Dynamic method for rapidly filling identical batches of bottle of gas mixtures with high metrological precision

Patent metadata

Field	Value
Publication number	US-12189404-B2
Application number	US-202318210214-A
Country	US
Kind code	B2
Filing date	Jun 15, 2023
Priority date	Jun 17, 2022
Publication date	Jan 7, 2025
Grant date	Jan 7, 2025

Abstract

A method for filling a batch of gas bottles with a gas mixture, wherein the gas mixture may have of a single constituent in a matrix or a plurality of constituents in a matrix, which matrix has of one or more base gases, in which a real-time analysis of all the constituents of the gas mixture is carried out at the exit of a mixing chamber and before it enters a compression stage.

First claim

What is claimed is:

1. A method for filling a batch of gas bottles with a gas mixture, wherein the gas mixture may consist of a single constituent in a matrix or a plurality of constituents in a matrix, which matrix consists of one or more base gases, in which a filling installation having the following elements is provided:
one or more reservoirs storing the matrix gas or gases;
one or more high-pressure bottles storing the said constituent or constituents;
one or more high-pressure bottles storing one or more reference gases, configured to calibrate an analytical system;
a mixing chamber;
gas lines configured for conveying the mixing gases and the matrix gases to the mixing chamber, which gas lines are each equipped with one or more mass flow controllers;
a compression stage comprising a gas compressor;
a gas line configured for conveying the gas mixture formed in the mixing chamber to the compression stage, which compression stage is configured for pressurizing the gas mixture in order to fill each of the bottles of the said batch of bottles therewith;
an analytical system having selected analysers;
a gas line configured for conveying a part of the gas mixture formed in the mixing chamber to the analytical system configured to carry out real-time analysis of the gas mixture sampled in this way, which line is advantageously placed in bypass on the said gas line connecting the mixing chamber to the compression stage;
one or more filling stations making it possible to position the bottles of the said batch of bottles to be filled and suitable for distributing the gas mixture into each of the bottles of the said batch of bottles;
a gas line suitable for conveying the pressurized gas mixture from the compression stage to the filling station or stations, the filling station or stations being capable of being entirely full or partially populated with the bottles of the said batch of bottles;
one or more gas lines suitable for conveying a part of the pressurized gas mixture in the bottles of the said batch of bottles to the analytical system in order to be able in particular to perform a post-filling verification analysis of the bottles after the filling cycle;

wherein the following measures are carried out:
conveying the gas mixture at the exit of the mixing chamber to the compression stage, which carries out an increase of the pressure of the mixture to a desired setpoint;
conveying the gas mixture at the exit of the compression stage to the filling station or stations and the distribution of the gas mixture into the said batch of bottles is carried out, and the filling is stopped once a pressure setpoint has been reached in at least one of the bottles of the said batch;
analysing on-line in real-time all the mixing components of the gas mixture by the analytical system at the exit of the mixing chamber and before entering the compression stage;
estimating in real-time the composition of the gas mixture in one of the bottles is carried out by real-time integration from the start of filling of the composition of the gas mixture leaving the mixing chamber or real-time composition of the gas mixture entering the bottle or bottles of the said batch of bottles as a function of the result of the said real-time analysis of the composition of the gas mixture coming from the mixing chamber, at a given instant; and
comparing this estimation with one or more setpoint values for the final concentration or concentrations intended in each of the bottles of the batch is carried out, and if necessary feedbacks are carried out automatically and in real time in order to modify the gas flow rates of each component of the mixture reaching the chamber, by modifying the setting of the mass flow controllers associated with each component, so as to maintain and/or correct upwards and/or correct downwards the particular concentrations of the components of the mixture leaving the mixing chamber, and thus to be able to continue the filling with a nominal composition or a composition enriched or depleted with respect to one or some of the components of the mixture.

2. The method according to claim 1 , wherein a preliminary operation of preparing the mixture is carried out in the following way:
a) analyzing the mixture leaving the compression stage before this mixture arrives in one or more of the stations;
b) comparing the result of this analysis with a setpoint and venting the mixture if the difference between the result of the analysis and the setpoint is greater than a value considered to be acceptable;
c) filling of the said batch of bottles is authorized when the result of the comparison of step b) is less than the said value considered to be acceptable.

Assignees

• Air Liquide

Inventors

• Le Gendre Erwann
• Daviet Christian
• Weterings Werner
• Koch Maurice

Classifications

• F17C13/02

  Special adaptations of indicating, measuring, or monitoring equipment (measuring in general G01) · CPC title

• F17C5/00

  Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures (adding propellants to aerosol containers B65B31/00) · CPC title

• B65B31/04

  Evacuating, pressurising or gasifying filled containers or wrappers by means of nozzles through which air or other gas, e.g. an inert gas, is withdrawn or supplied · CPC title

• B65B1/30

  Devices or methods for controlling or determining the quantity or quality or the material fed or filled · CPC title

• B65B1/04

  Methods of, or means for, filling the material into the containers or receptacles · CPC title