US3402065A - Phenyloxyalkanol coating of particle - Google Patents
Phenyloxyalkanol coating of particle Download PDFInfo
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- US3402065A US3402065A US140148A US14014850A US3402065A US 3402065 A US3402065 A US 3402065A US 140148 A US140148 A US 140148A US 14014850 A US14014850 A US 14014850A US 3402065 A US3402065 A US 3402065A
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- 239000011248 coating agent Substances 0.000 title claims description 19
- 238000000576 coating method Methods 0.000 title claims description 19
- 239000002245 particle Substances 0.000 title description 8
- 239000000463 material Substances 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 38
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 238000009835 boiling Methods 0.000 claims description 7
- 239000003223 protective agent Substances 0.000 claims description 6
- 239000011343 solid material Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 239000011802 pulverized particle Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 description 16
- 238000001179 sorption measurement Methods 0.000 description 16
- 230000003750 conditioning effect Effects 0.000 description 14
- 239000000203 mixture Substances 0.000 description 13
- 239000002360 explosive Substances 0.000 description 12
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000000356 contaminant Substances 0.000 description 6
- 239000011253 protective coating Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 230000008016 vaporization Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000008246 gaseous mixture Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- XEFAJZOBODPHBG-UHFFFAOYSA-N 1-phenoxyethanol Chemical compound CC(O)OC1=CC=CC=C1 XEFAJZOBODPHBG-UHFFFAOYSA-N 0.000 description 3
- FFWXHQFJNOGDJE-UHFFFAOYSA-N 2-(4-methylphenoxy)ethanol Chemical compound CC1=CC=C(OCCO)C=C1 FFWXHQFJNOGDJE-UHFFFAOYSA-N 0.000 description 3
- RBRMRNWFSHTPPN-UHFFFAOYSA-N 2-phenoxypropan-2-ol Chemical compound CC(C)(O)OC1=CC=CC=C1 RBRMRNWFSHTPPN-UHFFFAOYSA-N 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000005474 detonation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- -1 phenyloxy Chemical group 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 125000004104 aryloxy group Chemical group 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- IETSNCRJKUUQTD-UHFFFAOYSA-N 1-phenoxyoctan-1-ol Chemical compound C1(=CC=CC=C1)OC(CCCCCCC)O IETSNCRJKUUQTD-UHFFFAOYSA-N 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 208000037516 chromosome inversion disease Diseases 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003701 inert diluent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000011814 protection agent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Definitions
- This invention relates to surface conditioning materials and more particularly to a method of treatment of inv fusible pulverized mixtures. Specifically, this invention relates to a method and agents for protectively preparing the surfaces of pulverized materials so as to facilitate their ready incorporation into slurries which may be molded or cast into shaped articles.
- an inert material to explosive compositions has been found useful as a means of regulating the rate and brisance of a detonation.
- the normal method of incorporating the inert material into the explosive com position is to add it in a finely-divided state to a melt or a solution of the explosive material to form a slurry having the desired proportions of the suspended inert component for the particular purposes at hand.
- the suspended inert material must be introduced in a finely-divided state and preferably should be dispersed as thoroughly as possible throughout the fusible component to produce on cooling a solidified charge having a minimum porosity and a maximum uniformity of compositions. Such a composition is desirable only if there is no separation of the suspended component from the fusible component during the cycles of mixing, molding or casting the slurry into desired shapes.
- This invention provides a method and agents to overcome this last mentioned difiiculty and will be disclosed in more detail following a delineation of the objects of this invention.
- the successful preparation of slurries containing dispersed solids is dependent, in part, upon the surface characteristics of the suspended particles, and upon such factors as the quantity of the solid or infusible component, the degree of subdivision and the completeness of dispersing the infusible component throughout the fusible explosive component.
- Maximum uniformity of slurry composition is obtained by introducing the solid component in a finely-divided form and dispersing it as thoroughly as possible in the fusible vehicle.
- any solid comminuted component increases as the mean diameters of the particles comprising this component decrease.
