Fine Grain Filler with Improved Wettability
20210171789 · 2021-06-10
Assignee
Inventors
Cpc classification
C01P2004/61
CHEMISTRY; METALLURGY
C09C3/006
CHEMISTRY; METALLURGY
C09C3/10
CHEMISTRY; METALLURGY
C01P2004/51
CHEMISTRY; METALLURGY
International classification
C09C3/00
CHEMISTRY; METALLURGY
C09C3/04
CHEMISTRY; METALLURGY
C09C3/08
CHEMISTRY; METALLURGY
Abstract
A filler for a coating including a powder formed from igneous rock with substantially no free silica and a Mohs hardness of at least 5 and a controlled maximum particle size of less than 6 microns, wherein said particles have a surface fluid layer of a lubricative fluid to drastically increase the wettability of said powder and a method of producing the same.
Claims
1. A filler for a coating comprising a powder formed from igneous rock with substantially no free silica and a Mohs hardness of at least 5 and a controlled maximum particle size of less than 6 microns, wherein said particles have a surface fluid layer of a lubricative fluid to drastically increase the wettability of said powder.
2. The filler as defined in claim 1 wherein said increased wettability is less than 60 seconds as measured by the IDF method of determining wettability.
3. The filler as defined in claim 2 wherein said particles have at least a majority of the particle surface area covered by said fluid layer.
4. The filler as defined in claim 1 wherein said particles have at least a majority of the particle surface area covered by said fluid layer.
5. The filler as defined in claim 2 wherein said surface fluid layer is also a cohesive fluid so the density of said powder is defined by said particles being clumped into clusters having many particles with diverse particle sizes loosely held together until said powder is deposited into said coating.
6. The filler as defined in claim 1 wherein said surface fluid layer is also a cohesive fluid so the bulk density of said powder is defined by said particles being clumped into clusters having many particles with diverse particle sizes loosely held together until said powder is deposited into said coating.
7. The filler as defined in claim 6 wherein said lubricative and cohesive fluid is a treating fluid having lubricative and cohesive properties technically equivalent to propylene glycol.
8. The filler as defined in claim 6 wherein said lubricative and cohesive fluid is propylene glycol.
9. The filler as defined in claim 6 wherein said igneous rock is nepheline syenite.
10. The filler as defined in claim 5 wherein said igneous rock is nepheline syenite.
11. The filler as defined in claim 6 wherein the moisture content of said filler is less than 1.0 percent.
12. The filler as defined in claim 5 wherein the moisture content of said filler is less than 1.0 percent.
13. The filler as defined in claim 5 wherein said surface fluid layer comprises less than 1.0 percent of the weight of the particles in said filler.
14. The filler as defined in claim 13 wherein said surface fluid layer comprises 0.2 to 0.6 percent of the weight of the articles in said filler.
15. A filler as defined in claim 5 wherein said coating is selected from the class consisting of: paint, automotive base coat, automotive clear coat, UV curable pud clear wood coating, conventional clear wood floor coating, ink, colorant, and powder coating.
16. A method of producing a filler for a coating, said method comprising: (a) converting a particle mass of igneous rock having a maximum particle size D99 at a given level into a dry final particles having a reduced maximum particle size of less than 6 microns; and, (b) during said converting operation applying a surface layer of a treating fluid onto said dry final particles which fluid is lubricative so said dry final particles have a drastically increased wettability, said treating fluid being applied in an amount to obtain the desired increase in wettability of said dry final particles which comprises said filler.
17. The method as defined in claim 16 wherein said converting operation is a wet grinding operation to create a slurry having a wet mass of said final particles and including: (c) drying said wet mass of said final particles into dried agglomerated pieces of said final particles; (d) mechanically changing said dried agglomerated pieces into individual dry final particles; and, (e) applying said surface layer to said dry final particles during said mechanically changing operation.
18. The method as defined in claim 16 wherein said converting operation is merely a dry grinding operation to form said dry final particles and including: (c) applying said surface layer to said dry final particles during said grinding operation.
