WO2017070406A1 - Procédé de production de particules solides - Google Patents
Procédé de production de particules solides Download PDFInfo
- Publication number
- WO2017070406A1 WO2017070406A1 PCT/US2016/058005 US2016058005W WO2017070406A1 WO 2017070406 A1 WO2017070406 A1 WO 2017070406A1 US 2016058005 W US2016058005 W US 2016058005W WO 2017070406 A1 WO2017070406 A1 WO 2017070406A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- liquid
- solid
- solid particles
- energy source
- produced
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 116
- 239000007787 solid Substances 0.000 title claims abstract description 104
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000007788 liquid Substances 0.000 claims abstract description 73
- 238000000034 method Methods 0.000 claims abstract description 61
- 238000009826 distribution Methods 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims description 45
- 239000011347 resin Substances 0.000 claims description 45
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
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- BVQVLAIMHVDZEL-UHFFFAOYSA-N 1-phenyl-1,2-propanedione Chemical compound CC(=O)C(=O)C1=CC=CC=C1 BVQVLAIMHVDZEL-UHFFFAOYSA-N 0.000 description 2
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical class C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 2
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- ZXHDVRATSGZISC-UHFFFAOYSA-N 1,2-bis(ethenoxy)ethane Chemical class C=COCCOC=C ZXHDVRATSGZISC-UHFFFAOYSA-N 0.000 description 1
- VNQXSTWCDUXYEZ-UHFFFAOYSA-N 1,7,7-trimethylbicyclo[2.2.1]heptane-2,3-dione Chemical compound C1CC2(C)C(=O)C(=O)C1C2(C)C VNQXSTWCDUXYEZ-UHFFFAOYSA-N 0.000 description 1
- VOBUAPTXJKMNCT-UHFFFAOYSA-N 1-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound CCCCCC(OC(=O)C=C)OC(=O)C=C VOBUAPTXJKMNCT-UHFFFAOYSA-N 0.000 description 1
- ZWVHTXAYIKBMEE-UHFFFAOYSA-N 2-hydroxyacetophenone Chemical compound OCC(=O)C1=CC=CC=C1 ZWVHTXAYIKBMEE-UHFFFAOYSA-N 0.000 description 1
- 238000010146 3D printing Methods 0.000 description 1
- AKQVBBOVHAEKMA-UHFFFAOYSA-N 4-ethenoxybutyl benzoate Chemical compound C=COCCCCOC(=O)C1=CC=CC=C1 AKQVBBOVHAEKMA-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- XWUNIDGEMNBBAQ-UHFFFAOYSA-N Bisphenol A ethoxylate diacrylate Chemical compound C=1C=C(OCCOC(=O)C=C)C=CC=1C(C)(C)C1=CC=C(OCCOC(=O)C=C)C=C1 XWUNIDGEMNBBAQ-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229920002633 Kraton (polymer) Polymers 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 244000028419 Styrax benzoin Species 0.000 description 1
- 235000000126 Styrax benzoin Nutrition 0.000 description 1
- 239000002174 Styrene-butadiene Substances 0.000 description 1
- 235000008411 Sumatra benzointree Nutrition 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical class NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000008062 acetophenones Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 150000008365 aromatic ketones Chemical class 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 229960002130 benzoin Drugs 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229930006711 bornane-2,3-dione Natural products 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
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- ISAOCJYIOMOJEB-UHFFFAOYSA-N desyl alcohol Natural products C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 1
- 125000004386 diacrylate group Chemical group 0.000 description 1
- 239000012955 diaryliodonium Substances 0.000 description 1
- 125000005520 diaryliodonium group Chemical group 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 235000019382 gum benzoic Nutrition 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- 238000010329 laser etching Methods 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
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- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical class [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
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- 229920002223 polystyrene Polymers 0.000 description 1
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- 229920002635 polyurethane Polymers 0.000 description 1
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- 238000003908 quality control method Methods 0.000 description 1
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- 150000003254 radicals Chemical class 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
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- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
- B29C64/129—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
- C08F222/1025—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate of aromatic dialcohols
Definitions
- Photocuring resins are widely used in the coatings industry as they do not require volatile organic solvents which can pose environmental and safety hazards. Curing of uniform layers is usually performed as a protective coating.