- the viscosities of the resulting slurries increase rapidly as the proportion of the suspended solid component is increased.
- a concentration is readily obtained which results in the slurry becoming so viscous, immobile and plastic that it can be neither mixed, molded nor transferred to molds for shaping in articles of the desired dimensions and mass.
- Agents which can be employed to effectively eliminate water contamination and maintain protective coatings on the newly created surfaces of pulverized materials are composed of dipole molecules, i.e., one terminal group capable of adsorbing with high energy of adhesion to the surface of the suspended infusible component and other molecular groupings capable of orienting the molecule to the fusible component.
- R is an alkyl group or hydrogen atom
- R is substituted or unsubstituted aryl or polyaryl nucleus.
- R is an alkylene group of from 2 to 18 carbon atoms
- X is a polar group, such as hydroxy, halide, nitrate, sulfonate, sulfate or phosphate radical.
- the phenyloxy alkanols have been found to be particularly suitable.
- the phenyloxy alkanols which are preferable having boiling points in the range of 100 C. to 300 C. at a pressure of millimeters of mercury, molecular weights in the range of 124 to 400 and fire points above 100 C.
- these compounds are readily soluble in organic solvents such as carbon tetrachloride, naptha, acetone, ethanol and other alcohols, while at the same time difiicultly soluble in 'water.
- Phenyloxyoctanol Several methods of deposing surface conditioning agents on to newly created surfaces of infusible components have been divided. One effective method is to add the conditioning agent to a volatile solvent, which, after deposition of the agent, may be readily removed by evaporation.
- the agent may be vaporized at atmospheric pressure and allowed to condense on to the freshly ground infusible component contained in an adsorption train.
- the vaporization may be produced by an external source of heat or, by the heat resulting from the mechanical work done in grinding.
- the agent may be combined with the unground material, and, during the process of grinding, is then deposited on to the surfaces of the freshly pulverized material, simultaneously with the formation of said surfaces.
- EXAMPLE I Two kilograms of pulverized barium nitrate are dried in an oven at C. for three hours. While still hot, the material is transferred to a distillation receiver which is then connected toa vaporizer containing phenyloxyethanol. The system is evacuated to about 10 mm. mercury absolute pressure and the phenyloxyethanol is heated to about C. The phenyloxyethanol vapor flows into the distillation receiver containing the pulverized barium nitrate and condenses on the dehydrated, cooler surfaces of the barium nitrate, forming an impervious, protective layer on same.
- Another successful method of preparing moisture-avid surfaces of pulverized materials can be had by vaporizing an agent of the desired material into a mill or grinder with the material to be pulverized whereby the vapor condenses on the new surfaces of the pulverulent as they are created by the pulverizing action of the mill.
- EXAMPLE II Five kilograms of dry calcium nitrate are placed in a ball mill fitted with a connection on the upper portion for the admittance of a gas. 250 milliliters of phenyloxyisopropanol are heated in a flask which is connected by means of a flexible tubing to the connection of the grinder. The mill is placed in operation at the time the phenyloxyisopropanol is volatized and the vapor replaces the air within the grinder immediately thereafter. As new surfaces are created by the grinding process the phenyloxyisopropanol vapor coats the new surfaces formed, effectively preventing the adsorption of moisture by said surfaces. In this manner it is virtually impossible for the finely-divided inert material to adsorb moisture or other contaminants before they are protectively coated with the organic material.
- Still another technique applicable to the coating of new surfaces created by comminution is to disperse the conditioning agent or protective coating material in the unground inert material. Transient local temperatures in grinding may reach as high as 175 C. which is sufficient to cause substantial vapor pressure of the agent, or complete vaporization if the agent is selected with a sufficiently low boiling point.
- the following example illustrates the preferred method in which p-methylphenyloxyethanol is selected as the surface conditioning agent.
