Aqueous disinfectant, comprising performic and peracetic acid, method of preparation and use
Abstract
This record has no abstract on file.
Term
Term ended
Expired 19 March 2019, 7.5 years ago.
- Priority
- Filed
- Granted
- Expired
- Today
7 claims: 7 independent, 0 dependent
- 1Method for the preparation of an aqueous disinfectant containing peracetic acid and performic acid, by adding a source of formic acid to an aqueous phase containing hydrogen peroxide, characterised in that formic acid or a water-soluble salt of formic acid, in a quantity of 0.1 to 1.0 mol formic acid or 0.1 to 1.0 equivalents of formate per kg of the disinfectant to be prepared, is used as the source of formic acid and an equilibrium solution of peracetic acid containing 20 to 60 wt.% hydrogen peroxide, 0.5 to 6 wt.% peracetic acid, less than 10 wt.%, in particular less than 2 wt.%, acetic acid and up to 3 wt.% of a mineral acid is used as the aqueous phase containing hydrogen peroxide and the mixture is allowed to stand for at least 1 minute up to 5 hours prior to use. Procédé de production d'un agent désinfectant aqueux contenant de l'acide peracétique et de l'acide performique par addition d'une source d'acide formique à une phase aqueuse contenant du peroxyde d'hydrogène, caractérisé en ce qu' on utilise comme source d'acide formique l'acide formique ou un sel soluble dans l'eau de l'acide formique en une quantité de 0,1 à 1,0 mole d'acide formique ou de 0,1 à 1,0 équivalent de formiate par kg du désinfectant à préparer, et comme phase aqueuse contenant du peroxyde d'hydrogène, une solution d'acide peracétique à l'équilibre ayant une teneur de 20 à 60 % en poids de peroxyde d'hydrogène, 0,5 à 6 % en poids d'acide peracétique, moins de 10 % en poids, en particulier moins de 2 % en poids, d'acide acétique, et jusqu'à 3 % en poids d'un acide minéral, et on laisse reposer le mélange avant utilisation pendant 1 minute à 5 heures. Verfahren zur Herstellung eines Peressigsäure und Perameisensäure enthaltenden wäßrigen Desinfektionsmittels durch Zugabe einer Quelle für Ameisensäure zu einer Wasserstoffperoxid enthaltenden wäßrigen Phase, dadurch gekennzeichnet,daß man als Quelle für Ameisensäure Ameisensäure oder ein wasserlösliches Salz der Ameisensäure in einer Menge von 0,1 bis 1,0 Mol Ameisensäure oder 0,1 bis 1,0 Äquivalent Formiat pro kg des herzustellenden Desinfektionsmittels und als Wasserstoffperoxid enthaltende wäßrige Phase eine Gleichgewichtsperessigsäurelösung mit einem Gehalt von 20 bis 60 Gew.-% Wasserstoffperoxid, 0,5 bis 6 Gew.-% Peressigsäure, weniger als 10 Gew.-%, insbesondere weniger als 2 Gew.-% Essigsäure und bis zu 3 Gew.-% einer Mineralsäure verwendet und das Gemisch vor der Verwendung mindestens 1 Minute bis 5 Stunden stehen läßt.
- 2Method according to claim 1, characterised in that an alkali-metal formate, in particular sodium formate, is used as the source of formic acid and 0.1 to 0.8 mequivalents of formate is added per mequivalent of mineral acid present. Procédé selon la revendication 1, caractérisé en ce qu' on utilise comme source d'acide formique un formiate de métal alcalin, en particulier le formiate de sodium, et en ce qu'on ajoute par milliéquivalent (mEq) d'acide minéral présent, de 0,1 à 0,8 mEq de formiate. Verfahren nach Anspruch 1, dadurch gekennzeichnet,daß man als Quelle für Ameisensäure ein Alkalimetallformiat, insbesondere Natriumformiat, verwendet und pro mÄquivalent anwesender Mineralsäure 0,1 bis 0,8 mÄquivalent Formiat zugibt.
- 3Method according to claim 1 or 2, characterised in that an equilibrium peracetic acid wherein the mineral acid is selected from among sulfuric acid, phosphoric acid, pyrophosphoric acid and polyphosphoric acid is used. Procédé selon la revendication 1 ou 2, caractérisé en ce qu' on utilise un acide peracétique à l'équilibre dont l'acide minéral est choisi dans la série constituée par l'acide sulfurique, l'acide phosphorique, l'acide pyrophosphorique et l'acide polyphosphorique. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet,daß man eine Gleichgewichtsperessigsäure verwendet, deren Mineralsäure ausgewählt ist aus der Reihe Schwefelsäure, Phosphorsäure, Pyrophosphorsäure und Polyphosphorsäure.
