Production of metal-organic frameworks

Patent metadata

Field	Value
Publication number	US-9630163-B2
Application number	US-201514545594-A
Country	US
Kind code	B2
Filing date	May 27, 2015
Priority date	May 27, 2015
Publication date	Apr 25, 2017
Grant date	Apr 25, 2017

Abstract

An apparatus for producing metal organic frameworks, comprising: a tubular flow reactor comprising a tubular body into which, in use, precursor compounds which form the metal organic framework are fed and flow, said tubular body including at least one annular loop.

First claim

The invention claimed is:

1. An apparatus for producing metal organic frameworks, comprising:
a tubular flow reactor comprising a heated tubular body into which, in use, precursor compounds which form the metal organic framework are fed and flow, said tubular body including at least one annular loop comprising a coil;
a flow restriction device comprising a back-pressure controller downstream of the tubular reactor for controlling the pressure within the tubular reactor; and
an apparatus for separating a metal organic framework (MOF) from a solution, comprising:
a housing having a reservoir capable of receiving a MOF containing solution; and
a high frequency ultrasound transducer operatively connected to the reservoir and capable of applying megasonic frequencies of at least 400 kHz to the MOF containing solution,

wherein the precursor compounds are provided as at least one precursor solution fed into an inlet of the tubular reactor and heated during flow through the tubular body.

2. An apparatus according to claim 1 , wherein the average radius of each annular loop is between 10 and 1000 mm.

3. An apparatus according to claim 1 , wherein the at least one annular loops form a substantially tubular shaped coil radially centered about a central axis of said coil.

4. An apparatus according to claim 1 , wherein the length of the coil is greater than 50 mm.

5. An apparatus according to claim 1 , wherein the internal diameter of the tubular body is between 0.5 mm and 50 mm.

6. An apparatus according to claim 1 , wherein the tubular body is in located inside a heated housing.

7. An apparatus according to claim 6 , wherein the tubular body heats the precursor compounds to a temperature of between 20 and 200° C., preferably between 25 and 150° C., more preferably between 25 and 130° C.

8. An apparatus according to claim 1 , wherein the housing comprises a container including at least one wall position to contact the MOF containing, and the transducer is high frequency ultrasound transducer is position within the reservoir or in engagement with the at least one wall.

9. An apparatus according to claim 1 , wherein the housing includes at least one reflector surface designed to reflect the applied megasonic frequencies within the reservoir.

10. An apparatus according to claim 1 , wherein the applied high frequency ultrasound is between 400 kHz and 4 MHz, preferably between 600 kHz and 2 Mhz, more preferably between 600 kHz and 1 MHz.

11. An apparatus according to claim 1 , wherein the precursor compounds are provided in at least two different precursor solutions containing different precursor compounds, the precursor solutions being mixed through inline mixing in a feed conduit fluidly connected to the inlet of the tubular body where the different precursor solutions are fed into the same inlet, the two or more precursor solutions being mixed at or proximate that inlet.

12. An apparatus according to claim 6 , wherein the housing is heated via heating inlet and outlet port connections through which heated fluid is fed and extracted to heat the tubular body.

13. An apparatus according to claim 12 , wherein the tubular reactor comprises a tube and shell reactor type.

14. A system for producing a metal organic framework (MOF), comprising:
an apparatus for forming a metal organic framework from precursor materials which comprises:
a tubular flow reactor comprising a heated tubular body into which, in use, precursor compounds which form the metal organic framework are fed and flow, said tubular body including at least one annular loop comprising a coil; and
a flow restriction device comprising a back-pressure controller downstream of the tubular reactor for controlling the pressure within the tubular reactor,
wherein the precursor compounds are provided as at least one precursor solution fed into an inlet of the tubular reactor and heated during flow through the said tubular body; and

an apparatus for washing and/or purifying the metal organic framework, comprising: a housing having a reservoir capable of receiving a MOF containing solution from the reactor; and a high frequency ultrasound transducer operatively connected to the reservoir and capable of applying megasonic frequencies of at least 20 kHz to the MOF containing solution.

Assignees

• Commw Scient Ind Res Org

Inventors

• Rubio Martinez Marta
• Hill Matthew Roland
• Batten Michael
• Lim Kok Seng
• Polyzos Anastasios
• Barton Timothy Raymond
• Hadley Trevor Deon
• Monch Andreas Alexander

Classifications

• B01J2531/48

  Zirconium · CPC title

• B01J2531/0216

  Bi- or polynuclear complexes, i.e. comprising two or more metal coordination centres, without metal-metal bonds, e.g. Cp(Lx)Zr-imidazole-Zr(Lx)Cp · CPC title

• C07F5/06

  Aluminium compounds · CPC title

• B01J2531/16

  Copper · CPC title

• B01J2219/00087

  with heat exchange elements outside the reactor · CPC title