Use of a reactor, methods, and device for quantitatively obtaining molecular hydrogen from substances

Patent metadata

Field	Value
Publication number	US-11465113-B2
Application number	US-201615550724-A
Country	US
Kind code	B2
Filing date	Feb 11, 2016
Priority date	Feb 13, 2015
Publication date	Oct 11, 2022
Grant date	Oct 11, 2022

Abstract

The invention relates to the use of a reactor, methods, and devices for the quantitative recovery of molecular hydrogen from solid, liquid, or gaseous substances which contain hydrogen and which have heteroatoms, as well as to reactors. In this case, the reactors have material containing chromium. The subject matter of the invention also includes the use of the reactor, the method, and the device for the compound-specific or component-specific measurement of the isotope ratio (δ2H) of hydrogen using online apparatuses.

First claim

The invention claimed is:

1. A method for the quantitative recovery of molecular hydrogen from a sample of solid, liquid, or gaseous substances which have heteroatoms, comprising:
introducing the sample, via an inlet, into a pyrolysis reactor with material containing chromium;
performing pyrolysis of the sample to form hydrogen, characterized in that a zone with temperatures above 1100° C. is generated in the pyrolysis reactor, in which a reactive chromium layer of the material containing chromium of the pyrolysis reactor is at least partially arranged within the zone and adjacent to a quartz layer; and
providing the hydrogen via an outlet of the pyrolysis reactor, the reactive chromium layer of the material containing chromium arranged between the inlet and the quartz layer, and the quartz layer arranged between the chromium layer and the outlet of the pyrolysis reactor, the quartz layer including quartz wool, and a layer of chippings arranged next to the quartz layer, the layer of chippings including one or more of: quartz, ceramic, or glassy carbon.

2. The method according to claim 1 , wherein the zone with temperatures above 1100° C. is generated in the reactor to pyrolize substance.

3. The method according to claim 2 , characterized in that the pyrolysis of the substances is carried out using a carrier gas.

4. The method according to claim 3 , characterized in that the reactor's material containing chromium ensures a flow of carrier gas of up to 10 mL/min.

5. The method according to claim 3 , characterized in that the reactor's material containing chromium ensures a flow of carrier gas of up to 300 mL/min.

6. The method according to claim 3 , characterized in that the reactor's material containing chromium ensures a flow of carrier gas of up to 1000 mL/min.

7. The method according to claim 2 , characterized in that the reactor is positioned in an apparatus for high-temperature conversion (in HTC systems).

8. The method according to claim 2 , characterized in that the reactor is positioned in an apparatus for elemental analysis.

9. The method according to claim 2 , characterized in that the reactor is made at least partially of heat-resistant materials suitable for pyrolysis of inserted substances at temperatures≥1100° C., which do not allow the passage of molecular hydrogen from the inside or of air from the outside.

10. The method according to claim 1 , characterized in that at least one section of a reactor inner wall is made of, at least on its inner side, material containing chromium, and/or at least one section of a reactor inner wall has a coating containing chromium, and/or a material containing chromium is embedded in at least one section of a reactor inner wall, at least on its inner side.

11. The method according to claim 1 , characterized in that the reactor's material does not contain any hydrogen or do not react with molecular hydrogen above 1100° C.

12. The method according to claim 1 , characterized in that silver wool is arranged in a first region of the reactor, as a halogen trap, where there is a temperature zone between 500° C. and 800° C. during pyrolysis due to the temperature zone generated above 1100° C.

13. The method according to claim 1 , characterized in that the solid, liquid, or gaseous substances from which the molecular hydrogen will be recovered are separated into their components by means of gas chromatography prior to entry into the reactor.

14. The method according to claim 1 , characterized in that the zone with temperatures above 1100° C. is only generated in a subvolume of the pyrolysis reactor which makes up at most 50% of the reactor volume.

15. The method according to claim 1 , characterized in that the reactor has at least one reactor tube with material containing chromium, in that the zone with temperatures above 1100° C. is generated over at least 90% of the length of the reactor tube in the direction of the longitudinal axis of the reactor tube, and in that the reactor tube's material containing chromium is arranged in the reactor tube at least over the length of the zone with temperatures above 1100° C.

16. The method according to claim 15 , characterized in that the reactor's material containing chromium extends over 40% to 60% of the length of the zone with temperatures above 1100° C., in the longitudinal direction of the reactor tube.

17. The method according to claim 15 , characterized in that the longitudinal axis of the reactor tube is oriented vertically, and the reactor tube's material containing chromium is present as a layer constructed horizontally.

Assignees

• Thermo Fisher Scient Bremen Gmbh

Inventors

• Gehre Matthias
• Renpenning Julian
• Kuemmel Steffen

Classifications

• C01B3/22

  by decomposition of gaseous or liquid organic compounds · CPC title

• B01J2219/00916

  by chromatography · CPC title

• B01J2219/0236

  Metal based · CPC title

• B01J19/02

  Apparatus characterised by being constructed of material selected for its chemically-resistant properties · CPC title

• B01J2219/029

  Non-ferrous metals · CPC title