WO2013107943A1 - Procédé de production de biocides à partir des eaux de processus industriels - Google Patents

Procédé de production de biocides à partir des eaux de processus industriels Download PDF

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Publication number
WO2013107943A1
WO2013107943A1 PCT/FI2013/050065 FI2013050065W WO2013107943A1 WO 2013107943 A1 WO2013107943 A1 WO 2013107943A1 FI 2013050065 W FI2013050065 W FI 2013050065W WO 2013107943 A1 WO2013107943 A1 WO 2013107943A1
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WO
WIPO (PCT)
Prior art keywords
electrolysis
water
conductivity
superfiltrate
biocides
Prior art date
Application number
PCT/FI2013/050065
Other languages
English (en)
Inventor
Heikki Pajari
Irina TSITKO
Pauliina TUKIAINEN
Jenni SIEVÄNEN
Tanaka Atsushi
Jari Kiuru
Original Assignee
Teknologian Tutkimuskeskus Vtt
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Teknologian Tutkimuskeskus Vtt filed Critical Teknologian Tutkimuskeskus Vtt
Priority to US14/373,051 priority Critical patent/US20140360885A1/en
Priority to EP13738656.1A priority patent/EP2804838A4/fr
Publication of WO2013107943A1 publication Critical patent/WO2013107943A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • C02F1/4674—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation with halogen or compound of halogens, e.g. chlorine, bromine
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/26—Chlorine; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/02—Non-contaminated water, e.g. for industrial water supply
    • C02F2103/023—Water in cooling circuits
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
    • C02F2103/28—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/29—Chlorine compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents

Definitions

  • the present invention relates to the production of biocides.
  • the present invention concerns a method of producing biocides from industrial process waters.
  • Microbes in the process can cause a multitude of production problems, from decreased production efficiency via impaired runnability and raw material spoilage to product safety issues [2, 3, 4].
  • biocide chemicals
  • They act either by killing microorganisms or by inhibiting the growth of micro-organisms.
  • An ideal biocide should meet several requirements such as: applicability over a wide range of operating conditions, no interference with other additives, broad spectrum of activity towards microbes, efficient and fast-acting, environmentally friendly and non-toxic, safe for the operator, low-cost, and easy-to -handle [2].
  • biocide Unfortunately, there is no biocide that can encompass all the requirements, and none of the biocides is suitable for all applications.
  • biocide strategy for a paper mill is always a compromise between the costs and performance. An insufficient use of biocides endangers the machine runnability and product quality [3, 5]. On the other hand, extensive use of biocides is not only expensive, but may result in unwanted interactions with the process and other chemicals [6, 7].
  • biocide development has been rapid. Reductive biocides were first replaced by strong oxidizers. After noticing the problems with the strong oxidizers [7] the development has been towards weak oxidizers and stabilized halogens. Both continuous and batch additions of these biocides have been used [8]. Biocide usage and microbial growth both can cause chemical variations in papermaking processes [9]. Active compounds in predominant biocide programs are salts, they are dosed in certain pH, and they do interact with the process and with other chemicals.
  • Elevated conductivity, charge, and dissolved calcium levels have shown to increase the formation of defects on paper machine [10, 11] have showed that stable chemical conditions together with functioning microbial control enable stable production and acceptable product quality. Elevated and fluctuating conductivity due to the salts added with biocides might be a thread to paper machine runnability. On the other hand, also the problems due to storage and transportation of hazardous materials related to biocide production and use - as well as corrosion and waste water quality issues related to halogen usage, should not be forgotten.
  • Biocides contain salts which are usually detrimental to the process the chemical are dosed into.
  • the present invention is based on the concept of utilizing industrial process water for producing biocides.
  • Existing technologies do not utilize process waters for biocide generation.
  • biocides are generated using brine solutions external to the process.
  • Predominant technologies do not even provide on-site applications. Inactivation of bacteria in an electrolysis cell has been carried out but the application in industrial process waters has not been conducted.
  • the present invention provides a method in which an industrial process water flow containing ions causing conductivity is fed through an electrolysis cell.
  • electrochemical treatment partly converts these compounds into chemicals with biocidal performance.
  • Commercial cells can be used. Cell construction and operation parameters can be modified according to the application. More specifically, the present invention is mainly characterized by what is stated in the characterizing part of claim 1.
  • the present technology with (preferably direct) electrolysis of process water is capable of inactivating in practice all commonly present microbes in sample.
  • the electrolysis disclosed in the examples generated excess amount of biocidal compounds.
  • the electrolyzed fractions can be utilized as biocide to treat other process flows.
  • the technology has been shown to be effective also in samples with high consistency.
  • the electrolysis performance can be increased by compensating the salt loss with the addition of salt.
  • This technology decreases the conductivity level of the process by decreasing the halogen concentration. This has several advantages from process efficiency, chemical performance, corrosion, and waste water management perspectives.
  • the present technology finds broad application. Thus, it can be carried out using papermaking process waters (for example shower water, filtrate water, white water, headbox furnish or broke).
  • papermaking process waters for example shower water, filtrate water, white water, headbox furnish or broke.
  • the concept is applicable to any aqueous process requiring microbial control, such as fresh and waste water systems, cooling systems, fermentation, mining and biorefming.
  • the electrolysis technology is highly cost-efficient. It does away with the costs of raw materials for producing biocides. It can be estimated that the total costs for applications at, e.g., a paper mill would be on the order of 0.2 €/ton of paper.
  • Figure 1 is a bar chart showing the total bacterial count for each sample (in logarithmic scale);
  • Figure 2 shows in perspective view an EC-electro MP-cell
  • Figure 3 indicates in graphical form the experimental setup with one compartment MP- cell
  • Figure 4 shows the effects of current and flow rate on total bacterial count in SUPER sample.
  • the flow rate was fixed at 80mL/min in the current trials (left), while current levels were fixed at 4 A and 7 A in the flow rate trial (right);
  • Figure 5 indicates biocidability of electrolyzed superfiltrate against (a) original
  • Figure 6 shows biocidability of supernatant fractions of (a) white water and (b) headbox furnish. Total bacterial count was plotted against different dosage levels;
  • Figure 7 shows free available chlorine in the electrolyzed superfiltrate, as a function of time after electrolysis. Measurement with photometer, Dulcotest DTI ⁇ Prominent);
  • Figure 8 shows the total bacterial count for the superfiltrate mixtures (original superfiltrate + electrolyzed superfiltrate) in two dosage levels (25% and 33%). They were mixed with time delay to check time dependence;
  • Figure 9 indicates the pH of the superfiltrate mixtures (original superfiltrate + electrolyzed superfiltrate, cf. Fig. 5a);
  • Figure 10 shows biocidability of electrolyzed superfiltrate against original superfiltrate at the controlled pH level, (a) Total bacterial count was plotted against different dosage levels, (b) pH was kept at 8.3-8.4 in all the testing points;
  • Figure 11 indicates the conductivity of the superfiltrate mixtures (original superfiltrate + electrolyzed superfiltrate, cf. Fig. 5a);
  • Figure 12 shows biocidability of electro lyzed superfiltrate against white water at controlled conductivity by adding sodium chloride, (a) Total bacterial count was plotted against different dosage levels, (b) Conductivity was kept at ⁇ 1.05mS/cm in all the testing points;
  • Figure 13 shows biocidability of electro lyzed superfiltrate against white water at controlled conductivity by adding sodium bicarbonate, (a) Total bacterial count was plotted against different dosage levels, (b) Conductivity was kept at ⁇ 1.07mS/cm in all the testing points;
  • Figure 14 indicates biocidability of electrolyzed superfiltrate against white water at controlled sodium carbonate, (a) Total bacterial count was plotted against different Conductivity was kept at ⁇ 1.07mS/cm in all the testing points; and
  • Figure 15 shows voltage in electrolysis at different conductivities (current was constant as 10A). Conductivity was controlled by adding NaCl or Na 2 C03.
  • Electrolysis considerably reduces the need of halogen containing biocides, thus lessening risk of corrosion.