- 4Aqueous disinfectant, characterised in that it contains 0.1 to 3 wt.% performic acid, 0.1 to 5 wt.% peracetic acid, formic acid and acetic acid in a total quantity of up to 10 wt.%, preferably less than 2 wt.%, hydrogen peroxide in a quantity of 20 to 50 wt.% and a mineral acid in a quantity of up to 3 wt.%. Désinfectant aqueux caractérisé en ce qu' il contient de 0,1 à 3 % en poids d'acide performique, de 0,1 à 5 % en poids d'acide peracétique, de l'acide formique et de l'acide acétique en une quantité totale allant jusqu'à 10 % en poids, de préférence inférieure à 2 % en poids, du peroxyde d'hydrogène en une quantité allant de 20 à 50 % en poids et un acide minéral en une quantité allant jusqu'à 3 % en poids. Wäßriges Desinfektionsmittel, dadurch gekennzeichnet,daß es 0,1 bis 3 Gew.-% Perameisensäure, 0,1 bis 5 Gew.-% Peressigsäure, Ameisensäure und Essigsäure in einer Gesamtmenge von bis zu 10 Gew.-%, vorzugsweise weniger als 2 Gew.-%, Wasserstoffperoxid in einer Menge von 20 bis 50 Gew.-% und eine Mineralsäure in einer Menge von bis zu 3 Gew.-% enthält.
- 5Aqueous disinfectant according to claim 4, characterised in that it contains up to 1 wt.% sodium ions from sodium formate used during the preparation. Désinfectant aqueux selon la revendication 4, caractérisé en ce qu' il contient jusqu'à 1 % en poids d'ions sodium provenant du formiate de sodium utilisé dans la préparation. Wäßriges Desinfektionsmittel nach Anspruch 4, dadurch gekennzeichnet,daß es bis zu 1 Gew.-% Natriumionen aus bei der Herstellung eingesetztem Natriumformiat enthält.
- 6Use of the aqueous disinfectant according to claim 4 or 5 for the control of microorganisms from among the bacteria, viruses, fungi and algae in aqueous systems and on surfaces. Utilisation du désinfectant aqueux selon la revendication 4 ou 5 pour la lutte contre les microorganismes de la série des bactéries, des virus, des champignons et des algues dans les systèmes aqueux et sur les surfaces. Verwendung des wäßrigen Desinfektionsmittels gemäß Anspruch 4 oder 5 zum Bekämpfen von Mikroorganismen aus der Reihe der Bakterien, Viren, Pilze und Algen in wäßrigen Systemen und auf Oberflächen.
- 7Use according to claim 6, characterised in that the agent is used for the disinfection of water in swimming baths. Utilisation selon la revendication 6, caractérisé en ce qu' on utilise l'agent pour la désinfection de l'eau des piscines. Verwendung nach Anspruch 6, dadurch gekennzeichnet,daß man das Mittel zur Desinfektion von Schwimmbadwasser verwendet.
Independent claims7
40 paragraphs, as filed
The invention is directed to a performic acid and Peracetic acid-containing aqueous disinfectant, a process for its preparation and its use for combating microorganisms, in particular in aqueous Systems.
For the treatment of aqueous solutions, in particular municipal wastewater, surface water and industrial Circulatory and effluents containing microorganisms, which for hygienic, operational or environmental reasons will not be discharged untreated or reused can, effective treatment methods are needed. Effective chemical methods, the same environmentally friendly are based on the use of Active oxygen compounds such as in particular Hydrogen peroxide, peracetic acid and Peroxyformic acid, peracetic acid commonly referred to as and performic acid-containing disinfectants. The term "disinfectant" is a means understood that of the fight against all kinds Microorganisms such as bacteria, viruses, fungi and algae, suitable is; in addition, this product is suitable for Combating microorganisms, such as zooplankton.
It is known that hydrogen peroxide is a moderately-acting, mild disinfectant with bacteriostatic Properties. While H<sub>2</sub>O<sub>2</sub>Concentrations of 25 mg / l Although inhibit the growth of some bacteria, a effective lowering of the number of bacteria even at a much higher H<sub>2</sub>O<sub>2</sub>Concentration for many hours or an additional UV irradiation. Such measures are, in the case of Disinfection of large quantities of water, such as for the treatment of Water in sewage treatment plants and their disposal, and inadequate also uneconomical.