- EXAMPLE III 1.5 kilogram of ammonium nitrate crystals previously dried for one hour at 105 C. are placed in a ball mill. 25 grams of p-methylphenyloxyethanol are added to the inert material, the mill is closed and rotated at r.p.m. until the unground material is completely pulverized. Heat produced by the grinding process combined with agitation effects substantial vaporization of the p-methylphenyloxyethanol and thus effectively coats all of the newly formed surfaces of the finely comminuted material.
- phenyloxyalkanols may be protectively coated onto pulverized solids in a mill or grinder by directly passing the oxyalkanol into the mill, they may be diluted and vaporized in a stream of hot, inert gas as described in the following example.
- EXAMPLE IV Three kilograms of dry barium nitrate crystals are placed in a suitable enclosed grinder equipped with a gas admittance connection. Terbutylphenyloxyethanol vapor is admixed with nitrogen at a temperature of about 250 C. and admitted into the grinder to replace the normal atmosphere therein. The grinder is placed in operation and the ter-butylphenyloxyethanol-nitrogen gas mixture is permitted to flow into the grinder. Newly created surfaces of barium nitrate are thus effectively coated almost simultaneously with their formation with a thin film of ter-butyloxyethanol and protected from the influence of moisture in the air. The inert nitrogen is then flushed out with air leaving the protectively coated crystal surfaces free of moisture and other contaminants.
- conditioning agents disclosed hereinbefore can be readily deposed in the most mobile phase, that is, the vapor phase, at the time of the formation of newly created surfaces.
- the introduction of the surface conditioning or protective coating agents in the gaseous phase for adsorption on the surface of newly comminuted materials can be performed with standard laboratory equipment.
- the method greatly retards their subsequent contamination by air, water or other undesirable components, and substantially eliminates the nuisance usually associated with the adsorption of said contaminants by freshly comminuted materials.
- the method therefore lends itself to wide and diverse applications for the control of surface characteristics of finely ground materials such as pigments, metallic powders, dusting materials and the like. Slight excesses of conditioning agents are not harmful in most applications of the method. Ionic, valence and other crystals treated in the manner disclosed hereinbefore are thus protectively coated against moisture adsorption and can readily be dispersed in any explosive component for the formation of moldable and castable explosive charges useful in sundry ordnance materials.
- a method of coating comminuted materials with a surface protective agent which comprises contacting .a finely ground solid material with an aryloxy alkanol having a boiling point substantially below the melting point of the comminuted material.
- a method of coating freshly pulverized particles by deposition of surface protective agents thereon which comprises contacting a freshly ground solid material with a substituted aryloxy alkanol having a mm. mercury boiling point of at least 100 C.
- a method of coating newly formed pulverized particles of deposition of surface protective agents thereon which comprises contacting a freshly ground solid material with the vapor of any aryloxyalkanol having a molecular weight of at least 124 and not in excess of 400.
- a method of protectively coating freshly comminuted surfaces of moisture-avid materials which comprises volatilizing a protective substituted oxyalkanol in the presence of the freshly comminuted material.
- a method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting a newly comminuted material with the vapor of phenyloxyalkanols having a molecular weight of at least 124.
- a method of protectively coating the surfaces of newly comminuted materials which comprises mixing a low boiling phenyloxyalkanol with the unground material, comminuting the unground material to a finely-divided state whereby the phenyloxyalkanol is vaporized by the heat produced by comminution and is intimately dispensed throughout the comminuted material.
- a method of protectively coating the surfaces of newly comminuted moisture-avid materials against the adsorption of moisture which comprises contacting the surface of a newly comminuted material with the vapor of a phenyloxyalkanol having a molecular weight of at least 124, said protective coating vapor being in contact with said surfaces of the newly comminuted material at the instant of formation of said surfaces of said newly comminuted material.
- a method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with a gaseous mixture comprising ,an inert gas and the vapor of a phenyloxyalkanol having a molecular weight of at least 124, said gaseous mixture elevated to a temperature sufficiently above the melting point of said phenyloxyalkanol at the instant of contact of said phenyloxyalkanols with said surfaces of the newly comminuted material.
