Chemistry of inorganic compounds – Oxygen or compound thereof – Peroxide
Reexamination Certificate
1999-01-15
2001-12-25
Langel, Wayne (Department: 1754)
Chemistry of inorganic compounds
Oxygen or compound thereof
Peroxide
C210S652000, C210S654000, C423S588000, C423S589000, C423S590000
Reexamination Certificate
active
06333018
ABSTRACT:
The present invention relates to an industrial process for producing hyperpure hydrogen peroxide also having titre up to about 60-70% by weight, to be used in electronic, pharmaceutical and food industries. Specifically it is used in the electronic field in the semiconductor industry wherein H
2
O
2
electronic grade is required. The presence of impurities, such as ions, in the commercial hydrogen peroxide requires purification processes so that this product can be used in said industry.
It is well known that hydrogen peroxide as all peroxides requires a precaution series with regard to its industrial production, storage and transport. The safety of these operations is a must on an industrial and commercial scale. An essential characteristic of the commercial hydrogen peroxide is the persistence in the long term of the peroxidic oxygen (active oxygen) content. This quality issue is conventionally characterized as thermal stability, for example by the ISO 7161 test (titre loss after 16 hours at 96° C.).
However the correlation of hydrogen peroxide thermal stability with its purity is not univocal, as the influence of the various impurities, in terms of stability decay, is different and said influence changes also in connection with the distribution of the impurities in their complex.
The thermal stability of the industrial scale hydrogen peroxide is by itself an issue, both for the big volumes of product involved and the importance of the invested capitals, and for the safety warranties required for logistic and transport purposes. This issue becomes much more critical when H
2
O
2
titre reaches values up to about 60-70% by weight.
The chemical industry solves this problem as follows: on one side, by the careful selection of the technical materials in contact with hydrogen peroxide—the production plants are made with aluminum or stainless steel; the storage tanks with stainless steel or with special plastic materials—; on the other side, by adding to hydrogen peroxide specific chemical products which are able to improve the thermal stability thereof also by the inhibition of chemical agents able to catalyze any product decomposition reactions.
Practically to obtain hyperpure hydrogen peroxide it is necessary to start from commercial stabilized hydrogen peroxide and to process it by means of extreme purification processes to remove the impurities which are not acceptable in the indicated applications, for example in the electronic industry.
The purification processes of the hydrogen peroxide for the removal of various polluting agents are known in the art. However all the known prior art purification processes are carried out in a small scale and the output in purified product is very limited. The ratio of the output product with respect to the input is very low, well below 20%, in the process of reverse osmosis of the prior art.
All these processes use as starting material commercial grade stabilized H
2
O
2
(see U.S. Pat. No. 4,879,043).
To reach a higher purity level, that is necessary for high purity applications, it is necessary to retreat the purified product. The disadvantage is that the yield in purified product is even lower. From the industrial point of view this is a great disadvantage.
In particular see the patents having as an object the treatment of hydrogen peroxide by reverse osmosis, U.S. Pat. No. 4,525,265; U.S. Pat. No. 4,879,043; the patents relating to the purification of hydrogen peroxide by treatment with ions exchange resins, WO 92/06918; DE 4,214,075; the patents describing the purification processes of hydrogen peroxide which are carried out by mixed techniques JP 7,109,109; U.S. Pat. No. 4,985,228; EP 626,342; DE 4,222,109.
The combination of different indicated techniques, necessary in order to obtain high purity hydrogen peroxide which is therefore free from all the polluting agents, until the analytical detectability, must fully comply with operating safety criteria. This safety is however compromised by the lack of the chemical stabilizers of the product. Obviously the relevance of this problem increases with the production scale. Moreover, this problem becomes more critical as the concentration of the produced hydrogen peroxide reaches about 60-70% titre.
Therefore the obtainment of hydrogen peroxide at increasing purity levels in industrial amounts is an open technological problem. The more, when its concentration is as high as about 60 to 70% titre.
Moreover another drawback of the processes of the art is that the purified product yields are not high and the processing duration of the ions exchange resins is very short. Besides, the risk due to a prolonged use of said resins is very high. Moreover the amount of hydrogen peroxide containing impurities which requires specific treatments for its disposal is considerable; this requires treatment plants of remarkable sizes with consequent increase of the purification costs.
It was felt the need to have available an industrial process to produce hyperpure hydrogen peroxide also having high concentration, up to about 60-70% by weight (titre), which neither implies risks from the safety point of view nor implies the above mentioned disadvantages.
The Applicant has surprisingly and unexpectedly found that it is possible to obtain on industrial scale hydrogen peroxide also at high concentration up to about 60-70% by weight with the purity levels required by the most sophisticated applications with the process described hereinafter.
An object of the present invention is an industrial process for the production of hyperpure hydrogen peroxide also at high concentration, up to about 60-70% by weight, characterized in that the hydrogen peroxide produced in an industrial plant, and used as such without addition of any stabilizing agent, also at high concentration up to about 60-70% by weight is directly fed to a purification unit, being part of the same production plant, in which the reverse osmosis, separation of the high purity permeate flow and direct recycle of the concentrated flow to the production plant, are carried out.
The osmosis is carried out in one or more steps in series or in parallel, with direct recycle of the concentrated flow to the production plant of the hydrogen peroxide, preferably to the final distillation unit. The membranes used to carry out the reverse osmosis are based on polyamides, polypiperazinamides, polyacrylonitrile and polysulphones.
Preferably the purification process of the invention comprises also a treatment unit based on ions exchange resins for the above mentioned permeate, in order to obtain hydrogen peroxide with even higher purity levels. It has been indeed surprisingly found that the product coming out from the osmosis units has very high stability characteristics and can be further treated as hereabove indicated with the utmost safety.
If desired, one or more units charged with ions exchange resins in series or in parallel can be used.
The ions exchange resins are preferably of strong cationic type. Amberlite 200C and Amberjet 1500H by Rohm & Haas can for example be mentioned.
If desired, the process of the invention can comprise ultrafiltering
anofiltering units to remove the particles that may be possibly present in the hydrogen peroxide. This step is generally inserted before the reverse osmosis unit and optionally also after the osmosis unit or the treatment with resin.
Also for the ultrafiltering one or more units in series or in parallel can be used.
By the process of the invention it has been achieved the possibility to integrate the purification unit with the hydrogen proxide industrial producing units, in the full compliance with the industrial fixed criteria of the risk control.
Thus there are no scale limitations in the production of hyperpure hydrogen peroxide with respect to the current production of technical grade hydrogen peroxide. This is a remarkable advantage of the process of the invention in comparison with the processes of the art since it allows to solve the economic conflicts in their whole.
It has been found that by the invention process
Bianchi Ugo Piero
Leone Umberto
Lucci Mauro
Arent Fox Kintner & Plotkin & Kahn, PLLC
Langel Wayne
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