Peracetic acid (PAA) is a highly effective contrast Active agent, the use rapid microbial reduction allows. Accordingly, peracetic acid is inter alia to Sterilization in the food industry, bottle and Hospital disinfectants used. commercial Peracetic acid with a content of 15 wt .-% PES additionally comprise about 14 wt .-% H<sub>2</sub>O<sub>2</sub> and 28 wt .-% Acetic acid. The use of such solutions PES prepares because of their unpleasant corrosive and oxidizing Properties handling, warehousing, materials and Transport problems. A further disadvantage is the high Acetic acid content, which increased to a COD content and additionally result in a dramatic reappearance can.
Let the above mentioned disadvantages of the PAA solutions in accordance with DE-OS 195 31 241.4 by using a low-concentration peracetic acid solution with a content from 0.5 to 2.5 wt .-% PES, 40 to 50 wt .-% Hydrogen peroxide, and less than 2 wt .-% acetic acid avoid. Despite its famously good effect of such Peracetic acid as a disinfectant is to some applications need for a rapid and possibly effective nor efficient Disinfectants on the basis of Active oxygen compounds, which previously the disadvantages said PAA solutions with a PES content of 15 wt .-% or it does not have.
An alternative to disinfectants based on Peracetic acid and hydrogen peroxide containing solutions are aqueous solutions containing performic acid (PAS), PES, Hydrogen peroxide and formic acid. According to J. Hyg. Epidem. Microbiol. Immunol. (1968) 12, 115 includes possibly performic acid better fungicidal properties on as peracetic acid, but the effect could also be due formic acid. Using a such a solution can be as described in EP 231 632 A2 0 Microorganisms on surfaces and in accordance with WO 94/20424 in Water circuits at a use level in the field 1-1000 ppm, especially 5 to 100 ppm, combat performic acid within about 0.5 to 60 minutes or kill.
The PAS solution according to WO 94/20424 and EP 0231632 is by reacting hydrogen peroxide with formic acid in situ generated, where the molar ratio of H<sub>2</sub>O<sub>2</sub> to Formic acid in the range of 1: 10 to 10: 1. are used highly concentrated formic acid and 20 to 50 wt .-% hydrogen peroxide. Disadvantage of such a PFA solution are the not inconsiderable risk of explosion and high corrosiveness and hence handling and Security problems.
From WO 95/24388 it is known that the reaction of Formic acid with hydrogen peroxide to Equilibration is very slow, the PAS-Education but in the presence of a carboxylic acid ester, for As ethyl acetate, are accelerated as a catalyst can. Additionally or alternatively to a carboxylic acid ester a compound having a -C (O) -O-group, wherein but not a carboxylic acid group, as Catalyst used; However, this document does not given excitation, what it is in such compounds could act.
A performic acid containing disinfectant also known from WO 95/32625: Made is the Performic acid by reaction of an acid ester, such as ethyl formate, with an oxidizing agent, in particular Hydrogen peroxide. Although it is advantageous that over the System formic acid / hydrogen peroxide lower Corrosiveness, disadvantageous, however, as evidenced in the Examples very low concentration of performic acid, so only after a long exposure time a sufficient kill rate is achievable. In addition, a Formic acid ester expensive than the formic acid.
In DE-A 39 29 335 a process is for disinfection taught by textiles in washing streets, where the last Rinse a peroxycarboxylic containing agent is added. The means are, in particular a Gleichgewichtsperoxycarbonsäurelösung with a Content of 40 to 60 wt .-% carboxylic acid, 2 to 5 wt .-% Peroxycarboxylic acid, and 0.1 to 3 wt .-% hydrogen peroxide. As the carboxylic acid for preparing the composition, in addition to Acetic acid and formic acid and propionic and Mixtures of such acids are used; Details of two Carboxylic acids, and accordingly, the corresponding Peroxycarboxylic containing agents can be the Do not remove the document.
Although disinfectants on the basis of Performic acid, in some cases a higher microbicidal can have an effect as such on the basis of Peracetic acid, is the production and handling of Performic acid containing a higher concentration Solutions problematic. The object of the invention therefore, a performic acid, peracetic acid and hydrogen peroxide show containing disinfectant that easy and safely prepared in situ and after a short Reaction time be used for disinfection purposes can. In addition, the disinfectant should be short Exposure time to a high kill rate of carry microorganisms in aqueous systems.
found a process for preparing a Peracetic acid and performic acid-containing aqueous Disinfectant by adding a source of Containing formic acid to hydrogen peroxide aqueous phase, which is characterized in that, as Source of formic acid, formic acid or a water-soluble salt of formic acid in an amount of 0.1 to 1.0 mol formic acid or 0.1 to 1.0 equivalent Of formate per kg of the disinfectant to be produced and containing hydrogen peroxide as an aqueous phase Gleichgewichtsperessigsäurelösung with a content of 20 to 60 wt .-% of hydrogen peroxide, from 0.5 to 6 wt .-% Peracetic acid, less than 10 wt .-%, in particular less than 2 wt .-% acetic acid and up to 3 wt .-% of a Mineral acid used and the mixture before use at least 1 minute left to stand up to 5 hours.