- Photocuring resins are also widely used in 3D printing and additive manufacturing techniques. Printing is performed in a layer-by-layer process where often many hundreds of layers are required to achieve sub millimeter resolution of even small models. Much emphasis in the additive manufacturing industry is placed on printing larger and larger objects with almost no examples of mass production of small objects.
- LCM loss circulation materials
- LCM LCM is often supplied as dry particulates in sacks and is kept at the rig-site as an insurance against lost circulation events. Deliveries of LCM from regional warehouses is periodic, so rig site managers must estimate what products they may need and are prepared to store.
- LCM products are very low cost and may be waste products of other processes.
- Nutshells, wood fibres, mica, graphite and limestone are all common examples of LCM materials.
- the present disclosure relates to a method of producing a plurality of solid particles or a solid surface of non-uniform depth of predetermined size and shape distribution by exposing a liquid to a first energy source of spatially varying intensity, forming the solid particles or the solid surface of non-uniform depth of pre-determined size and shape distribution. Additionally, the method may also comprise separating the solid particles from the liquid transferring the solid particles into a transparent medium; and exposing the solid particles to a second energy source.
- a first aspect of the present disclosure relates to a method of producing solid particles, comprising: determining size and shape distribution of the solid particles to be produced; exposing a liquid to a first energy source of spatially varying intensity; and forming the solid particles of pre-determined size and shape distribution.
- Liquid is solidified to a depth controlled by intensity of the energy source. Regions of higher intensity result in thicker solidified sections compared to regions of lower intensity. Depth of the resulting solid is therefore controlled spatially by spatial variation in intensity within a single exposure period.
- the method allows for rapid production of small particles of predetermined size and shape distribution in large quantities using a single exposure of the energy source. Additionally, control of other properties of the solid particles such as density, elasticity, and resilience made be achieved by e.g. adjusting the composition of the liquid.
- the method may further comprise: separating the solid particles from the liquid. The solid particles may be separated from the remaining unsolidified liquid by filtration. After separation, the surfaces of the solid particles may still remain covered by a layer of liquid, which may be sticky.
- the method may further comprise: transferring the solid particles into a transparent medium; and exposing the solid particles to a second energy source.
- a second step exposure to a second energy source may be performed to solidify the surface layer, thus reducing the stickiness of the surfaces of the solid particles according to requirements. This also allows the core of the solid particles to be further hardened according to requirements.
- the transparent medium may be a transparent liquid, or an Oxygen free gaseous environment.
- Oxygen inhibits the solidification of the liquid, therefore an Oxygen free environment allows the surfaces of the particles to be solidified to reduce the stickiness of the surfaces in at least some embodiments.
- An environment comprising Oxygen may be chosen if sticky surfaces are desirable. Therefore in some embodiments, the transparent medium may be an environment with a controlled oxygen concentration. The stickiness of the surfaces can be adjusted by controlling the amount of Oxygen in the environment.
- the liquid may be a photocuring resin and the first energy source may be a collimated light source of spatially varying light intensity.
- the collimated light source of spatially varying light intensity may be provided by a light mask and a uniform intensity light source, or an electronically controlled image projection system, or two or more intersecting beams.
- the liquid may be a heat triggered resin and the first energy source may be infrared source of spatially varying light intensity or an infrared laser scanned to create time- averaged spatially varying intensity.
- This method may be used to simultaneously produce a plurality of small solid particles by exposing the liquid to the first energy source once.
- the size of the solid particles depends on their intended application.
- the maximum Feret diameter of each solid particle may be less than 100mm.
- the maximum Feret diameter of each solid particle may be less than 60mm.