19. The method as defined in claim 16 wherein said amount of treating fluid is 0.2 to 0.6 percent by weight of said dry final particles.
20. The method as defined in claim 16 wherein said treating fluid is also cohesive so said dry final particles have a tendency to loosely adhere to each other thereby forming multi-particle clusters, which clusters rapidly disintegrate into individual final particles when said clusters are introduced into said coating.
21. The method as defined in claim 20 wherein said lubricative and cohesive fluid is a treating fluid having lubricative and cohesive properties technically equivalent to propylene glycol.
22. The method as defined in claim 20 wherein said lubricative and cohesive fluid is propylene glycol.
23. The method as defined in claim 16 wherein said igneous rock is nepheline syenite.
24. A coating composition comprising a filler defined in claim 1.
25. A coating composition as defined in claim 24 wherein the composition is selected from the class consisting of: paint, automotive base coat, automotive clear coat, UV curable pud clear wood coating, conventional clear wood floor coating, ink, colorant and powder coating.
26. A filler obtained by using the method defined in claim 16.
Description
BRIEF DESCRIPTION OF DRAWINGS
[0022] The invention may take physical form in certain parts and arrangement of parts, a preferred embodiment of which will be described in detail and illustrated in the accompanying drawings which forms a part hereof and wherein:
[0023]
[0024]
[0025]
[0026]
[0027]
DESCRIPTION OF PREFERRED EMBODIMENTS
[0028] Referring now to the drawings wherein the showings are for the purpose of illustrating preferred and alternative embodiments of the invention only and not for the purpose of limiting the same, the novel filler involves the concept of applying a lubricative and cohesive fluid layer of a surface treating agent onto the surfaces of the very low maximum size filler particles. This treating fluid increases the wettability of the filler. In accordance with a secondary benefit the treating agent is cohesive and causes the particles to naturally clump into a number of easily separated clusters, each containing a large number of very small dry particles. Propylene glycol is the lubricative and cohesive treating fluid used. In the invention, the wettability of the novel filler has been found to be less than 60 seconds using the standard IDF Method of measuring wettability. Indeed, it is less than 30-20 seconds. An inorganic rock filler, such as nepheline syenite with a maximum particle size of 4 microns; but, without surface application of the novel treatment agent, is substantially greater than three minutes (i.e. 180 seconds in this standard test) and the small particle filler merely floats. The moisture content of the novel powder is less than 1.0 percent, preferably 0.2 to 0.6 percent, so the consistency and particle spreadability of the novel filler is excellent. The novel filler is enhanced by the fact that the lubricative and cohesive surface treating fluid applied over the particle surfaces also physically captures the fines (particles less than 0.5 microns) resulting when the mass of particles of the filler are ground to a small size, by either wet grinding or dry grinding. The treating fluid holds the captured fines against the surfaces of the filler particles. In summary, the invention accomplishes the main objective of drastically increasing the wettability. But there are other advantages, such as increasing the Bulk Particle size by forming many particle clusters and also reducing dust created by very small particles. As shown in
[0029] Consequently, the invention broadly involves creating a novel filler employing the concept of treating the surfaces of the dry particles formed from a mass of igneous rock particles having substantially no free silica (defined as less than 0.01 percent by weight of silica). The new filler is a mass of fine particles having a maximum particle size of less than 6 microns, but preferably less than 4 microns. The surface treatment is applying a surface layer of a treating agent comprising a unique fluid applied over the surfaces of the particles when in a dry condition either (a) after the particles are wet ground into the desired small particle size, dried and converted into the dry ground size or (b) when the very small grain filler is produced by dry grinding. The fluid remains as an extremely thin layer on the surfaces and drastically increases the wettability of the individual particles of the final filler. The treating fluid layers on the particle surfaces have a secondary advantage of forming very small grain filler into a vast number of density defining clusters A, as schematically shown in
[0030] A first preferred embodiment, involves a laboratory production of the novel filler, as disclosed in
[0031] The final particles produced by operation 110 are converted from a wet version 112 to a dry version in the form of agglomerated hard pieces 116a and then to individual dry particles at milling operation 118. The dry particles produced by mill 118 are original particles created in grinding operation 110 and dried in operation 114. The invention is applying a treating agent onto the surface area of the dried final particles 120. In practice, the invention is performed by using a treating agent that is lubricative and cohesive, such as propylene glycol, as so far explained. Consequently, method 100 converts the large particles M3 into a final powder having dry particles with small particle size M14 as the “new final powder” 120. During the conversion of particles M3 to particles M14 constituting powder or filler 120 the wet ground particles are dried. The novel treating agent is applied to the particles when they are dry and at operation 118. The final particles must be dry and sized back to the ground size of operation 110 by operations 116 and 118. Only then do the particles receive and retain the novel surface coating comprising the invention. In this embodiment, the novel treating agent or fluid is used after final shattering of pieces 116a at the blender of operation 116 and during particle separation (jet mill) of operation 118. It is applied to the dried particles after they are returned back into the particle size from operation 110. They are the final particles 120 of the novel filler.