Preferably used as hydrogen peroxide and peracetic acid aqueous phase containing a Gleichgewichtsperessigsäure used, the equilibrium also requires acetic contains. Expediently contains the Gleichgewichtsperessigsäure additionally one of their Production derived mineral acid catalyst such as in particular one from the group of sulfuric acid, Phosphoric acid (H<sub>3</sub>PO<sub>4</sub>), Pyrophosphoric (H<sub>4</sub>P<sub>2</sub>O<sub>7</sub>) and Polyphosphoric acid (H<sub>n + z</sub>P<sub>n</sub>O<sub>3n + 1</sub>), Wherein n is an integer ≥ 3 is. Expediently containing peracetic acid 0.1 to 5 wt .-%, particularly 0.5 to 3 wt .-% mineral acid.
Appropriately, the content of peracetic acid (PAA) in the employed in Gleichgewichtsperessigsäure Range of 0.5 to 15 wt .-%, in particular 0.5 to 6 Wt .-%, and according to another preferred embodiment in the range of about 1 to 3 wt .-%. Such Gleichgewichtsperessigsäurelösungen generally have a hydrogen peroxide content in the range of about 20 to 60 wt .-%, in particular 20 to 50 wt .-%, based on; Preferred solutions having from 1 to 3 wt .-% of peracetic acid usually contain from 30 to 50 wt .-% hydrogen peroxide. Of the Acetic acid content of preferred Gleichgewichtsperessigsäurelösungen should be generally below 10 wt .-%. Solutions with 0.5 to 3 wt .-% PES preferably contain less than 2 wt .-% and particularly preferably less than 1 Wt .-% acetic acid. A lowest possible acid content reduces the risk of rapid regrowth after microbiocidal treatment of an aqueous system with a Disinfectants according to the invention. Accordingly, is in a preferred embodiment, as the aqueous phase a Gleichgewichtsperessigsäure with a content of 30 to 50 wt .-% H<sub>2</sub>O<sub>2</sub>, 1 to 3 wt .-% of peracetic acid (PES), less than 2 wt .-%, in particular less than 1 wt .-% Acetic acid, and 0.5 wt .-% 3 used to mineral acid.
As a source of formic acid, either formic acid, a lower acid esters such as methyl, ethyl or Propyl, or a water soluble salt of Formic acid are used. The salt can be in the solid Or in the form of an aqueous solution of H<sub>2</sub>O<sub>2</sub> and PES containing aqueous phase may be added. Water-soluble salts are alkali metal formates, especially sodium, and Erdalkalimetallformiate, in particular calcium. It is also possible Ammonium formate and quaternary ammonium formates, whereby the quaternary ammonium, such as (C<sub>10</sub>-C<sub>18</sub>) -Alkyltrimethylammonium, even microbicidal properties may have. The particular advantage of using a Alkali metal formate is in the safe and easy Manageability, the smell of salt and freedom in the Reduction of the corrosiveness of the product to Disinfectant.
The amount of formic acid or salt thereof is usually in the range of 0.1 to 1 mole of formic acid or 0.1 to 1 equivalent of formate per kg of the the disinfecting agent. If the Peracetic acid solution used has a sufficiently large contains mineral acid quantity, the amount used can also be in the use of formates be further increased. At the Use of a formic acid salt to the quantity be lower than for neutralization of the present Mineral acid is required. Preference per milliequivalents Present mineral acid 0.1 to 0.8 meq alkali metal, in particular Sodium formate, are used.
For the preparation of a preferred disinfectant is one of the aforementioned preferred Gleichgewichtsperessigsäurelösungen with a PES content from 0.5 to 6 wt .-%, a H<sub>2</sub>O<sub>2</sub>Content of 20 to 50 .-% And an acetic acid content of less than 10 wt .-% wt with 0.2 to 1 mol Ameisensäure.oder 0.2 to 1 equivalent of brought formate as a source of formic acid into contact. After brief standing or stirring, generally at least 1 minute to 5 hours, which can now Performic acid (PAS), peracetic acid (PAA) and Hydrogen peroxide-containing solution as Disinfectants are used. The achievement of the Balance is often not necessary since unreacted Formic even a microbicidal activity having. The solution containing PAS should preferably be used within about 12 hours, as the PAS-content decreases again after reaching a maximum value and the peracid content substantially back on values of Solution originally employed falls.