- the maximum Feret diameter of each solid particle is preferably less than 20mm. More preferably, the maximum Feret diameter of each solid particle may be less than 10mm.
- the method may further comprise: providing a surface on which the solid particles are formed.
- the surface may be an oxygen permeable surface.
- Oxygen can limit the solidification of a layer of liquid in a region close to the surface. Oxygen permeability of the surface can therefore limit adhesion between the desired obj ect and the supporting surface. In the absence of oxygen the solid particles may strongly adhere to the surface, making it difficult to remove the particles from the surface.
- Each solid particle may be formed by exposing the liquid to the first energy source by a predetermined time and the predetermined time for each solid particle may be the same.
- the method may further comprise: calculating the energy output of the first energy source of spatially varying intensity and the predetermined time needed for each solid particle based on the predetermined size and shape distribution of the solid particles to be produced.
- the energy output of the first energy source of spatially varying intensity and the predetermined time needed for each solid particle would also depend on the nature of liquid, the nature of the first energy source, temperature, pressure and other environmental factors.
- the method may further comprise: moving the surface laterally in between the first energy source and the liquid. As the surface moves into the active region in between the first energy source and the liquid, the liquid is solidified into particles of predetermined sizes and shapes. As the surface moves away, it carries with it solid particles already formed and leaves the active region to be occupied by empty surface areas moving into the region. This allows even faster production of solid particles when an even larger quantity is needed.
- the movement may be periodic or continuous.
- the movement may be periodic. A surface may be completely exposed before it is removed. A new surface is then placed in between the first energy source and the liquid to be exposed.
- the movement of the surface may be continuous, while the liquid is made to circulate in the same direction as the surface whereby reducing relative movement between the surface and the liquid, or eliminating relative movement if the liquid also circulates at the same speed as the surface.
- the first energy source may be turned off after a surface is completely exposed, and turned on again after a new surface is in place.
- a second aspect of the present disclosure relates to a method of producing a solid surface with non-uniform depth, comprising: determining size and depth distribution of the solid surface to be produced; exposing a liquid to a first energy source of spatially varying intensity; and forming the solid surface with the predetermined size and depth distribution.
- the method may further comprise: separating the solid surface with non-uniform depth from the liquid.
- the continuous surface with non-uniform depth may be the desirable final product.
- a mould may be produced using the solid surface with non-uniform depth produced as a template. The mould may then be used to give shape to a hardening liquid which could be a molten material or a liquid solidified by chemical or actinic radiation.
- Fig 1 shows single exposure manufacture of 3D particle shapes in example 2.
- Fig 2 shows depth control of curing in example 3.
- Fig 3 shows block testing of pyramid LCM in example 4.
- Fig 4 shows a selection of particle shapes produced in example 5.
- Fig 5 shows exposure using two intersecting beams in example 6.
- Fig 6 shows a sketch of an apparatus allowing continuous production of solid particles.
- Fig 7 shows a picture of an apparatus allowing continuous production of solid particles.
- Fig 8 shows a sketch of a machine comprising ten apparatus each allowing continuous production of solid particles.
- the present disclosure relates to a method for producing small polymer obj ects e.g. ⁇ 10mm in large quantities, rapidly e.g. ⁇ 5mins with low cost equipment such as patterned light source.
- the method produces solid polymer objects from a liquid photocuring resin cured using a light source with controlled spatial intensity.
- a range of precise shapes can be produced in a simple process that can be rapidly reconfigured.
- Spatial light intensity can be controlled using a collimated light source and light mask or dynamically by a projection system.
- a greyscale light mask for generating tetrapods is shown to produce different size objects by changing only the light exposure time. Controlling light paths in the curing process allows wider range of particle shapes to be produced.
- the current disclosure achieves a similar resolution to existing state of the art 3D printers using e.g. photocuring resins, but in a single exposure method at least 2 orders of magnitude faster.
