.2 to 2.5 wt.%, of at least one polyol, based on the sum of wax powder including polyol in the wax powder, wherein the wax powder consists of more than 97.5 wt.% exclusively of wax(es) and polyol(s) and wherein the polyol(s) has / have 2 to 12 carbon atoms, optionally 1 ether group per molecule, and at least 2 free hydroxyl groups per molecule. [10] Wax powder according to claim 9, characterized by that the powder consists of more than 98% by weight exclusively of wax(es) and polyol(s). [11] Wax powder according to at least one of claims 9 or 10, characterized by that the wax has a solidification point of greater than 40°C and less than 115°C, in particular less than 110°C.

Images