- a method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with a gaseous mixture comprising an inert gas and the vapor of a phenyloxyalkanol having a molecular Weight of at least 124, said gaseous mixture elevated to a temperature sufficiently above the melting point of said substituted phenyloxyalkanol at the instant of contact of said 'subsitued phenyloxyalkanol with said surfaces of the newly comminuted material.
- a method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with the vapor of a substituted aryloxyalkanol having a molecular weight of at least 124, said protective coating vapor being present at the instant of formation of said surfaces of said newly comminuted material.
- a method of protectively coating the surfaces of newly comminuted moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with the vapor of a para-substituted phenyloxyalkanol having a molecular weight of at least 124, said protective coating vapor being present at the instant of formation of 'said surfaces of said newly comminuted material.
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- Organic Chemistry (AREA)
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Description
3,402,065 PHENYLOXYALKANOL COATING F PARTICLE Louis McDonald, Inyokern, and Norman A. MacLeod, Altadena, Calif., assignors to the United States of America as represented by the United States Atomic Energy Commission No Drawing. Filed Jan. 23, 1950, Ser. No. 140,148
12 Claims. (Cl. 117-100) This invention relates to surface conditioning materials and more particularly to a method of treatment of inv fusible pulverized mixtures. Specifically, this invention relates to a method and agents for protectively preparing the surfaces of pulverized materials so as to facilitate their ready incorporation into slurries which may be molded or cast into shaped articles.
The addition of an inert material to explosive compositions has been found useful as a means of regulating the rate and brisance of a detonation. The normal method of incorporating the inert material into the explosive com position is to add it in a finely-divided state to a melt or a solution of the explosive material to form a slurry having the desired proportions of the suspended inert component for the particular purposes at hand.
Furthermore, it is well known that detonation velocities, blast characteristics and brisance of cast or molded charges are significantly affected by the chemical composition and mass and degree of subdivision of the suspended inert component of explosive slurry which is utilized in the preparation of the explosive charge.
It has been further established that the suspended inert material must be introduced in a finely-divided state and preferably should be dispersed as thoroughly as possible throughout the fusible component to produce on cooling a solidified charge having a minimum porosity and a maximum uniformity of compositions. Such a composition is desirable only if there is no separation of the suspended component from the fusible component during the cycles of mixing, molding or casting the slurry into desired shapes.
Also, it has been determined that the presence of rather small amounts of moisture in a slurry may have extremely deleterious effects on the processing of many explosive compositions. Moisture present in the components of the explosive mixture may result in such increased viscosities in a slurry that it is difficult to insure proper mixing of the slurry and satisfactory molding into the desired dimension and mass. In every case, erratic results are obtained from the detonation of explosive castings which are cracked, chipped or which lack uniformity of composition.
This invention provides a method and agents to overcome this last mentioned difiiculty and will be disclosed in more detail following a delineation of the objects of this invention.
It is a primary object of this invention to provide a method for protectively preparing the surface of comminuted explosive components so as to facilitate their ready incorporation into a slurry.
It is an object of this invention to provide a method for protectively preparing newly-developed surfaces of comminuted materials against the adsorption of contaminants until said pulverized materials are incorporated into a slurry.
It is another object of this invention to provide a method for deposing surface conditioning agents on to newlycreated surfaces of finely-divided infusible materials.
It is another object of this invention to provide a class of compounds which are set forth as successful surface conditioning agents.
It is still another object of this invention to provide a nited States Patent Olfice 3,402,065 Patented Sept. 17, 1968 preferred class of compounds which have proven especially suitable as surface conditioning agents.
Still other objects will become apparent from the description and examples which follow.
The successful preparation of slurries containing dispersed solids is dependent, in part, upon the surface characteristics of the suspended particles, and upon such factors as the quantity of the solid or infusible component, the degree of subdivision and the completeness of dispersing the infusible component throughout the fusible explosive component. Maximum uniformity of slurry composition is obtained by introducing the solid component in a finely-divided form and dispersing it as thoroughly as possible in the fusible vehicle.