[0032] In method 100, the final powder 120 has dry particles coated with the novel lubricative and cohesive fluid which is added in milling operation 118. The total amount is selected to obtain the desired results and in practice is less than 1.0 percent by weight of the final powder and preferably 0.2 to 0.6 percent.
[0033] The invention developed in the laboratory and shown as method 100 in
[0034] In summary, irrespective of the process operations to produce powder 120, though the processes are also novel and inventive, the novel final powder is a fine grain nepheline syenite dry powder with particle surfaces coated by a small amount of a lubricative surface treating fluid, i.e. propylene glycol. Such fine grain nepheline syenite powder is used as a mineral “filler” for a coating material, such as paint, etc. This novel mineral filler or powder 120, with particle surfaces coated with propylene glycol, increases hardness, scratch resistance, clarify and color of the coating. Most importantly, the propylene glycol coating allows the nepheline syenite filler to wet easily and quickly mix into the coating, such as paint P by the particle dispersion procedure illustrated in
[0035] Thus, a novel treating agent covers the surfaces of the very fine dry mineral powder with a thin layer, thereby creating the novel mineral filler or powder 120. The treating agent creates the properties of high wettability and the cluster forming and dispersing concept shown in
[0036] In an early implementation of the first embodiment, operation 110 involved 200 grams of Minex 3 with D99 of about 100 microns that was wet ground and a small amount of propylene glycol (preferably 0.25-1.0 percent by weight of the Minex 3, as a grinding aid, not as used in the invention). The mechanical grinding in operation 110 used any standard wet grinding mechanism. A wet mass (slurry) of nepheline syenite powder was produced after about 2-3 hours. The wet mass was dried overnight at 100-200° C. to an agglomerated dried mass as dry broken pieces or “chunks” 116a having the small dry particles. These pieces are then placed into an aggressive blending or grinding operation 116 and then into a jet mill of operation 118. The final processing mechanism of operations 116 and 118 may be a blender, a mechanical mill, etc., to convert aggressively the dry broken pieces 116a into the final, evenly dispersed, dry powder 120. This powder constitutes the novel invention of dry particles coated with propylene glycol, the lubricative and cohesive surface treating agent at operation 118.
