Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
  • B01F25/30—Injector mixers
  • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
  • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
• • 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
  • B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
  • B01F23/40—Mixing liquids with liquids; Emulsifying
  • B01F23/405—Methods of mixing liquids with liquids
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
  • B01F35/50—Mixing receptacles
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
  • B01F35/71—Feed mechanisms
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
  • B01F35/90—Heating or cooling systems
  • B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
• • 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
  • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
• • 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
  • B01J19/24—Stationary reactors without moving elements inside
  • B01J19/2415—Tubular reactors
• • 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
  • B01J19/24—Stationary reactors without moving elements inside
  • B01J19/2415—Tubular reactors
  • B01J19/242—Tubular reactors in series
• • 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
  • B01J19/24—Stationary reactors without moving elements inside
  • B01J19/2415—Tubular reactors
  • B01J19/244—Concentric tubes
• • 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
  • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
  • B01J3/008—Processes carried out under supercritical conditions
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
  • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
  • B01F2025/915—Reverse flow, i.e. flow changing substantially 180° in direction
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
  • B01F2101/2204—Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application
• • 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
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
  • B01J2219/00277—Apparatus
  • B01J2219/00495—Means for heating or cooling the reaction vessels
• • 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
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
  • B01J2219/00583—Features relative to the processes being carried out
  • B01J2219/0059—Sequential processes
• • 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
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
  • B01J2219/00583—Features relative to the processes being carried out
  • B01J2219/00599—Solution-phase processes

Definitions

• This invention relates to mixing reactors such as may (non-exclusively) be suitable for producing particles such as nanoparticles or Metal-Organic frameworks, a cascade of such reactors and a method of using such reactors to mix fluids, typically but non- exclusively so as to produce such particles.
• Metal and metal oxide particles with nanometre scale dimensions have a wide range of uses, including (but not limited to) catalysts, pigments, polishes, ultraviolet absorbers and in ceramics. It is well known that such particles can be formed by chemical reaction of aqueous solutions of metal salts with heated, pressurised or supercritical water. In principle, this methodology offers distinct advantages over other methods of nanoparticle creation in terms of cost and viability as it allows the reaction to be performed as a continuous process. However, it is difficult to perform this reaction on a commercial scale utilising current methods because existing reactor configurations do not allow the precipitation reaction to be controlled effectively leading to frequent blockage of the reactor and inadequate control of particle size and shape. Hence within this process, the design of the reactor where the water and the salt solution mix is of crucial importance to the size and properties of the nanoparticles produced.
• the PCT patent application published as WO2005/077505 describes a counter-current mixing reactor where supercritical water is introduced into a first inlet and a metal salt solution is introduced at a second inlet, the resultant nanoparticle-bearing suspension being extracted at an outlet.
• the first inlet is positioned within the outlet, so that the mixing occurs where the flow of supercritical water changes direction through 180 degrees.
• a mixing reactor comprising a body having a first inlet, a second inlet and an outlet, in which there is an inner passage through the body from the first inlet at a first end of the body to the outlet at a second end of the body along a length of the body, the inner passage having a side wall along the length, and an outer passage closer to a surface of the body than the inner passage, the outer passage running from the second inlet at the second end, travelling through the body along the length and meeting the inner passage at a junction at the first end, the outer passage joining the inner passage through the side wall at the junction.
• the outer passage is closer to the surface than the inner passage, it can be more easily heated by a heater surrounding the mixing reactor than the inner passage or the fluid flowing into the first inlet.
• a heater to the body will preferentially heat fluid flowing through the outer passage, and is unlikely to substantially heat fluid flowing into the first inlet until after it has passed the junction.
• a metal salt is introduced to the first inlet, there will be no significant heating of the first inlet by a heater attached to the body, but there will be heating of a (typically supercritical) fluid introduced into the second inlet.
• the outer passage may enter the inner passage at an angle of 90 degrees to the length, plus or minus 45 , 30, 15 , 5 or 1 degrees.
• the junction may comprise an orifice in the inner wall, with a portion of the outer passage preceding the orifice that is at the angle relative to the length.
• the further outer passage may be a further outer passage that is also closer to the surface than the inner passage, the further outer passage having a further second inlet at the second end, travelling through the body along the length and meeting the inner passage at a further junction at the first end, the further outer passage joining the inner passage through the side wall at the further junction.
• the further outer passage will be symmetrical to the outer passage relative to the inner passage; this allows for symmetrical mixing, which can allow the reactor generate the best products in terms of composition, uniform particle sizes and narrow particle size distribution.
• the outer passage could comprise a sleeve coaxially surrounding the inner passage; this would also provide for symmetrical mixing.
• the surface will exclude the first and second ends.
• the reactor may further comprise a heater coupled to the surface, such as a band heater. This will, as discussed previously, preferentially heat the outer passage rather than the inner passage or the first inlet.
• the body may be made of heat-conductive material, such as a metal material, such as stainless steel, typically stainless steel 3 16, or alloys such as Hastelloy, Inconel, Monel or Nimonic.
• the reactor may comprise an extension passage, extending out of the body from the outlet. This can allow the fluid flowing out of the reactor to be provided with heating or cooling as desired.
• the extension passage may be provided with heating or cooling apparatus through which it passes.
• the reactor may be suitable for mixing two fluids. Typically, it will be suitable for forming particles, such as nanoparticles or metal-organic framework (MOF) particles.
• a cascade of mixing reactors comprising a first mixing reactor in accordance with the first aspect of the invention and a second mixing reactor in accordance with the first aspect of the invention, in which the outlet of the first mixing reactor is coupled to the first inlet of the second mixing reactor.
• the present reactor provides little opportunity for particle accumulation and/or lining of internal surfaces of the reactor, which are most likely to occur where the product stream is hot.
• the potential for particle accumulation can be minimised by avoiding narrow constrictions, artefacts such as edges, ridges and corners (on the internal surfaces of the apparatus) and changes in overall flow direction in the region of apparatus between the mixing point (that is, the junction 1 1) and where the product stream is cooled after the outlet 4.
• the present design allows for a reactor that is completely free of zones which may allow particle accumulation.
• the present reactor can be made substantially seamless and without any loss of symmetry between the junction 1 1 and the point where the product has been substantially cooled in, for example, a downstream heat exchanger.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Organic Chemistry (AREA)
• Physical Or Chemical Processes And Apparatus (AREA)

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Citations (5)

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• 2013
  • 2013-11-19 GB GBGB1320417.7A patent/GB201320417D0/en not_active Ceased
• 2014
  • 2014-11-19 JP JP2016532596A patent/JP2016538995A/ja active Pending
  • 2014-11-19 KR KR1020167016065A patent/KR102405044B1/ko active Active
  • 2014-11-19 US US15/037,520 patent/US10406499B2/en active Active
  • 2014-11-19 WO PCT/GB2014/053413 patent/WO2015075439A1/en not_active Ceased
  • 2014-11-19 EP EP14820913.3A patent/EP3071320B1/en active Active
• 2020
  • 2020-01-16 JP JP2020004996A patent/JP7013040B2/ja active Active

Patent Citations (5)

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