- the technique is ideally suited to mass production of small shapes where rapid manufacture of bespoke particle shapes and sizes is an advantage. Changes to the particle size can be achieved with a single greyscale light mask by changing only the light intensity. Changes to particle shape can easily be achieved with an image projection system.
- the liquid may be any suitable photocuring resin and the first energy source may be a collimated light source of spatially varying light intensity. Suitable photoinitiators may be added to the resin mixture.
- Suitable resin examples include:
- VectomersTM vinyloxybutyl benzoate and bis and tris variants.
- Ethylene glycol divinyl ethers (varying molecular weight) • Vinyl functionalised polymers and oligomers such as polybutadienes or polyisoprenes, block copolymers such as styrene- butadiene, SEBS, SIS ... examples given by the Kraton polymers. They are primarily solvated in nonaqueous base fluids and would be especially useful for OBM.
- Suitable photoinitiators include:
- Type I cleavable typically benzoin ethers, dialkoxy acetophenones , phosphine oxide derivatives, amino ketones.
- Type II hydrogen abstraction or electron transfer typically aromatic ketones e.g. camphorquinone, anthraquinone, 1 -phenyl 1,2 propanedione, 2, combined with H donors such as alcohols, or electron donors such as amines.
- aromatic ketones e.g. camphorquinone, anthraquinone, 1 -phenyl 1,2 propanedione, 2, combined with H donors such as alcohols, or electron donors such as amines.
- Photoacid generators typically Diazonium or Onium salts eg diaryliodonium or triarylsulphonium PF6.
- Density of the solid particles to be produced can be adjusted by adding additives to the resin formulation.
- additives for example, silica can be added to increase density, and porous powders can be added to decrease the density.
- Additives can also be used to increase the brittleness, strength and abrasion resistance e.g. by adding silica or powdered plastic.
- the method may comprise the following steps:
- Step 1 Liquid photocuring resin is exposed to collimated light at a surface with spatially varied light intensity. Spatial variation of light intensity can be achieved by a light mask and a uniform intensity light source OR an electronically controlled image projection system such as a data projector. Curing commences at the surface closest to the light source and propagates at a rate determined by the light intensity. The curing process has been shown to incorporate a delay and a predictable rate allowing for single exposure curing of a range of 3D shapes.
- a grey scale mask can be a separate sheet from the surface on which the solid particles are to be produced. It should be placed in between the light source and the liquid.
- a grey scale mask can be part of the surface, e.g. it can be printed on the surface.
- High quality inkj et printing (>600dpi) may be used to achieve this.
- laser etching chemical etching
- even ebeam lithography There are also other methods like laser etching, chemical etching and even ebeam lithography.
- the range of 3D shapes is expanded. This may include curing resin between two illuminated surfaces to achieve more complex shapes as required.
- Curing surfaces could also be modified to control geometry. For instance curing through a window of hemispherical indentations in an array to create particles with curved surfaces.
- Shapes of equivalent precision and size produced by our commercial 3D printer would typically be made of 100 layers taking several hours and would need support material removed in a lengthy caustic washing process. ( ⁇ 3 days).
- the current disclosure requires a single exposure that has been shown to be as short as 8seconds in lab experiments. No support material is required however solid particles must be removed from uncured resin in a filtration process (currently -10 mins). Curing rates are sensitive to the resin formulation and temperature. In addition to formulation and temperature control, consistent particle size manufacture may require size feedback and compensation of the average light exposure intensity and time.
- Cured solid particles are removed from the uncured liquid resin by filtration.
- a surface which is oxygen permeable (most polymers) curing immediately adjacent to the illuminated surface is limited by trace oxygen and cured particles are not adhered, making separation from the surface unnecessary. Particles will suspend and flow with the liquid resin. If the particles are preferably produced on an oxygen impermeable surface they may be strongly adhered and hence may be damaged on removal by a scraping device.
- Filtration will leave a layer of liquid resin around each solid particle.
- the particles could be directly dispersed into a drilling fluid, however it may be preferable to disperse them in a transparent liquid so that the uncured liquid resin layer can be further exposed to light and solidify.