[0037] The disclosed, developed inventive concept is treating the surfaces of the individual dry particles in the total mass of igneous rock particles to create a surface layer of treating agent or fluid on the final particles. The layer of the treating agent or fluid remains on each particle constituting the particles of the novel filler and covers a majority of the surfaces, i.e. at least 50 percent and preferably over 60 percent. In summary, a novel filler has been created where layers of cohesive, lubricative fluid causing the high wettability dry particles of the mass to automatically clump into a vast number of small clusters A and quickly disperse, as schematically illustrated in
[0038] The novel filler or new final powder 120 is a mass of igneous rock particles with substantially no free silica. It has particles with a defined small maximum particle size of less than 5 microns and with surfaces having a layer of treating agent or fluid imparting novel properties to the particle mass, as explained. This new filler performs the characteristics of a hard, small grain filler and the particles have a high wettability to allow the rapid acceptance and dispersion of particles 10. As a secondary advantage, this agent or fluid controls the density of the filler by forming into a number of multiple effective diameter clusters A, each with loosely held together, individually dispersible, particles that separate automatically, and immediately, once the clusters are fed or dropped into a liquid substance, as shown in
[0039] The coatings using the new filler may be various types, i.e. paint, wood coating or other surface coatings. Although the invention has been described as a mineral “filler”, the novel dry final powder 120 modified to include surface treatment to provide a treating agent, such as propylene glycol over the surfaces of the fine powder may have other uses. The advantages obtained by the discovery of using a lubricative liquid or fluid to coat the particles of ultra-fine mineral powder (nepheline syenite at D99 of less than 5 microns), may be obtained by using a treating fluid so long as it has the wettability values obtained by lubricative property of propylene glycol. It is also advantageous for the treating fluid to have the cohesive property of propylene glycol so the features described in
[0040] As mentioned earlier in this disclosure, it was found that use of propylene glycol in the amount of 0.2 to 0.6 in operation 118 of
Production Run
[0041] The actual production run of the invention is illustrated in
[0042] The stated particle size of the input powder in supply 202 and the PG dosage of pump 208 are used in production method 200. However, the “particle size” of the powder in supply 202 can be any larger sized nepheline syenite available at the manufacturing plant, such as M-3 with a D99 particle size of about 50 microns and M-7 with a D99 particle size of about 20 microns. As a general inventive definition, the size could be stated as “less than 100 microns” or “less than 50 microns”. The dosage of propylene glycol PG from tank 206 is less than 1.0 percent by weight of the input mass from supply 202 so the final dry powder has a preferred coating of 0.2 to 0.6 percent by weight. Dry grinding with PG is theoretically different from using wet grinding in method 100 where propylene glycol could also (but irrelevantly) be used as an aid to the wet grinding. The invention is not novel grinding. The invention is a very fine filler with dry powders having novel surface conditions caused by surface coating with a thin layer. The layer is applied onto the surfaces of dry particles as method 200 converts the large particles of supply 202 into the “final” particles in output line 222.
[0043] Mill 210 dry grinds the nepheline syenite powder into a fine, ground powder that is carried by the air flow from mill 210 through line 212 to a somewhat standard particle classifier 220 to separate the dry propylene glycol coated particles (less than 0.5 percent moisture content) having the final “targeted size” for discharge through line 222. This discharge is the novel filler with particle size of less than 6 microns or preferably less than 4 microns. Indeed, less than 5 microns. Thus, the separated particles discharged through output line 222 are the filler or final powder of the invention. In practice, the particles from line 222 are the size of Minex 14, i.e. with maximum size of less than 4 microns. In accordance with SOP, coarse fraction particles return to mill 210 from classifier 220 by way of output line 224. Method 200 is a second embodiment and does not need drying to convert the final particles to a dry condition so they can be treated in accordance with the invention. It is, thus, different from the wet grinding method 100.
[0044] The described method 200 run had a set PG dosage of 0.5 percent by weight and the final coated particles (filler) are transported to the output receptacle by line 222. The final powder had the desired maximum particle size as already described. Furthermore, the final powder had an IDF Method test of less than 60 seconds and, indeed, less than 20-30 seconds. This desired high wettability property was obtained when up to 1.0 percent by weight PG was employed in method 200. It was discovered that less than 1.0 percent by weight was the “limited” amount necessary for a commercially usable product. As the amount approached 1.0 percent, the treated powder started “caking” and the “not” floating property was compromised. Indeed, it was discovered that 0.2 to 0.6 percent by weight was preferred to obtain both high wettability and a commercially usable product.