A preferred, according to the invention by the method available aqueous disinfectant contains per kg: 0.1 to 3 wt .-% performic acid, 0.1 to 5 wt .-% Peracetic acid, formic acid and acetic acid in a Total amount of less than 10 wt .-% and 20 to 50 wt .-% Hydrogen peroxide.
Additionally, the disinfectant may contain conventional Additives, including active oxygen stabilizers such as Complexing agents from the series of the phosphonic acid compounds, Tin compounds and pyridine carboxylic acids or salts thereof or contain scavengers, further corrosion inhibitors, Hardness stabilizers, scale inhibitors and surfactants, in particular, anionic and nonionic surfactants. Furthermore, microbicides from others can also his classes present as active oxygen compounds.
The disinfectant according to the invention available characterized by their high effectiveness in combating of micro-organisms from the series of bacteria, viruses, Fungi and algae. Already within 30 seconds after Adding the disinfectant to an aqueous system decreases the number of bacteria [cfu / ml] by 3 to 4 orders of magnitude. A Such a high and particularly rapid rate of kill is when Use a disinfectant in swimming pools necessary due to legal requirements. Obviously acts a PAS invention and PES containing Disinfectant solution, based on the total Percarboxylic acid, better than a previously customary Solution which only contains a percarboxylic PAS. As seen from the Example B2 and Comparative Examples VB2 and VB0 apparent, was charged with the inventive solution achieved rapid and complete microbial count reduction as with a prior art, as percarboxylic only Performic acid-containing solution. This was surprising, because all the percarboxylic acid in Example 2 only about 40% of that of Comparative Example 2, respectively. indeed contained the Example B2 more hydrogen than the Comparative Example CE2, however, it is known that Although hydrogen peroxide bacteriostatic, but hardly bactericidal effect.
The amount of disinfectant depends on itself the intended purpose. Usually 1 to 1000 mg, in particular 1 to 100 mg, and more preferably 5 to 20 mg of disinfectant per 1 to be treated Water used.
The inventive method can be in Apply different areas. As an example, called: circulation water from the food, Brewing and dairy industry; Recycling and waste water chemical processes in which it without disinfectant and / or inhibition of microbial growth can lead to problems - About slime and odor; Water and sludge from the petrochemical industry and municipal sewage treatment plants; Swimming pool water. Another application of the Method of the invention is in the range of Soil remediation: The addition of the disinfectant in be the water of infiltration well same microorganisms in the immediate vicinity is reduced; so is the biological decomposition of the Oxidant hydrogen peroxide present reduced and a greater range of undecomposed Hydrogen peroxide reaches the ground.
Major advantages of the method are the safe handling and rapid availability of Performic acid conveyance of light and storable Substances. Sodium formate as a source of formic acid is in Compared to formic acids easily transportable, storable, odor-free and non hautkorrosiv.
The disinfection effect can be controlled via the amount the source of formic acid and composition of the employed peracetic acid easily control. A further advantage is the rapid effect and the high Germicidal rate. Solutions with a very low Acetic acid content are characterized by delayed Recontamination from. The invention Disinfectant is particularly suitable where a too high acidity is undesirable. The concentration of the by the preparation of the composition according to the invention formed Performic acid decreases after a few hours off again, while the effect of peracetic acid present in the composition substantially retained. The agent is therefore especially where initially an enhanced effect, but at the same time a longer-lasting microbicidal Action is required.
Example 1 and Comparative Example 1
An inventive disinfectant was prepared by adding 20 g of formic acid (AS) to 980 g of a Gleichsgewichtsperessigsäure which 2 wt .-% of peracetic acid (PES), 1 wt .-% acetic acid (ES) and 48 wt .-% Hydrogen peroxide and 2 wt .-% H<sub>2</sub>SO<sub>4</sub> contained.
After a standing time of just 2 hours, this solution was as a disinfectant used in comparison to the Gleichgewichtsperessigsäure for the treatment of Pool water used; Quantity 10 mg Disinfectant per 1 water.