The specific surface of any solid comminuted component increases as the mean diameters of the particles comprising this component decrease. When powders of high specific surfaces are dispersed in fusible vehicles the viscosities of the resulting slurries increase rapidly as the proportion of the suspended solid component is increased. A concentration is readily obtained which results in the slurry becoming so viscous, immobile and plastic that it can be neither mixed, molded nor transferred to molds for shaping in articles of the desired dimensions and mass. By the addition of small amounts of dispersing agents, phase boundary lubricants, or other conditioning agents, such as nitrocellulose, benzocellulose and the like, it is possible to greatly increase the concentration of suspended solids in a specific slurry without significant effect on the chemical and physical properties of the product resulting therefrom. Thus the proper use of surface conditioning agents and/or phase boundary lubricants make possible the processing of slurries containing high concentrations of suspended pulverized materials of high specific surface which show maximum uniformity of composition and little or no tendency to segregate during the molding or mixing cycles.
In the preparation of comminuted materials, new surfaces are created on the cleavage planes of the crystals which have a particular avidity for moisture and other contaminants. This is especial-1y true when the non-fusible components is ground into finely comminuted particles of high specific surface before their incorporation in the fusible vehicle. Moisture present in the atmosphere or in other components of the mixture is most readily absorbed on the newly created surface planes of the crystals in the form of monomolecular or polymolecular layers. Such adsorption, even in minute quantities may have exteremely adverse effects on the resulting cast or molded product.
As the energy of desorption of moisture to ionic and other crystal surfaces is greater than the energy of adsorption of usable phase lubricants or dispersing agents, the types of surface active materials heretofore employed cannot function in the desired manner when even monomolecular layers of water are absorbed on the surface of the particles to be dispersed. Consequently, it is extremely difiicult to process some slurries containing high proportions of high specific surface particles when moisture in amounts of the order of 0.02 percent or more is present.
It has been found that certain materials which desirably function as conditioning agents and/or surface pro tective agents can be deposited in the vapor phase or liquid phase, either alone or mixed with a suitable inert diluent, as a vehicle, on the newly created surface of ionic, covalent, or molecular crystals at the time of their formation by plane cleavage or other means. As the deposed protection agents exhibit a high energy of adsorption to the noted classes of materials, preferential desorption and replacement by water molecules is not readily achieved. Thus it is seen that advantage is taken of the avidity of such newly developed surfaces before said surfaces can be contaminated by water or other contaminants.
Agents which can be employed to effectively eliminate water contamination and maintain protective coatings on the newly created surfaces of pulverized materials are composed of dipole molecules, i.e., one terminal group capable of adsorbing with high energy of adhesion to the surface of the suspended infusible component and other molecular groupings capable of orienting the molecule to the fusible component.
Compounds of the general formula have been founnd to be effective. R is an alkyl group or hydrogen atom, R is substituted or unsubstituted aryl or polyaryl nucleus. is an oxygen, nitrogen, sulphur, or phosphorous atom, R is an alkylene group of from 2 to 18 carbon atoms and X is a polar group, such as hydroxy, halide, nitrate, sulfonate, sulfate or phosphate radical.
Of the preferred components, the phenyloxy alkanols have been found to be particularly suitable. The phenyloxy alkanols which are preferable having boiling points in the range of 100 C. to 300 C. at a pressure of millimeters of mercury, molecular weights in the range of 124 to 400 and fire points above 100 C. In addition, these compounds are readily soluble in organic solvents such as carbon tetrachloride, naptha, acetone, ethanol and other alcohols, while at the same time difiicultly soluble in 'water.
Examples of aryl oxyalkanols which may effectively be employed to coat ionic, valence and other types of solids are tabulated hereinbelow:
Phenyloxyoctanol Several methods of deposing surface conditioning agents on to newly created surfaces of infusible components have been divided. One effective method is to add the conditioning agent to a volatile solvent, which, after deposition of the agent, may be readily removed by evaporation.