[0045] In one implementation of method 200, device 210 is a conical grinding mill having a cylindrical section with dimensions of 8 feet by 48 inches (external), running at about 21 rpm with a critical speed of 72 percent. It has 5 inch liners. Mill 210 has a grate at the discharge end with original slots of % inches. It has a 45-50% by volume of an alumina pebble media. The fresh (original) charge of media is (a) 3,000 pounds of 1¼ inch pebbles; (b) 2,500 pounds of 1 inch pebbles; and (c) 1,000 pounds of % inch pebbles. Rotation of the mill creates a tumbling action of the media. The media hits the particles of the input mass from supply 202 and also coats the particle with a surface layer of propylene glycol from tank 206. This action coats and breaks the particle into finer sizes. Indeed, the propylene glycol is used to create the novel particle surface treatment. Propylene glycol is used in the disclosed production development method 200 to obtain the invention. Air flow through the mill carries the most fine particles with surface layers of PG while the coarser particles stay in the mill until they ultimately reach a size that could be carried from the mill by air flow out line 212.
[0046] As a background test using dry grinding, Minex-3 nepheline syenite powder (D99 over 50 microns) was ground dry in a grinder 210 comprising an orbital ball mill for 2.5 hours at 350 rpm using 3 mm (Yttria) resulting in a fine powder with a D99 of less than 4 microns. This is “less than 6 microns”, the broadest particle size limitation of the invention and less than 5 microns, as preferred. Without adding lubricative fluid surface treating agent, the powder had an IDF Method wettability time of well over three minutes. The powder merely floated on the test water surface. This was unacceptable. When the procedure was repeated with 0.6 percent propylene glycol by weight of Minex-3 powder used during dry grinding, the wettability of the powder was drastically increased to an IDF Method wettability time of less than 30 seconds (drastically less than the acceptable 60 seconds) and the moisture content was about 0.5 percent so the particles were easily handled. Surprisingly, the mass naturally formed into many clusters A, as shown in
Amount of Treating Fluid
[0047] The treating fluid must cover a majority of the surfaces of the particles with a thin layer. This is done when the particles are dry and converted to the size of the “final” particles as by method 100 or method 200. This action of coating dry particles is different from a wet grinding where propylene glycol has been used as a grinding aid. Grinding aids have no purpose after grinding. They do not coat the particles. Indeed, when particles are wet ground, a grinding aid is in solution. It evaporates with the water as the “final” particles are heated as in operation 114. In the invention, a majority of the particle surface area must be covered by the fluid to obtain the invention disclosed herein. This requires a surface treatment agent which is less than 1.0 percent by weight of the “final” dry particles. Preferably, the weight of the surface treatment agent is 0.2 to 0.6 percent by weight of the particles. Consequently, the very large surface area caused by the creation of a vast number of very small particles is covered by a thin layer of the treating agent. The purpose of the treating fluid coating the particles relates to its use of the dry particles after grinding. The objective is to apply a coating on the surfaces of the fine particles forming the final dry powder. The actual amount of fluid is in the inventive range of less than 1.0 percent by weight and preferably 0.2 to 0.6 percent by weight. It has been discovered that if this amount is exceeded, the filler is inoperative and cannot be used as a filler because of the unacceptable “caking”. Indeed, the critical amount of treatment liquid and its limitation is a discovery constituting another important aspect of the invention.