- the degree to which the sticky liquid resin is cured to the less sticky solid state could control the stickiness of the particles themselves which may prove advantageous when sealing fractures.
- Fig 1 shows single exposure manufacture of 3D particle shapes.
- Experimental temperature is 22deg C (+-2 deg C).
- Resin 55 contained in a polystyrene petri dish is exposed to light intensity 15000 LUX, light source CREE XM-L white light LED driven at 0.6 Amp
- C Pyramids are filtered off and separated from the uncured resin that can be reused.
- Fig 2 shows depth control of curing.
- Resin formulation 55 (see example 2 above) was cured at 22 Deg C, using Laser (540nm, ⁇ lmW). Pillar of 8mm long was produced after exposure of 16 seconds.
- the photocuring resin absorption spectrum in Fig 2A shows absorption of blue-green light by resin 55.
- Resin formulation 30 was cured at 22 Deg C using white light source DELL 2400MP, light intensity 32000 LUX at sample. Exposure times are shown on the graph.
- the depth of cure is controlled by both the light exposure time (30-120 secoonds) and the light intensity (30-100% arb).
- Resin 55 was cured at 22 Deg C using light intensity 15000 LUX, light source CREE XM-L white light LED 0.6Amp. Tetrapods with 3mm edges were produced after 30s exposure. Light mask for terapods with 5mm edges, linear gradient (30% edge to 100% centre) were used.
- Using a greyscale mask resin is cured to different depths in a single exposure by controlling the spatial light intensity.
- Triangle based pyramids are generated with edges 1.6-1.9 mm in length.
- Fig 3 shows block testing results of pyramid LCM.
- the base fluid used was "Rheliant" oil based mud with 200g/L barite and 10 ppb G Seal+ added.
- the block was a 6" cube of sandstone with a 1" bore hole. The block was prefractured and the fracture opened to 1.5mm using brass shims.
- A Stable fluid sealing is achieved up to 150psi only when pyramids are added. Without pyramids the fluid poured freely through the fracture.
- B Images of the fracture and pyramids. Transparent pyramids can be seen near the fracture mouth mixed with black G Seal+ particles.
- the block test proves that particles produced by this method can be effective in sealing large fractures.
- the disclosure provides a method to help achieve the optimal size and shape distribution on-demand without the need for a large inventory of LCM products.
- Fig 4 shows a selection of particle shapes is produced by using different masks.
- Resin formulation 30 was exposed to white light source DELL 2400MP, light intensity 32000 LUX at sample at 22 Deg C for 90sec.
- Particles on the 2-4mm scale are produced from a single exposure of photocuring resin using binary masks(A-I) and greyscale masks(J-N).
- Fig 5 shows double exposure or single simultaneous exposure by two intersected beams.
- Loss circulation might happen during drilling, cementing or after fracturing.
- LCM Long ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇
- LCM of the correct size distribution must be available at surface to add to the drilling fluid as quickly as possible.
- LCM loading in the drilling fluid is often limited by the risk of blocking ("screen out") of the bottom hole assembly (BHA) so control of the size distribution is very important for the LCM to be effective.
- BHA bottom hole assembly
- the largest size fraction of LCM may also be limited by BHA screen out specifications.
- the largest size fractions of LCM need to be made of low density material to limit settling.
- the larger size fraction of the LCM blend (primary bridging particles) can be manufactured to the required size specification on-demand.
- a single batch of liquid photocuring resin could be processed into particles of the desired size and shape as required.
- the photocured LCM is inherently low density (avoids settling issues) and can be tailored precisely, lowering the total LCM concentration required and reducing the risk of BHA blockage.
- LCM size distribution is known to be critical and ideally should be tailored for every use. Current LCM distributions are often limited by LCM stocks. LCM shape is known to be important but currently there are few methods to control this. This method provides the opportunity to control LCM size, size distribution and shape on-demand at the rig site thereby optimizing the LCM performance (minimize loading), reducing rig LCM inventory/space/weight requirements, and simplifying the supply chain.