This invention discloses other methods for efficaciously deposing the surface active agent on to the newly formed surfaces. For example, the agent may be vaporized at atmospheric pressure and allowed to condense on to the freshly ground infusible component contained in an adsorption train. The vaporization may be produced by an external source of heat or, by the heat resulting from the mechanical work done in grinding. For example, by the proper selection of a surface active agent having a sufficiently low temperature of vaporization, the agent may be combined with the unground material, and, during the process of grinding, is then deposited on to the surfaces of the freshly pulverized material, simultaneously with the formation of said surfaces.
Other methods of coating newly formed surfaces have been developed, such as passing high boiling phenyloxyalkanols'over the newly formed surfaces by means of an inert vehicle such as helium or nitrogen at an elevated temperature. Crystal particles treated in this manner are effectively coated against the adsorption of moisture and other contamination and the protected pulverized material can be readily processed into products utilizing powdered infusible materials or safely stored for future use.
The following examples will serve to illustrate with greater clarity the facility of the methods of this invention.
EXAMPLE I Two kilograms of pulverized barium nitrate are dried in an oven at C. for three hours. While still hot, the material is transferred to a distillation receiver which is then connected toa vaporizer containing phenyloxyethanol. The system is evacuated to about 10 mm. mercury absolute pressure and the phenyloxyethanol is heated to about C. The phenyloxyethanol vapor flows into the distillation receiver containing the pulverized barium nitrate and condenses on the dehydrated, cooler surfaces of the barium nitrate, forming an impervious, protective layer on same.
Another successful method of preparing moisture-avid surfaces of pulverized materials can be had by vaporizing an agent of the desired material into a mill or grinder with the material to be pulverized whereby the vapor condenses on the new surfaces of the pulverulent as they are created by the pulverizing action of the mill.
EXAMPLE II Five kilograms of dry calcium nitrate are placed in a ball mill fitted with a connection on the upper portion for the admittance of a gas. 250 milliliters of phenyloxyisopropanol are heated in a flask which is connected by means of a flexible tubing to the connection of the grinder. The mill is placed in operation at the time the phenyloxyisopropanol is volatized and the vapor replaces the air within the grinder immediately thereafter. As new surfaces are created by the grinding process the phenyloxyisopropanol vapor coats the new surfaces formed, effectively preventing the adsorption of moisture by said surfaces. In this manner it is virtually impossible for the finely-divided inert material to adsorb moisture or other contaminants before they are protectively coated with the organic material.
Still another technique applicable to the coating of new surfaces created by comminution is to disperse the conditioning agent or protective coating material in the unground inert material. Transient local temperatures in grinding may reach as high as 175 C. which is sufficient to cause substantial vapor pressure of the agent, or complete vaporization if the agent is selected with a sufficiently low boiling point. The following example illustrates the preferred method in which p-methylphenyloxyethanol is selected as the surface conditioning agent.
EXAMPLE III 1.5 kilogram of ammonium nitrate crystals previously dried for one hour at 105 C. are placed in a ball mill. 25 grams of p-methylphenyloxyethanol are added to the inert material, the mill is closed and rotated at r.p.m. until the unground material is completely pulverized. Heat produced by the grinding process combined with agitation effects substantial vaporization of the p-methylphenyloxyethanol and thus effectively coats all of the newly formed surfaces of the finely comminuted material.
While phenyloxyalkanols may be protectively coated onto pulverized solids in a mill or grinder by directly passing the oxyalkanol into the mill, they may be diluted and vaporized in a stream of hot, inert gas as described in the following example.
EXAMPLE IV Three kilograms of dry barium nitrate crystals are placed in a suitable enclosed grinder equipped with a gas admittance connection. Terbutylphenyloxyethanol vapor is admixed with nitrogen at a temperature of about 250 C. and admitted into the grinder to replace the normal atmosphere therein. The grinder is placed in operation and the ter-butylphenyloxyethanol-nitrogen gas mixture is permitted to flow into the grinder. Newly created surfaces of barium nitrate are thus effectively coated almost simultaneously with their formation with a thin film of ter-butyloxyethanol and protected from the influence of moisture in the air. The inert nitrogen is then flushed out with air leaving the protectively coated crystal surfaces free of moisture and other contaminants.
