Device and method for determination of a catalyst state in a chemical reactor
The invention pertains to a device for determination of a catalyst state in a chemical reactor and to a method for detecting a catalyst state under in situ reaction conditions. A reactor is provided with a solid catalyst provided in a reactor chamber. A fluid sample is taken from the reactor chamber and is transferred to a sample chamber. The temperature at the extraction site of the sample in the reactor chamber is determined and the temperature of the sample chamber is adjusted to the same temperature. A small amount of the catalyst provided in reactor chamber is provided in sample chamber and is contacted with the sample flow. Spectroscopic information is then obtained on the catalyst provided in sample cell, e.g. by an IR spectrometer.
1 . A device for determination of a catalyst state in a chemical reactor, comprising:
the chemical reactor comprising a reactor chamber with at least one inlet for introducing a fluid phase into the reactor chamber and at least one outlet for draining off the fluid phase,
a sampling device for collecting a fluid sample inside the reactor chamber,
a temperature-sensitive sensor arranged at the sampling device for detecting temperature of the fluid phase and/or a solid phase at a site of the sampling device where the fluid sample is collected, wherein
a spectroscopic detection unit arranged outside the reactor, said spectroscopic detection unit comprising a sample chamber for configured to arrange a solid catalyst sample therein and a spectroscopic analysis device for obtaining spectroscopic data on the catalyst sample arranged in the sample chamber,
wherein the fluid phase, while flowing through reactor chamber is configured to interact with said solid catalyst and components comprised in the fluid phase are configured to undergo chemical reactions,
a conduit is provided between sampling device and the sample chamber of the spectroscopic detection unit for introducing a fluid sample taken at the sampling device into the sample chamber of the spectroscopic detection unit,
heating and/or cooling means and a temperature control unit are provided in the spectroscopic detection unit and are configured for adjustment of a temperature of the sample chamber.
2 . A device according to claim 1 , wherein the sampling device is a sampling capillary comprising a sampling orifice for collecting the fluid sample inside the reactor chamber, wherein the sampling capillary is introduced into the reactor chamber and the sampling orifice is arranged inside the reactor chamber.
3 . A device according to claim 2 , wherein the reactor and the sampling capillary are movably relative to each other.
4 . A device according to claim 2 , wherein the reactor is arranged stationary and the sampling capillary is slidably relative to the reactor.
5 . A device according to claim 1 , wherein the temperature-sensitive sensor has a fiber form.
6 . A device according to claim 5 , wherein the temperature-sensitive sensor is arranged inside the sampling capillary wherein a tip of the temperature-sensitive sensor having the fiber form is arranged at the sampling orifice.
7 . A device according to claim 1 , wherein the spectroscopic analysis device is an infrared-spectrometer.
8 . A device according to claim 7 , wherein the infrared spectrometer is a diffuse reflection mode infrared spectrometer.
9 . A device according to claim 1 , wherein the spectroscopic analysis device is an XRD-spectrometer.
10 . A method for detecting a catalyst state under in situ reaction conditions, wherein
a reactor chamber is provided comprising a solid catalyst and a mobile fluid phase passing through the reactor chamber,
a fluid sample is taken inside the reactor chamber at a first extraction site,
the temperature of the mobile fluid phase at the first extraction site is determined,
the fluid sample is transferred to a sample chamber of a spectroscopic detection unit, wherein a catalyst sample of the solid catalyst comprised in the reactor chamber is provided in the sample chamber,
the temperature of the mobile fluid phase in the sample chamber of the spectroscopic detection unit is adjusted to the temperature of the mobile fluid phase at the first extraction site, and
spectroscopic data of the solid catalyst provided in the sample chamber are acquired,
wherein the first sample of the mobile fluid phase is taken at the first extraction site inside the reactor chamber and the spectroscopic data of the solid catalyst provided in the sample chamber are acquired whilst the solid catalyst is in contact with the first sample of the mobile fluid phase; and at least one further fluid sample of the mobile fluid phase is taken at least one further extraction site in the reactor chamber and further spectroscopic data of the solid catalyst provided in the sample chamber are acquired whilst the solid catalyst is in contact with the one further fluid sample.
11 . A method according to claim 10 , wherein a pressure of the mobile fluid phase inside the sample chamber is adjusted to a pressure of the fluid phase inside the reactor chamber.
12 . A method according to claim 10 , wherein the spectroscopic data are acquired by diffuse reflection infrared spectroscopy.
13 . A method according to claim 10 , wherein the spectroscopic data are acquired by spatial XRD.