A swimming pool water were standardized Conditions pure cultures of the test microbial suspension and added to a concentration of 10<sup>7</sup> until 10<sup>8th</sup> CFU / ml set. After addition of the disinfectant were after a contact time of 10, 20 and 30 seconds Sample taken and in this by inactivating the Disinfectant the remaining concentration of determined test germs and from the disinfection capacity (KR<sub>t</sub>) Determined. KR<sub>t</sub> = Log CFU<sub>(KO)</sub> - Log cfu<sub>(D)</sub>Where KBE<sub>(KO)</sub>the number CFU per ml without action of Disinfectant and KBE<sub>(D)</sub> those after the action. <tables><table><tgroup cols="3"><tbody><row><entry align="center" /><entry align="left">example 1</entry><entry align="center">Comparative Example 1</entry></row><row><entry align="left">Germicidal speed</entry><entry align="left">22 - 30 seconds</entry><entry align="left">greater 60 seconds</entry></row><row><entry align="left">Pseudomonas aernginosa ATCI 15442</entry><entry align="left">4 log steps</entry><entry align="left">4 log steps</entry></row><row><entry align="left">Escherichia coli ATCI 11229</entry><entry align="left">3 log steps</entry><entry align="left">3 log steps</entry></row></tbody></tgroup></table></tables>
The DIN 19643 as well as the recommendation of the BGA (Federal Health Office (DE)) required Disinfection capacity is achieved. Another Advantage is that the use of PAA alone to a lead high COD and germ killing speed not would reach. The PAS alone hand would not achieve requirements for service life. Only the Combination of the two assures that it is possible to get all the requirements in more detail.
Example 2 (E2) AND COMPARATIVE EXAMPLE 2 (CE2)
We investigated the biological effectiveness of a Peracetic acid and performic acid according to the invention Disinfectants containing solution (B2) compared to one as percarboxylic exclusively performic acid Containing solution (VB2). The composition of the solutions follows from the table: <tables><table><tgroup cols="3"><tbody><row><entry align="center" /><entry align="center">B 2</entry><entry align="center">VB 2</entry></row><row><entry align="center">manufacturing</entry><entry align="center">Mixing a 2 wt .-% PES, 48 wt .-% H<sub>2</sub>O<sub>2</sub>, 1 wt -.% ES and 2 wt .-% H<sub>2</sub>SO<sub>4</sub> Peracetic acid solution containing (= VB 0) 3 wt .-% HCOOH (AS); let stand for 4 hours</entry><entry align="center">Mixing 68 g of a 35 wt .-% H<sub>2</sub>O<sub>2</sub>Solution with 32 g of formic acid (AS); let stand for 4 hours</entry></row><row><entry align="left">Composition (in wt .-%)</entry></row><row><entry align="center">PAS</entry><entry align="center">1.55</entry><entry align="center">8.0</entry></row><row><entry align="center">PES</entry><entry align="center">1.90</entry><entry align="center">-</entry></row><row><entry align="center">AS</entry><entry align="center">1.85</entry><entry align="center">27.1</entry></row><row><entry align="center">IT</entry><entry align="center">1.0</entry><entry align="center">-</entry></row><row><entry align="center">H<sub>2</sub>O<sub>2</sub></entry><entry align="center">45.1</entry><entry align="center">19.6</entry></row></tbody></tgroup></table></tables>
Examines the bacterial count of E. history Cols K12 was at a quantity of 50 ppm of the solution according to B2, 50 ppm the solution according to VB2 and 50 ppm of for preparing the Solution according to B2 used peracetic acid solution (= V B0). The effect was measured by a bioluminescence-rapid tests determined.
The course of the values for the luminescence (RLU value) - Dimension for the number of bacteria decrease - follows from the table: <tables><table><tgroup cols="4"><tbody><row><entry align="center">RLU after minutes</entry><entry align="center">B 2</entry><entry align="center">VB 2</entry><entry align="center">VB 0</entry></row><row><entry align="center">5</entry><entry align="center">320</entry><entry align="center">270</entry><entry align="right">950</entry></row><row><entry align="center">10</entry><entry align="center">40</entry><entry align="center">160</entry><entry align="right">560</entry></row><row><entry align="center">15</entry><entry align="center">25</entry><entry align="center">150</entry></row><row><entry align="center">30</entry><entry align="center">0</entry><entry align="center">50</entry><entry align="right">110</entry></row></tbody></tgroup></table></tables>
The RLU value decreased using the invention Disinfectant over 30 minutes to 0 from (= B2), while using the previously known performic acid solution (= CE2) a final value of 50 and using the preparation for B2 used peracetic acid solution (= V B0) a final value was achieved by the 110th
Examples 3 and 4
Analyzes formation of performic acid were after Addition of 1 wt .-% formic acid (= B3) or 1 Wt .-% sodium (Nafo) (= B4) to a Gleichgewichtsperessigsäure (G-PES 2) with a content of 2 wt .-% PES, 1 wt .-% ES, 2 wt .-% H<sub>2</sub>SO<sub>4</sub> and 48 wt .-% H<sub>2</sub>O<sub>2</sub>Further stability of percarboxylic resulting active oxygen content (% AO).