Statements of Invention
[0048] A. A filler for a coating comprising a powder formed from igneous rock with substantially no free silica and a Mohs hardness of at least 5 and a controlled maximum particle size of less than 6 microns, wherein said particles have a surface fluid layer of a lubricative fluid to drastically increase the wettability of said powder. [0049] B. The filler as defined in claim A wherein said increased wettability is less than 60 seconds as measured by the IDF method of determining wettability. [0050] C. The filler as defined in claim B wherein said particles have at least a majority of the particle surface area covered by said fluid layer. [0051] D. The filler as defined in claim A wherein said particles have at least a majority of the particle surface area covered by said fluid layer. [0052] E. The filler as defined in claim B wherein said surface fluid layer is also a cohesive fluid so the density of said powder is defined by said particles being clumped into clusters having many particles with diverse particle sizes loosely held together until said powder is deposited into said coating. [0053] F. The filler as defined in claim A wherein said surface fluid layer is also a cohesive fluid so the bulk density of said powder is defined by said particles being clumped into clusters having many particles with diverse particle sizes loosely held together until said powder is deposited into said coating. [0054] G. The filler as defined in claim F wherein said lubricative and cohesive fluid is a treating fluid having lubricative and cohesive properties technically equivalent to propylene glycol. [0055] H. The filler as defined in claim F wherein said lubricative and cohesive fluid is propylene glycol. [0056] I. The filler as defined in claim F wherein said igneous rock is nepheline syenite. [0057] J. The filler as defined in claim E wherein said igneous rock is nepheline syenite. [0058] K. The filler as defined in claim F wherein the moisture content of said filler is less than 1.0 percent. [0059] L. The filler as defined in claim E wherein the moisture content of said filler is less than 1.0 percent. [0060] M. The filler as defined in claim E wherein said surface fluid layer comprises less than 1.0 percent of the weight of the particles in said filler. [0061] N. The filler as defined in claim M wherein said surface fluid layer comprises 0.2 to 0.6 percent of the weight of the articles in said filler. [0062] O. A filler as defined in claim E wherein said coating is selected from the class consisting of: paint, automotive base coat, automotive clear coat, UV curable pud clear wood coating, conventional clear wood floor coating, ink, colorant, and powder coating. [0063] P. A method of producing a filler for a coating, said method comprising:
[0064] (a) converting a particle mass of igneous rock having a maximum particle size D99 at a given level into a dry final particles having a reduced maximum particle size of less than 6 microns; and,
[0065] (b) during said converting operation applying a surface layer of a treating fluid onto said dry final particles which fluid is lubricative so said dry final particles have a drastically increased wettability, said treating fluid being applied in an amount to obtain the desired increase in wettability of said dry final particles which comprises said filler. [0066] Q. The method as defined in claim P wherein said converting operation is a wet grinding operation to create a slurry having a wet mass of said final particles and including:
[0067] (c) drying said wet mass of said final particles into dried agglomerated pieces of said final particles;
[0068] (d) mechanically changing said dried agglomerated pieces into individual dry final particles; and,
[0069] (e) applying said surface layer to said dry final particles during said mechanically changing operation. [0070] R. The method as defined in claim P wherein said converting operation is merely a dry grinding operation to form said dry final particles and including:
[0071] (c) applying said surface layer to said dry final particles during said grinding operation. [0072] S. The method as defined in claim P wherein said amount of treating fluid is 0.2 to 0.6 percent by weight of said dry final particles. [0073] T. The method as defined in claim P wherein said treating fluid is also cohesive so said dry final particles have a tendency to loosely adhere to each other thereby forming multi-particle clusters, which clusters rapidly disintegrate into individual final particles when said clusters are introduced into said coating. [0074] U. The method as defined in claim T wherein said lubricative and cohesive fluid is a treating fluid having lubricative and cohesive properties technically equivalent to propylene glycol. [0075] V. The method as defined in claim T wherein said lubricative and cohesive fluid is propylene glycol. [0076] W. The method as defined in claim P wherein said igneous rock is nepheline syenite. [0077] X. A coating composition comprising a filler defined in any one of claims A to O. [0078] Y. A coating composition as defined in claim X wherein the composition is selected from the class consisting of: paint, automotive base coat, automotive clear coat, UV curable pud clear wood coating, conventional clear wood floor coating, ink, colorant and powder coating. [0079] Z. A filler obtained by using the methods defined in any one of claims P-W.
[0080] While considerable emphasis has been placed on the preferred embodiments of the invention illustrated and described herein, it will be appreciated that other embodiments, and equivalences thereof, can be made and that many changes can be made in the preferred embodiments without departing from the principles of the invention. Furthermore, the embodiments described above can be combined to form yet other embodiments of the invention of this application. Accordingly, it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the invention and not as a limitation. In addition, the claims form part of the disclosure.