Use of multiple stream high pressure mixer/reactor

• US 6,159,442 A
• Filed: 08/05/1998
• Issued: 12/12/2000
• Est. Priority Date: 08/05/1997
• Status: Expired due to Term

• Current Assignee: Microfluidics International Corporation (RELX PLC)
• Original Assignee: MFIC Corporation
• Inventors: Ginter, David Mark, Kieken, Laurent DAny, King, David Lassen, Thumm, Jeffrey R., Higgins, Jerome S., Lento, Michael A.
• Primary Examiner(s): Straub, Gary P.
• Application Number:
  US09/129,294
• Time in Patent Office: 860 Days
• Field of Search: 423/328.1, 423/328.2, 423/330.1, 423/430, 423/420.2, 423/659, 423/493, 423/600, 502/235, 502/244, 502/250, 502/84, 502/8, 502/252, 502/341, 502/346, 422/224, 422/131, 422/132, 422/133, 239/310, 239/420, 239/434, 239/435, 137/3, 366/159.1, 366/132
• US Class Current: 423/659
• CPC Class Codes: B01F 23/40 Mixing liquids with liquids; Emulsifying
• CPC Class Codes: B01F 25/23 Mixing by intersecting jets
• CPC Class Codes: B01F 33/30 Micromixers
• CPC Class Codes: B01J 14/00 Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor B01J8/00, B01J19/08 take precedence
• CPC Class Codes: B01J 19/0093 Microreactors, e.g. miniaturised or microfabricated reactors laboratory containers with capillary fluid transport in microfabricated channels or chambers B01L3/5027
• CPC Class Codes: B01J 19/26 Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
• CPC Class Codes: B01J 2208/00672 Particle size selection
• CPC Class Codes: B01J 2219/00162 controlling the pressure
• CPC Class Codes: B01J 2219/00164 controlling the flow
• CPC Class Codes: B01J 2219/00889 Mixing
• CPC Class Codes: B01J 2219/00891 Feeding or evacuation
• CPC Class Codes: B01J 23/80 with zinc, cadmium or mercury
• CPC Class Codes: B01J 3/00 Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor pressure vessels for containing or storing compressed, liquefied or solidified gases F17C
• CPC Class Codes: B01J 4/02 for feeding measured , i.e. prescribed quantities of reagents
• CPC Class Codes: C01B 13/36 by precipitation reactions in aqueous solutions C01B13/328 takes precedence
• CPC Class Codes: C01B 13/363 Mixtures of oxides or hydroxides by precipitation
• CPC Class Codes: C01B 33/26 Aluminium-containing silicates , i.e. silico-aluminates
• CPC Class Codes: C01F 11/181 Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
• CPC Class Codes: C01F 11/462 Sulfates of Sr or Ba
• CPC Class Codes: C01G 1/02 Oxides
• CPC Class Codes: C01G 9/006 : Compounds containing, besides zinc, two ore more other elements, with the exception of oxygen or hydrogen
• CPC Class Codes: C01P 2002/22 : layered hydroxide-type, e.g. of the hydrotalcite-type
• CPC Class Codes: C01P 2002/72 : by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/38 : cube-like
• CPC Class Codes: C01P 2004/52 : highly monodisperse size distribution
• CPC Class Codes: C01P 2004/61 : Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C01P 2004/62 : Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

Processes for use of a controlled continuous high pressure multiple reactant streams flowing into a chemical mixer/reactor. Individual reactant streams are pressurized to about 8,000 to 50,000 psi and achieve velocities up to about 250 meters/second in the final stage of the chemical mixer/reactor.

Claims

1. A process for the production of a solid state, particulate product by combining in a reaction chamber two or more liquid reactant streams containing chemical reactants which, upon reaction, form a solid particulate product of uniformly sized particles in less than 10 micron diameter size range, said process comprising:

a) pressurizing each separate liquid reactant stream to a pressure of at least 8000 psi;

b) passing said liquid streams into a reaction chamber as high velocity liquid jets which collide with each other at an anile ∝

ranging from about 10°

to about 350° and

react to form a solid product; and

c) recovering the precipitated or solid particulate product from the reaction chamber at atmospheric pressure.