It is thus seen that many advantages of the method of the present invention are possible. The conditioning agents disclosed hereinbefore can be readily deposed in the most mobile phase, that is, the vapor phase, at the time of the formation of newly created surfaces.
The introduction of the surface conditioning or protective coating agents in the gaseous phase for adsorption on the surface of newly comminuted materials can be performed with standard laboratory equipment.
By prior coating of the adsorption-avid new surfaces, the method greatly retards their subsequent contamination by air, water or other undesirable components, and substantially eliminates the nuisance usually associated with the adsorption of said contaminants by freshly comminuted materials. The method therefore lends itself to wide and diverse applications for the control of surface characteristics of finely ground materials such as pigments, metallic powders, dusting materials and the like. Slight excesses of conditioning agents are not harmful in most applications of the method. Ionic, valence and other crystals treated in the manner disclosed hereinbefore are thus protectively coated against moisture adsorption and can readily be dispersed in any explosive component for the formation of moldable and castable explosive charges useful in sundry ordnance materials.
While many embodiments of the methods and compositions of matter are possible, it is to be understood that the present invention is not limited except as indicated in the appended claims.
What is claimed is:
1. A method of coating comminuted materials with a surface protective agent which comprises contacting .a finely ground solid material with an aryloxy alkanol having a boiling point substantially below the melting point of the comminuted material.
2. A method of coating newly comminuted materials with a surface protective agent which comprsies contacting a newly comminuted material with a liquid phenyloxyalkanol.
3. A method of coating freshly pulverized particles by deposition of surface protective agents thereon which comprises contacting a freshly ground solid material with a substituted aryloxy alkanol having a mm. mercury boiling point of at least 100 C.
4. A method of coating newly formed pulverized particles of deposition of surface protective agents thereon which comprises contacting a freshly ground solid material with the vapor of any aryloxyalkanol having a molecular weight of at least 124 and not in excess of 400.
5. A method of protectively coating freshly comminuted surfaces of moisture-avid materials which comprises volatilizing a protective substituted oxyalkanol in the presence of the freshly comminuted material.
6. A method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting a newly comminuted material with the vapor of phenyloxyalkanols having a molecular weight of at least 124.
7. A method of protectively coating the surfaces of newly comminuted materials which comprises mixing a low boiling phenyloxyalkanol with the unground material, comminuting the unground material to a finely-divided state whereby the phenyloxyalkanol is vaporized by the heat produced by comminution and is intimately dispensed throughout the comminuted material.
8. A method of protectively coating the surfaces of newly comminuted moisture-avid materials against the adsorption of moisture which comprises contacting the surface of a newly comminuted material with the vapor of a phenyloxyalkanol having a molecular weight of at least 124, said protective coating vapor being in contact with said surfaces of the newly comminuted material at the instant of formation of said surfaces of said newly comminuted material.
9. A method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with a gaseous mixture comprising ,an inert gas and the vapor of a phenyloxyalkanol having a molecular weight of at least 124, said gaseous mixture elevated to a temperature sufficiently above the melting point of said phenyloxyalkanol at the instant of contact of said phenyloxyalkanols with said surfaces of the newly comminuted material.
10. A method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with a gaseous mixture comprising an inert gas and the vapor of a phenyloxyalkanol having a molecular Weight of at least 124, said gaseous mixture elevated to a temperature sufficiently above the melting point of said substituted phenyloxyalkanol at the instant of contact of said 'subsitued phenyloxyalkanol with said surfaces of the newly comminuted material.
11. A method of protectively coating the surfaces of newly comminuted, moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with the vapor of a substituted aryloxyalkanol having a molecular weight of at least 124, said protective coating vapor being present at the instant of formation of said surfaces of said newly comminuted material.