The table shows the results -% AO from peracids in Time dependence. <tables><table><tgroup cols="4"><tbody><row><entry align="center" /><entry align="center">for comparison</entry><entry align="center">B 3</entry><entry align="center">B 4</entry></row><row><entry align="center">Time (h)</entry><entry align="center">G-2 PES</entry><entry align="center">G-2 PES + 1% AS</entry><entry align="center">G-2 PES + 1% Nafo</entry></row><row><entry align="center">0</entry><entry align="center">0.42</entry></row><row><entry align="center">1</entry><entry align="right" /><entry align="right" /><entry align="center">0.45</entry></row><row><entry align="center">3</entry><entry align="right" /><entry align="center">0.52</entry></row><row><entry align="center">4</entry><entry align="right" /><entry align="right" /><entry align="center">0.48</entry></row><row><entry align="center">5</entry><entry align="right" /><entry align="center">0.62</entry></row><row><entry align="center">6</entry><entry align="right" /><entry align="right" /><entry align="center">0.50</entry></row><row><entry align="center">7</entry><entry align="right" /><entry align="right" /><entry align="center">0.47</entry></row><row><entry align="center">65</entry><entry align="center">0.42</entry><entry align="center">0.50</entry><entry align="center">0.43</entry></row></tbody></tgroup></table></tables>
By addition of formic acid or sodium formate rises the percarboxylic acid to. The rate of formation using sodium is lower because thereby a part of the catalytically active sulfuric acid is neutralized; for the same reason, the Stability lower. An improved buffering reached.
Examples 5 and 6
Analogously to Examples 3 and 4, a 5 wt .-% strength Gleichgewichtsperessigsäurelösung (G-PES 5) (5% PES, 7% ES, 23% H<sub>2</sub>O<sub>2</sub> and 2% H<sub>2</sub>SO<sub>4</sub>) With 1 wt .-% formic acid (FA) (Based on the G-PES) and 1 wt .-% Sodium (Nafo) added. The table shows the Education and AO stability in time dependence. <tables><table><tgroup cols="4"><tbody><row><entry align="center" /><entry align="center">for comparison</entry><entry align="center">B 5</entry><entry align="center">B 6</entry></row><row><entry align="center">Time (h)</entry><entry align="center">G-PES 5</entry><entry align="center">G-PES 5 + 1% AS</entry><entry align="center">G-PES 5 + 1% Nafo</entry></row><row><entry align="center">0</entry><entry align="center">1.05</entry></row><row><entry align="center">4</entry><entry align="right" /><entry align="center">1.15</entry></row><row><entry align="center">6</entry><entry align="right" /><entry align="center">1.13</entry><entry align="center">1.13</entry></row><row><entry align="center">8th</entry><entry align="right" /><entry align="right" /><entry align="center">1.05</entry></row><row><entry align="center">65</entry><entry align="center">1.05</entry><entry align="center">1.07</entry><entry align="center">1.03</entry></row></tbody></tgroup></table></tables>
Every citation, both ways
| Document | Relation | Office |
|---|---|---|
| WO9421122A | Cites | World Intellectual Property Organization (WIPO) |
14 members in 9 offices
Priority claims5
| Document | Office | Kind | Date |
|---|---|---|---|
| 19812589 | Germany | A | |
| 19812589 | Germany | A | |
| 19812589 | Germany | – | |
| 19812589 | – | – | – |
| DE1998112589 | – | – | – |
Members14
| Document | Office | Kind | |
|---|---|---|---|
| CA2266523A1 | Canada | A1 | |
| EP0945404A2 | European Patent Office (EPO) | A2 | |
| ZA992230B | South Africa | B | |
| DE19812589A1 | Germany | A1 | |
| JPH11322523A | Japan | A | |
| EP0945404A3 | European Patent Office (EPO) | A3 | |
| BR9900604A | Brazil | A | |
| US6211237B1 | United States of America | B1 | |
| EP0945404B1This record | European Patent Office (EPO) | B1 | |
| AT227695T | Austria | T | |
| ATE227695T1 | Austria | T1 | |
| DE59903367D1 | Germany | D1 | |
| ES2184364T3 | Spain | T3 | |
| CA2266523C | Canada | C |