2. The process of claim 1, wherein the size distribution between the largest and smallest particles, measured in linear dimension is no greater than a factor of about 5.

3. A process for the production of a gel product formed by the reaction of two or more chemical components producing a precipitated product in a reaction chamber where the chemical reaction components are provided to the reaction chamber as two or more liquid reactant streams containing said components, which upon reaction form a gel product of uniform composition, said process comprising:

a) pressurizing each separate liquid reactant stream to a pressure of at least 8000 psi;

b) passing said liquid streams into a reaction chamber as high velocity liquid jets which collide with each other at an angle ∝

ranging from about 10°

to about 350° and

react to form the gel product; and

c) recovering the gel product from the reaction chamber at atmospheric pressure.

4. A process for the production of a precipitated product of high phase purity wherein separate liquid-based streams comprising one or more reactants in solution and precipitating agent in dispersed or dissolved form in liquid media are combined on a continuous basis and wherein the composition and phase purity of the precipitated product are controlled by maintaining a constant pH in the combined liquid streams at the time of mixing and precipitation, which comprises:

a) initially adjusting the pH of each liquid stream to afford the desired pH on mixing;

b) pressurizing each separate liquid stream containing a reactant or precipitating agent, respectively, at the adjusted pH, to a pressure of at least 8000 psi;

c) passing said liquid streams into a reaction chamber as high velocity liquid jets which collide with each other at an angle ∝

ranging from about 10°

to about 350° and

react to form the precipitated product; and

d) recovering the precipitated product from the reaction chamber at atmospheric pressure.

5. The process of claim 4, wherein the precipitated product is made up of at least 90 percent by weight of a single phase.

6. A process for the production of mixed metal and metal oxide solid state materials of small crystallite size and desired phase purity by co-precipitation of two or more metals from metal salt solutions with a precipitating agent wherein separate liquid-based streams comprising dispersions or solutions of each metal salt and a precipitating agent are combined on a continuous basis with the potential to form two or more precipitated product phases depending on the intensity of mixing and presence of homogeneous mixtures of the metal salt components at supersaturated conditions which comprises:

a) pressurizing each separate liquid stream containing a metal salt or a precipitating agent to a pressure of at least 8000 psi;

b) passing said liquid streams into a reaction chamber as opposed high velocity liquid jets which collide with each other at an angle ∝

ranging from about 10°

to about 350° and

react to form the mixed metal and metal oxide solid state materials; and

c) recovering the mixed metal and metal oxide solid state materials from the reaction chamber at atmospheric pressure.

7. A process for the production of a copper/zinc/aluminum hydrotalcite catalyst by co-precipitation of copper, zinc and aluminum salts to form a particulate catalyst which is enriched in the hydrotalcite phase relative to the malachite phase and which is made up of crystallites having an average size below about 20 nm which comprises:

a) preparing separate liquid solutions containing metal salts of copper, zinc and aluminum and of a precipitating agent;

b) pressurizing each separate liquid solution to a pressure of at least 8000 psi;

c) passing said pressurized liquid streams into a reaction chamber as high velocity liquid jets which collide with each other at an angle ∝

ranging from about 10°

to about 350° and

react to form the mixed metal and metal oxide solid state materials; and

d) recovering the particulate catalyst product from the reaction chamber at atmospheric pressure.

8. A process for the preparation of a precipitated aluminosilicate gel formed by precipitation reaction of a silicon-containing compound and an aluminum-containing compound wherein the atomic ratio of Si/Al in the gel, defined as the number of Al atoms which are coordinatively bonded to Si via an oxygen atom, closely approximates the atomic ratio of Si/Al in the silicon-containing and aluminum containing compounds used as starting materials which comprises:

a) pressurizing each separate liquid solution or suspension to a pressure of A <

at least 8000 psi;

b) passing said pressurized liquid solutions or suspensions into a reaction chamber as high velocity liquid jets which collide with each other at an angle ∝

ranging from about 10°

to about 350° and

react to form the gel product; and

c) recovering the gel product from the reaction chamber at atmospheric pressure.