12. A method of protectively coating the surfaces of newly comminuted moisture-avid materials against the adsorption of moisture which comprises contacting the surfaces of a newly comminuted material with the vapor of a para-substituted phenyloxyalkanol having a molecular weight of at least 124, said protective coating vapor being present at the instant of formation of 'said surfaces of said newly comminuted material.
References Cited UNITED STATES PATENTS 6/ 1945 Burdett et al. 52-21 7/1919 Snelling 117-100
Claims (2)
1. A METHOD OF COATING COMMINUTED MATERIALS WITH A SURFACE PROTECTIVE AGENT WHICH COMPRISES CONTACTING A FINELY GROUND SOLID MATERIAL WITH AN ARYLOXY ALKANOL HAVING A BOILING POINT SUBSTANTIALLY BELOW THE MELTING POIN OF THE COMMINUTED MATERIAL.
4. A METHOD OF COATING NEWLY FORMED PULVERIZED PARTICLES OF DEPOSITION OF SURFACE JPROTECTIVE AGENTS THEREON WHICH COMPRISES JCONTACTING A FRESHLY GROUND SOLID MATERIAL WITH THE VAPOR OF ANY ARYLOXYALKANOL HAVING A MOLECULAR WEIGHT OF AT LEAST 124 AND NOT IN EXCESS OF 400.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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US140148A US3402065A (en) | 1950-01-23 | 1950-01-23 | Phenyloxyalkanol coating of particle |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US140148A US3402065A (en) | 1950-01-23 | 1950-01-23 | Phenyloxyalkanol coating of particle |
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US3402065A true US3402065A (en) | 1968-09-17 |
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US140148A Expired - Lifetime US3402065A (en) | 1950-01-23 | 1950-01-23 | Phenyloxyalkanol coating of particle |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3523839A (en) * | 1962-09-17 | 1970-08-11 | Union Carbide Corp | Encapsulation of rocket and missile fuels with metallic and polymeric coatings |
US4073977A (en) * | 1975-08-07 | 1978-02-14 | Basf Aktiengesellschaft | Stabilization of pyrophoric metal powders with alkylene oxide polymers |
US4115166A (en) * | 1970-01-12 | 1978-09-19 | Aerojet-General Corporation | Coated ammonium perchlorate |
US4175143A (en) * | 1979-01-02 | 1979-11-20 | Gte Sylvania Incorporated | Color cathode ray tube phosphors coated by a wetting agent |
US4342797A (en) * | 1979-07-05 | 1982-08-03 | Apollo Technologies, Inc. | Wet flow characteristic of coal and other water-insoluble solid particles |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1310037A (en) * | 1919-07-15 | Coating process and apparatus | ||
US2377670A (en) * | 1943-08-26 | 1945-06-05 | Remington Arms Co Inc | Ammunition priming mixtures |
-
1950
- 1950-01-23 US US140148A patent/US3402065A/en not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1310037A (en) * | 1919-07-15 | Coating process and apparatus | ||
US2377670A (en) * | 1943-08-26 | 1945-06-05 | Remington Arms Co Inc | Ammunition priming mixtures |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3523839A (en) * | 1962-09-17 | 1970-08-11 | Union Carbide Corp | Encapsulation of rocket and missile fuels with metallic and polymeric coatings |
US4115166A (en) * | 1970-01-12 | 1978-09-19 | Aerojet-General Corporation | Coated ammonium perchlorate |
US4073977A (en) * | 1975-08-07 | 1978-02-14 | Basf Aktiengesellschaft | Stabilization of pyrophoric metal powders with alkylene oxide polymers |
US4175143A (en) * | 1979-01-02 | 1979-11-20 | Gte Sylvania Incorporated | Color cathode ray tube phosphors coated by a wetting agent |
US4342797A (en) * | 1979-07-05 | 1982-08-03 | Apollo Technologies, Inc. | Wet flow characteristic of coal and other water-insoluble solid particles |
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