- the method may further comprise: moving the surface laterally in between the first energy source and the liquid. This allows fast and continuous production of solid particles when an even larger quantity is needed e.g. at a rig site.
- the movement may be periodic or continuous.
- a cylindrical surface is provided which is rotatable around its axis.
- a first energy source is located inside the cylindrical surface.
- a container for a liquid is located underneath the cylindrical surface, and the cylindrical surface is positioned to be able to dip into and out of the liquid as it rotates.
- the first energy source is directed to the liquid so that the liquid may be exposed to the first energy source.
- a mask is located inside and next to the surface to create a spatially varying energy output.
- the liquid As the surface dips into the liquid, the liquid is solidified into particles of predetermined sizes and shapes as dictated by the patterns on the mask. As the surface dips out of the liquid, it carries with it solid particles already formed and leaving space and allowing empty surface areas to dip into the liquid.
- the solid particles formed on the surface are removed from the surface by a scraping device.
- the particles are collected at a platform and any excess liquid is filtered off and runs through the mesh of the platform into the liquid container to be re-used.
- LCM manufacturing process described hereby could feasibly be performed downhole. Similar resins have been cured in weighted drilling fluids. If LCM are manufactured downstream of the BHA, limitations on loading and particle size can be lifted allowing a wider range of larger fracture sizes to be sealed. Response time to loss events is also reduced to an absolute minimum thereby limiting fluid losses and NPT even further.
- a BHA or drill pipe may comprise a liquid storage, a first energy source and a transparent surface on which the solid particles are to be produced.
- the surface may be a ring shaped transparent structure around the external surface of the BHA or drill pipe, the liquid storage may be arranged to delivery liquid to the ring shaped structure, and the first energy source is preferably located inside the ring structure.
- Solid particles are produced on the ring structure before being scraped off and released to surrounding drilling fluid. In such cases, the solid particles may not be actively separated from the liquid, and some liquid might be released to the surrounding drilling fluid together with the solid particles.
- a solid surface with non-uniform depth may be produced by exposing a liquid to a first energy source of spatially varying intensity.
- the principle is exactly the same and the only difference is that instead of producing a plurality of solid particles, particle arrays are produced for generating a solid surface with surface texture.
- the solid particles are j oint together to produce a continuous solid surface with non-uniform depth. This is achieved by adjusting spatial intensity of the first energy source so that the whole solid surface area is exposed to the first energy source to a greater or less degree.
- Potential applications of this method include: 1. Producing a 3D map.
- Solids control - Shaker screens that MI SWACO make have complex shapes and are frequently replaced. Being able to create templates for screens and/or adding texture to solids control equipment can enhance performance
- the continuous solid surface with varying depth may be the final desirable product, or a mould can be made using the solid surface as a template.
- the solid surface template is preferably produced using an oxygen impermeable surface to cure on such as glass.
- the template may then be left attached to the oxygen impermeable surface such as glass. It can then be used to make a mould.
- the mould itself is preferably made from a liquid that sets to a flexible solid so that it can be separated from the rigid particle template.
- This may be a silicone polymer which have nonstick properties and are easily released from the template.
- the mould can be made of polyurethane.
- the mould can then give shape to a molten material when it cools and hardens.
- the material poured into the mould could be a chemically set liquid (eg epoxy + catalyst) or a thermoset polymer (heat triggered curing) or a thermoplastic (liquid above melting point).
- the mould can be filled with another photocuring resin.
- moulds can also be filled with liquids highly loaded with solids. This can increase the brittleness, strength and abrasion resistance e.g. by adding silica or powdered plastic.
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Abstract
La présente invention concerne un procédé de production d'une pluralité de particules solides ou d'une surface solide de profondeur non uniforme présentant une répartition prédéfinie de taille et de forme en exposant un liquide à une première source d'énergie d'intensité variant dans l'espace, formant ainsi lesdites particules solides ou ladite surface solide de profondeur non uniforme présentant une répartition prédéfinie de taille et de forme. De plus, ledit procédé peut également consister à séparer les particules solides du liquide en transférant les particules solides dans un milieu transparent ; et à exposer les particules solides à une seconde source d'énergie.
