Method for producing activated carbon and activated carbon obtained in this way and use thereof

Patent metadata

Field	Value
Publication number	US-11655155-B2
Application number	US-201616061187-A
Country	US
Kind code	B2
Filing date	Aug 24, 2016
Priority date	Dec 10, 2015
Publication date	May 23, 2023
Grant date	May 23, 2023

Abstract

The invention relates to a method for the production of activated carbon, in particular particulate activated carbon, having an increased mesopore and/or macropore volume fraction, preferably having an increased mesopore volume fraction.

First claim

The invention claimed is:

1. A particulate activated carbon having a Gurvich total pore volume including an increased mesopore volume fraction,
wherein the activated carbon is granular or spherical,
wherein 60% to 99.5% of the Gurvich total pore volume formed by mesopores is formed by mesopores having pore diameters in the range from 2 nm to 20 nm;
wherein the activated carbon has an average pore diameter in the range from 3 nm to 20 nm;
wherein the activated carbon has a Gurvich total pore volume in the range from 0.5 cm 3 /g to 4 cm 3 /g;
wherein the activated carbon has an abrasion resistance of at least 99%, as determined according to modified CEFIC standard;
wherein the activated carbon has a specific BET surface area in the range from 500 m 2 /g to 4500 m 2 /g;
wherein the activated carbon has an iodine number in the range from 1400 mg/g to 2100 mg/g;
wherein the activated carbon has a butane adsorption in the range from 35% to 90%; and
wherein the activated carbon has a methylene blue value in the range from 17 ml to 65 ml;
wherein the activated carbon is obtained by a method, wherein the method comprises the following steps:
(a) sulfonating a particulate polymeric organic starting material by contacting the starting material with at least one sulfonating agent and subsequently causing to act and reacting the sulfonating agent with the starting material in such a way, namely for a duration in the range of from 0.5 h to 24 h and at temperatures in the range of from 50° C. to 330° C., that the sulfonation takes place with simultaneous volume expansion of the starting material, wherein the volume expansion of the starting material is increased by at least 2%, based on the particle size of the unsulfonated starting material; subsequently,
(b) carbonizing the sulfonated starting material obtained in step (a), then
(c) activating the carbonized starting material obtained in step (b) to give the activated carbon;
wherein, before step (b) is carried out, a step of leaving and/or repositing the sulfonated starting material is carried out.

2. A method for producing the particulate activated carbon of claim 1 ,
wherein the method comprises the following steps:
(a) sulfonating a particulate polymeric organic starting material by contacting the starting material with at least one sulfonating agent and subsequently causing to act and reacting the sulfonating agent with the starting material in such a way, namely for a duration in the range of from 0.5 h to 20 h and at temperatures in the range of from 75° C. to 330° C., that the sulfonation takes place with simultaneous volume expansion of the starting material, wherein the volume expansion of the starting material takes place in such a way that the particle size of the sulfonated starting material is increased by at least 2%, based on the particle size of the unsulfonated starting material; subsequently;
(b) carbonizing the sulfonated starting material obtained in step (a); then
(c) activating the carbonized starting material obtained in step (b) to give the activated carbon;
wherein, before step (b) is carried out, a step of leaving and/or repositing the sulfonated starting material is carried out.

3. The method as claimed in claim 2 ,
wherein the sulfonating agent used in step (a) is sulfur trioxide SO 3 .

4. The method as claimed in claim 2 ,
wherein the sulfonating agent used in step (a) is sulfur trioxide SO 3 in the form of oleum optionally in mixture with concentrated sulfuric acid and wherein the sulfonating agent is used in liquid form.

5. The method as claimed in claim 2 ,
wherein the leaving and/or repositing of the sulfonated starting material is carried out at temperatures in the range of from 15° C. to 30° C.

6. The method as claimed in claim 2 ,
wherein, during the leaving and/or repositing of the sulfonated starting material, the starting material is provided with chemical groups, wherein the chemical groups on their thermal decomposition leads to free radicals and thus to chemical crosslinking.

7. The method as claimed in claim 2 ,
wherein the volume expansion of the starting material takes place in such a way that the particle size of the sulfonated starting material is increased by at least 1%, based on the particle size of the unsulfonated starting material.

8. The method as claimed in claim 2 ,
wherein the volume expansion of the starting material takes place in such a way that the particle size of the sulfonated starting material is increased by at least 5%, based on the particle size of the unsulfonated starting material.

9. The method as claimed in claim 2 ,
wherein the starting material is in the form of a granular or spherical starting material which is porous and/or gel-like and wherein the starting material has a micropore volume fraction, based on the total pore volume of the starting material, in the range of from 30% to 85%.

10. The method as claimed in claim 2 ,
wherein the carbonizing in step (b) is carried out in such a way that the chemical groups of the sulfonated starting material obtained after step (a) are thermally decomposed with formation of free radicals and/or crosslinking.

11. The method as claimed in claim 2 ,
wherein the activating in step (c) is carried out in the presence of at least one activating gas selected from the group consisting of oxygen, air, water vapor and carbon dioxide and mixtures of these activating gases.

12. The method as claimed in claim 2 ,
wherein the activating in step (c) is carried out in multiple stages, wherein the carbonized starting material is first subjected in a first activating step to activation in a water vapor-containing atmosphere, followed by a second activating step of activation in a carbon dioxide-containing atmosphere.

13. A protective equipment for the civil or military sector, wherein the protective equipment is selected from the group consisting of protective suits, protective gloves, protective footwear, protective socks, protective headgear, and protective covers and wherein the protective equipment provides protective function with respect to chemical, biological and radioactive noxiants and poisons, wherein the protective equipment comprises an activated carbon as defined in claim 1 .

14. A particulate activated carbon having a Gurvich total pore volume including an increased mesopore volume fraction,
wherein 60% to 99.5% of the Gurvich total pore volume is formed by mesopores having pore diameters in the range from 2 nm to 20 nm;
wherein the activated carbon has an average pore diameter in the range from 3 nm to 20 nm;
wherein the activated carbon has a Gurvich total pore volume in the range from 2 cm 3 /g to 3 cm 3 /g;
wherein the activated carbon has an abrasion resistance of at least 99.5%, as determined according to modified CEFIC standard; and
wherein the activated carbon has a specific BET surface area in the range from 1200 m 2 /g to 2500 m 2 /g;
wherein the activated carbon has an iodine number in the range from 1450 mg/g to 2000 mg/g;
wherein the activated carbon has a butane adsorption in the range from 45% to 80%; and
wherein the activated carbon has a methylene blue value in the range from 19 ml to 50 ml.

15. A particulate activated carbon having a Gurvich total pore volume including an increased mesopore volume fraction,
wherein 60% to 99.5% of the Gurvich total pore volume is formed by mesopores having pore diameters in the range from 2 nm to 20 nm;
wherein the activated carbon has an average pore diameter in the range from 3 nm to 20 nm;
wherein the activated carbon has a Gurvich total pore volume in t

Assignees

• Bluecher Gmbh

Inventors

• Modrow Antje
• Böhringer Bertram
• Giebelhausen Jann-Michael

Classifications

• B01J20/28066

  being more than 1000 m2/g · CPC title

• B01J20/28076

  being more than 1.0 ml/g · CPC title

• B01J20/28083

  being in the range 2-50 nm, i.e. mesopores · CPC title

• A62D5/00

  Composition of materials for coverings or clothing affording protection against harmful chemical agents · CPC title

• B01J20/28085

  being more than 50 nm, i.e. macropores · CPC title