59 legal events, as 8 offices reported them to INPADOC
Over the term
Point at a mark for the eventEvents
| Event | Code | Office | |
|---|---|---|---|
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Announcement of lapse in spainLapsedFD2A | FD2A | ES | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Application deemed withdrawn, or ip right lapsed, due to non-payment of renewal feeWithdrawnR119 | R119 | DE | |
| Notification of lapseLapsedST | ST | FR | |
| Lapse because of not paying annual feesLapsedMM01 | MM01 | AT | |
| Gb: european patent ceased through non-payment of renewal feeCeasedGBPC | GBPC | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25 | PG25 | EP | |
| Ep patent has lapsedLapsedEUG | EUG | SE | |
| Lapsed because of non-payment of the annual feeLapsedV1 | V1 | NL | |
| Be: lapsedLapsedBERE | BERE | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP | PGFP | EP | |
| Assignments of patentsSD | SD | NL | |
| Modifications of names of proprietors of patentsTD | TD | NL | |
| Change of addressCA | CA | FR | |
| Change of name or company nameCD | CD | FR | |
| Change in legal formCJ | CJ | FR | |
| No opposition filedOpposition26N | 26N | EP | |
| No opposition filed within time limitOppositionORIGINAL CODE: 0009261PLBE | PLBE | EP | |
| Information on the status of an ep patent application or granted ep patentGrantedSTATUS: NO OPPOSITION FILED WITHIN TIME LIMITSTAA | STAA | EP | |
| Fr: translation filedET | ET | EP | |
| Definitive protectionFG2A | FG2A | ES | |
| Gb: translation of ep patent filed (gb section 77(6)(a)/1977)GBT | GBT | EP | |
| Corresponds to:REF | REF | EP | |
| Designated contracting statesAK | AK | EP | |
| European patent grantedGrantedNOT ENGLISHFG4D | FG4D | GB | |
| Corresponds to:REF | REF | EP | |
| (expected) grantORIGINAL CODE: 0009210GRAA | GRAA | EP | |
| Despatch of communication of intention to grant a patentORIGINAL CODE: EPIDOS IGRAGRAH | GRAH | EP | |
| First examination report despatched17Q | 17Q | EP | |
| Despatch of communication of intention to grantORIGINAL CODE: EPIDOS AGRAGRAG | GRAG | EP | |
| Despatch of communication of intention to grant a patentORIGINAL CODE: EPIDOS IGRAGRAH | GRAH | EP | |
| Despatch of communication of intention to grantORIGINAL CODE: EPIDOS AGRAGRAG | GRAG | EP | |
| Party data changed (applicant data changed or rights of an application transferred)RAP1 | RAP1 | EP | |
| Designation fees paidAT BE DE ES FI FR GB IT NL SEAKX | AKX | EP | |
| Request for examination filed17P | 17P | EP | |
| Designated contracting statesAK | AK | EP | |
| Request for extension of the european patentAL;LT;LV;MK;RO;SIAX | AX | EP | |
| Information provided on ipc code assigned before grant7C 02F 1/72 ARIC1 | RIC1 | EP | |
| Search report despatchedORIGINAL CODE: 0009013PUAL | PUAL | EP | |
| Designated contracting statesAK | AK | EP | |
| Request for extension of the european patentAL;LT;LV;MK;RO;SIAX | AX | EP | |
| Public reference made under article 153(3) epc to a published international application that has entered the european phaseORIGINAL CODE: 0009012PUAI | PUAI | EP |
Numbers
- Publication
- 0945404
- Publication, DOCDB
- 0945404
- Publication, EPODOC
- EP0945404
- Application
- 99105641
- Application, DOCDB
- 99105641
- Application, EPODOC
- EP19990105641
Titles3
- German
- Perameisensäure und Peressigsäure enthaltendes wässriges Desinfektionsmittel, Verfahren zu dessen Herstellung und dessen Verwendung
- English
- Aqueous disinfectant, comprising performic and peracetic acid, method of preparation and use
- French
- Agent désinfectant aqueux à base d'acide performique et d'acide peracétique,son procédé de préparation et son utilisation
Classification
- CPC, 2
- C02F1/722
- C02F1/50
- IPC, 6
- C07C407 00
- A01N59 00
- C02F1 50
- C02F1 72
- C07C409 24
- C07C409 26
Designated states10
- Contracting states, 10
- Austria
- Belgium
- Germany
- Spain
- Finland
- France
- United Kingdom
- Italy
- Netherlands (Kingdom of the)
- Sweden