  • the electrolysis concept is capable of decreasing the concentration of halogens in the process waters.
  • the conductivity of the process waters decreased indicating process purifying effect in addition to biocidal effects.
  • a water flow containing ions, such as halogens, which give rise to conductivity are conducted through an electrolysis cell in order to generate chemicals with biocidal performance.
  • ions such as halogens
  • the halogens are typically comprised of chlorine or bromine compounds.
  • the method comprises, in a preferred embodiment, simultaneously decreasing the conductivity level of the process water by decreasing the halogen concentration.
  • process water flow is subjected to direct electrolysis.
  • the process water flow is subjected to electrolysis in order to reduce conductivity of the water with at least 5 %, in particular at least 10 % and preferably with at least 15 to 85 %, e.g. with at least 20 %.
  • the water is subjected to electrolysis in an electrochemical cell.
  • the water is subjected to electrolysis using a current in the range of 0.1 to 1000 A, for example about 1 to 150 A, for example 1 to 100 A.
  • the voltage of the electrolysis varies broadly, from for example about 0.1 to 1000 V, for example the voltage is about 1 to 250 V.
  • the electrolysis can be carried out for clear water streams.
  • the method can also be carried out for process waters having a consistency of about 0.1 to 20 % by mass.
  • Table 1 Process water and furnishes from a Finnish fine paper mill
  • Figure 1 shows the total bacterial count for each sample (in logarithmic scale).
  • the electrochemical cell EC-Electro MP (Electrocell, Denmark) was employed for electrolysis. This is a modular multipurpose cell intended for process evaluations and experimental tests on laboratory scale. The structure of this filter-press type cell is shown in Fig.2. The projected electrode area was 200cm2, and the distance between cathode and anode was 3mm. Titanium was employed as cathode, while DSA (Dimensionally Stable Anode) as anode. DSA is iridium and ruthenium oxide coated titanium. According to the distributor, the ratio of iridium oxide and ruthenium oxide is 70/30. It has high oxygen over-potential and is corrosion-resistant.
  • Switch-Kraft Type SK 075 B (Kraftelektronik AB, Sweden) was used in the electrolysis.
  • the maximum current and voltage of this rectifier are 50A and 15 V, respectively.
  • All the electrolysis experiments were in the controlled-current mode and anode was continuously cooled down by water circulation system at 5°C. Experimental setup is shown in Fig.3. Superfiltrate sample was pumped into the cell where electrolysis was taking place. The temperature of the product was monitored after the cell, and the mixture of chlorine and oxygen gases was diluted with air and discharged. H, ORP (oxidation reduction potential) and conductivity were also measured. All of this data was recorded in a computer.
  • Treated white water samples were taken aseptically from test trials and transported in sterile plastic vials to laboratory. Samples were cultured within three hours. Logarithmic dilution series were prepared using sterile Ringer's solution. Culturing was performed by pipetting and spreading 1ml diluted sample on Aerobic Count Petrifilm (AC). Incubation took place in 30°C for 3 days. Red colonies were counted from AC Petrifilms containing 3 to 300 colonies.
  • AC Aerobic Count Petrifilm
  • Fig.4 Total bacterial count in the electrolyzed superfiltrate water was given in Fig.4. Bacteria were killed in electrolysis cell. The number depends on the current and flow rate, i.e. higher current or lower flow rate was more effective to reduce the bacteria. For this filtrate water, >4A current with ⁇ 80mL/min flow rate turned out to be enough to kill almost all bacteria. In practice this indicates, that the approach is more than capable of treating the process samples to ensure microbiologically clean process. In fact, it is probable that in case of high current and/or low flow rate the electrolysis generates excess amount of biocidal compounds.
  • Figure 4 shows the effects of current and flow rate on total bacterial count in SUPER sample. Flow rate was fixed at 80mL/min in the current trials (left), while current levels were fixed at 4 A and 7 A in the flow rate trial (right).
  • Electrochemically treated process waters as biocide As shown in Fig.1 , total bacterial count of superfiltrate was not so high compared with white water, headbox furnish or broke. Therefore one can expect that superfiltrate processed with higher current should still retain biocidability. This was simply checked by mixing the electrolyzed superfiltrate (at 7A, 80mL/min) with the original superfiltrate. As shown in Fig.5a, it behaved as biocide as expected. 17% dosage was enough to kill 99% of bacteria in the original superfiltrate. It was also mixed with other samples to find its biocidability too (Figs. 5b, 5c, 5d). Here higher dosage (33%) was required to kill 99% bacteria, simply due to larger number of bacteria in those samples. Also higher fiber consistency of the other samples may have affected the reduced biocide performance. This is well known feature of some oxidants, which are not highly selective in killing but are consumed by all organic material in the sample.
  • Figure 5 shows biocidability of electrolyzed superfiltrate against (a) original superfiltrate, (b) white water, (c) headbox furnish and (d) broke. Total bacterial count was plotted against different dosage levels.
  • hypochloric acid is known to be the most effective biocidal compound in hypochlorite solution and its concentration is known to increase along decreasing pH.
  • the effect of pH can be considered as rather insignificant for the biocide performance.
  • For chemical stability of papermaking pH stability is known to be highly important [12, 13]. Therefore pH control of electrolysis flow according to process pH is recommended.
  • hypochlorite As a halogen source.
  • Commercial hypochlorite generation generates equal amount of salt (C12(g) + 2NaOH ⁇ NaOCl + NaCl + H20). This salt amount in hypochlorite solution also further increases when hypochlorite decomposes. This means that in practice
  • hypochlorite sodium chloride (salt).
  • This salt addition has several disadvantages: Conductivity increase affect chemical interactions of particles in the process causing problems with retention, flocculation etc. Unnecessarily added chloride increases risk of corrosion. Any halogen addition increases the AOX (Adsobable Organic Halogen) load to waste waters. The electrolysis approach eliminates all these disadvantages. No salt is added - actually the salt amount is reduced as shown in Fig. l 1. This approach actually also enables addition of biocides without detrimental effects.
  • NaCl was the most effective. In terms of energy consumption, NaCl was also effective, i.e. voltage reduction by IV (8.7V ⁇ 7.7V at 7A). On the other hand,
  • NaHC03 and Na2C03 influenced little on the energy consumption. Extensive addition cases are compared in Fig.15 for NaCl and Na2C03. The voltage decreased linearly with conductivity increase in both cases.
  • the present novel technology does not require any transportation or production of hazardous materials. No biocides need to be transported to the production units. Actually the present technology does not require any transportation at all. Also the raw material for the on-site biocide production is extracted from the process. In case the biocide generation is boosted by the salt addition, only shipping of salt is required. Otherwise only electricity is needed. Also storage needs are minimal since the production can be performed according to the need. This is also recommended due to degradation of active compounds. References:

Abstract

Procédé de production de biocides à partir d'un flux aqueux d'eau de processus, ledit procédé comprenant l'étape consistant à guider un flux d'eau contenant des ions induisant la conductivité à travers une cellule électrolytique, afin de produire des produits chimiques à propriétés biocides. Le procédé peut être utilisé dans les systèmes de traitement d'eau douce et d'eaux usées, tels que des circuits d'eau pour systèmes de refroidissement, de fermentation, d'exploitation minière et de bioraffinage, par exemple les eaux résiduaires de papeterie. Il peut être utilisé pour réduire la concentration en halogènes.
PCT/FI2013/050065 2012-01-20 2013-01-21 Procédé de production de biocides à partir des eaux de processus industriels WO2013107943A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US14/373,051 US20140360885A1 (en) 2012-01-20 2013-01-21 Method of producing biocides from industrial process waters
EP13738656.1A EP2804838A4 (fr) 2012-01-20 2013-01-21 Procédé de production de biocides à partir des eaux de processus industriels

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201261588686P 2012-01-20 2012-01-20
US61/588,686 2012-01-20

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WO2013107943A1 true WO2013107943A1 (fr) 2013-07-25

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WO (1) WO2013107943A1 (fr)

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US20160326024A1 (en) * 2015-05-08 2016-11-10 Emo3 Inc. Water disinfection apparatus and method for disinfection of recirculated water in a cooling tower
WO2019006323A1 (fr) * 2017-06-30 2019-01-03 Ohio University Décontamination de fluides par un chauffage par effet joule

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JP2002138393A (ja) * 2000-10-25 2002-05-14 Mitsubishi Paper Mills Ltd 製紙工程における微生物の抑制方法およびこれを用いて製造された紙
EP1698594A1 (fr) * 2005-03-04 2006-09-06 Ecodis Procédé pour éliminer les polluants des fluides à base d'eau
WO2006103314A1 (fr) * 2005-03-30 2006-10-05 Oy Keskuslaboratorio-Centrallaboratorium Ab Procede electrochimique pour preparer des solutions microbiocides
EP1860071A1 (fr) * 2005-03-16 2007-11-28 Koganei Corporation Procede et appareil de nettoyage de l'eau de circulation
US20090173635A1 (en) * 2008-01-04 2009-07-09 Puricore, Inc. System and method for controlling the generation of a biocidal liquid

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AT377546B (de) * 1983-02-25 1985-03-25 Dieter J Becker Verfahren zur reinigung von bei der zellstoffherstellung, insbesondere bei der chlorbleiche von zellstoff, anfallenden abwaessern
DE4435631C2 (de) * 1993-05-01 1996-07-04 Wolfgang Alexander Huber Verfahren zum Ausschleusen von Mangan aus Prozeßwassern in der Papier-, Zellstoff- und übrigen fasererzeugenden und faserbearbeitenden Industrie beim chlorfreien Bleichen des Faserstoffes
US20040013563A1 (en) * 2000-05-19 2004-01-22 Romer Edward Adolph Cooling tower maintenance
IT1400219B1 (it) * 2009-03-27 2013-05-24 Eni Spa Processo per la produzione di una composizione acquosa biocida da acqua di produzione derivante da pozzi petroliferi o a gas e composizione acquosa biocida
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JP2002138393A (ja) * 2000-10-25 2002-05-14 Mitsubishi Paper Mills Ltd 製紙工程における微生物の抑制方法およびこれを用いて製造された紙
EP1698594A1 (fr) * 2005-03-04 2006-09-06 Ecodis Procédé pour éliminer les polluants des fluides à base d'eau
EP1860071A1 (fr) * 2005-03-16 2007-11-28 Koganei Corporation Procede et appareil de nettoyage de l'eau de circulation
WO2006103314A1 (fr) * 2005-03-30 2006-10-05 Oy Keskuslaboratorio-Centrallaboratorium Ab Procede electrochimique pour preparer des solutions microbiocides
US20090173635A1 (en) * 2008-01-04 2009-07-09 Puricore, Inc. System and method for controlling the generation of a biocidal liquid

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Title
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EP2804838A4 (fr) 2015-08-05
US20140360885A1 (en) 2014-12-11
EP2804838A1 (fr) 2014-11-26

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