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GB1518755.2 | 2015-10-22 | ||
GB1518755.2A GB2543755B (en) | 2015-10-22 | 2015-10-22 | Method for producing solid particles |
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WO2017070406A1 true WO2017070406A1 (fr) | 2017-04-27 |
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PCT/US2016/058005 WO2017070406A1 (fr) | 2015-10-22 | 2016-10-21 | Procédé de production de particules solides |
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WO (1) | WO2017070406A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2022132133A1 (fr) * | 2020-12-15 | 2022-06-23 | Halliburton Energy Services, Inc. | Procédés de fabrication d'une matière de perte de circulation dans un emplacement de forage |
Citations (5)
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US20070046862A1 (en) * | 2005-08-30 | 2007-03-01 | Hitachi Maxell, Ltd. | Microlens array substrate and method of manufacturing microlens array substrate |
US20100249979A1 (en) * | 2006-04-26 | 2010-09-30 | Envisiontec Gmbh | Device and method for producing a three-dimensional object by means of mask exposure |
US20100282462A1 (en) * | 2009-05-08 | 2010-11-11 | Liang Xu | Methods for making and using uv/eb cured precured particles for use as proppants |
US20110033887A1 (en) * | 2007-09-24 | 2011-02-10 | Fang Nicholas X | Three-Dimensional Microfabricated Bioreactors with Embedded Capillary Network |
US8071171B1 (en) * | 2007-10-10 | 2011-12-06 | Hrl Laboratories, Llc | Methods for creating spatially controlled composite materials |
Family Cites Families (3)
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JPH0560582A (ja) * | 1991-09-02 | 1993-03-09 | Sekisui Chem Co Ltd | 立体画像表示盤の製造方法 |
US6210644B1 (en) * | 1998-04-23 | 2001-04-03 | The Procter & Gamble Company | Slatted collimator |
US9829798B2 (en) * | 2013-03-15 | 2017-11-28 | Palo Alto Research Center Incorporated | Flow lithography technique to form microstructures using optical arrays |
-
2015
- 2015-10-22 GB GB1518755.2A patent/GB2543755B/en not_active Expired - Fee Related
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2016
- 2016-10-21 WO PCT/US2016/058005 patent/WO2017070406A1/fr active Application Filing
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070046862A1 (en) * | 2005-08-30 | 2007-03-01 | Hitachi Maxell, Ltd. | Microlens array substrate and method of manufacturing microlens array substrate |
US20100249979A1 (en) * | 2006-04-26 | 2010-09-30 | Envisiontec Gmbh | Device and method for producing a three-dimensional object by means of mask exposure |
US20110033887A1 (en) * | 2007-09-24 | 2011-02-10 | Fang Nicholas X | Three-Dimensional Microfabricated Bioreactors with Embedded Capillary Network |
US8071171B1 (en) * | 2007-10-10 | 2011-12-06 | Hrl Laboratories, Llc | Methods for creating spatially controlled composite materials |
US20100282462A1 (en) * | 2009-05-08 | 2010-11-11 | Liang Xu | Methods for making and using uv/eb cured precured particles for use as proppants |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022132133A1 (fr) * | 2020-12-15 | 2022-06-23 | Halliburton Energy Services, Inc. | Procédés de fabrication d'une matière de perte de circulation dans un emplacement de forage |
US11927062B2 (en) | 2020-12-15 | 2024-03-12 | Halliburton Energy Services, Inc. | Methods of manufacturing lost circulation material at a well site |
Also Published As
Publication number | Publication date |
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GB201518755D0 (en) | 2015-12-09 |
GB2543755A (en) | 2017-05-03 |
GB2543755B (en) | 2020-04-29 |
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