# US 9,433,919 B2 · Activated carbon-metal organic framework composite materials with enhanced gas adsorption capacity and process for the preparation thereof

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- Number: US 9,433,919 B2
- Document ID: US9433919B2
- Status: Granted
- Kind: B2
- Application number: 14/006,729
- Filed: 2012-03-30
- Published: 2014-01-16
- Granted: 2016-09-06
- Earliest claimed: 2011-03-31
- Assignees: Council of Scientific and Industrial Research; Bharat Petroleum Corporation Limited
- Applicants: Hari Chand Bajaj; Rajesh Shantilal Somani; Phani Brahma Rallapalli; Dinesh Patil; Karikkethu Prabhakaran Prasanth; Checkalazhikathu Raj Manoj; Rajendra Singh Thakur; Mathew John; Bharat Lakshman Newalkar; Nettem Venkateswarlu Choudary
- Inventors: Hari Chand Bajaj; Rajesh Shantilal Somani; Phani Brahma Rallapalli; Dinesh Patil; Karikkethu Prabhakaran Prasanth; Checkalazhikathu Raj Manoj; Rajendra Singh Thakur; Mathew John; Bharat Lakshman Newalkar; Nettem Venkateswarlu Choudary
- Web page: https://patentgrep.com/patent/US9433919B2

## CPC

- B01J 20/226: {Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF] (preparation of metal complexes containing carboxylic acid moieties C07C51/418; MOF's per se C07F)}
- B01J 20/20: comprising free carbon; comprising carbon obtained by carbonising processes
- B01J 20/223: {containing metals, e.g. organo-metallic compounds, coordination complexes}
- B01J 20/3064: {Addition of pore forming agents, e.g. pore inducing or porogenic agents}
- C07C 51/418: {Preparation of metal complexes containing carboxylic acid moieties}
- F17C 11/00: Use of gas-solvents or gas-sorbents in vessels {(absorbing compositions for acetylene C10L3/04; absorbing compositions for hydrogen C01B3/0005)}
- F17C 11/005: {for hydrogen}
- B01J 2220/40: Aspects relating to the composition of sorbent or filter aid materials
- Y02C 20/40: of CO2
- Y02E 60/32: Hydrogen storage
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- F17C: VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES (storing fluids in natural or artificial cavities or chambers in the earth B65G5/00; construction or assembling of bulk storage containers employing civil-engineering techniques E04H7/00; variable-capacity gas-holders F17B; liquefaction or refrigeration machines, plants, or systems F25)
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

The present invention discloses activated carbon-metal organic framework composite materials (AC@MOF) with enhanced gas adsorption capacity. The present invention also discloses a process for the preparation of carbon-metal organic framework composite materials (AC@MOF). The present invention involves the use of “void space filling method” in metal organic frameworks (MOFs), which have been accomplished by in-situ addition of selected type and appropriate amount of activated carbon during the synthesis of MOF such as Cu-BTC, in the storage of gases such as methane. The gas adsorption capacity of these AC@MOF composite materials is significantly increased through this method.

## Claims

### Claim 1

A process for the preparation of an activated carbon-metal organic framework composite material with enhanced gas adsorption capacity and having activated carbon from 1 wt % to 4 wt %, wherein the said process comprising the steps:
a. dissolving an organic ligand in ethanol;
b. dissolving a metal salt in the water;
c. mixing the solution as obtained in step (a) with solution as obtained in step (b) followed by stirring at temperature ranging from 298K to 308K for a period ranging between 10 to 50 min;
d. transferring the reaction mixture as obtained in step (c) into an autoclave and further adding activated carbon in the range 1 to 4 wt % in respect of weight of product followed by heating at temperature ranging between 383K and 423K for a period ranging between 15 to 20 hours to obtain an activated carbon-metal organic framework composite material.

### Claim 2 (depends on 1)

The process as claimed in claim 1, wherein the mole ratio of metal salt and organic ligand is in the range of 1.9 to 2.1.

### Claim 3 (depends on 1)

The process as claimed in claim 1, wherein the organic ligand used in step (a) is 1.3.5-Benzene tri-carboxylic acids.

### Claim 4 (depends on 1)

The process as claimed in claim 1, wherein the activated carbon used in step (d) is a porous pelletized activated carbon or a high activity virgin pelletized activated carbon.

### Claim 5 (depends on 1)

The process as claimed in claim 1, wherein the metal used in step (b) is Copper.

### Claim 6 (depends on 1)

The process as claimed in claim 1, wherein the yield of composite materials is in the range of 75 to 95%.