Method of cleaning equipment and filters

FIELD: cleaning apparatus.

SUBSTANCE: method comprises setting the filters and equipment in a contact with the cyclic nitroxyl and repeated oxidizer made of per acid or its salt or cyclic nitroxyl and repeated oxidizer made of hydroperoxide, or compound free of brome.

EFFECT: improved quality of cleaning.

9 cl, 4 tbl, 5 ex

 

The invention relates to a method of cleaning equipment for processing of food products, in particular membrane filters, which are used for food or for water purification, in which the filters are in contact with cyclic nitroxyl compound and re-oxidizing agent, or with cyclic nitrosonium connection.

The food industry uses membrane filters with increasing degree of purification, in particular plastic membrane, such as polyvinylpyrrolidone, polysulfone, polyethersulfone and certain types of polyamides, to remove unwanted insoluble substances from beverages and other liquids. Such membranes are also used for treatment of surface water. Such membranes provide adequate removal of undesirable constituent particles, in particular microorganisms, such as algae, fungi and bacteria.

However, the problem is that such membrane filters completely blocked after a short period of time, so that they become unusable. Blocked filters can be regenerated, for example, by washing in the opposite direction. However, this is a complex process, and it becomes ineffective at long term use, because the pollution accumulates. In addition, it is difficult UDA is resolved to some persistent organic pollutants in this way.

WO 97/45523 describes the use of 2,2,6,6-tetramethylpiperidine-N-oxyl (TAMRA) as nitroxyl compounds and hypochlorite and hypobromite as a re-oxidizing agent, for cleaning modules deposition of beer. The presence of residues of Halogens, especially bromine residues, is highly undesirable in the equipment used for the preparation or processing of beverages and other food products. The presence of bromine compounds having a negative impact on the durability of the filters and their tensile strength.

WO 99/15256 discloses the use of cyclic nitroxyl compounds, such as TAMRA, together with the agent, sequestered calcium, cleaning filters, which are designed for use when cleaning the surface of the water.

The oxidation of hydrocarbons and other primary alcohols nitroxyl compounds and percolate, in particular peracetic acid in the presence of catalytic amounts of bromine, in itself known from WO 99/57158.

It was found that the filters and other equipment used in the food industry and beverage industry and in water treatment, can effectively clean in halogen-free method by applying a cyclic nitroxyl compound. Re oxidant nitroxyl compound can be percolate or hydropeaking is/or metal complex, for example, in the form of an oxidative enzyme.

The following is a description of a cyclic nitroxyl compounds intended for use in the present invention, are described on the example of TAMRO only for purposes of simplicity, but it should be understood that other di-tert-alkylperoxy, such as 4,4-dimethyloxazolidine-N-oxyl (DOXYL), of 2.2.5.5-tetramethylpyrrolidine-N-oxyl (PROXYL) and 4-hydroxyamino and their derivatives and compounds described in WO 95/07303 can replace TEMRO. Especially preferred are TEMRO, 4-acetamidoxime and 4 acetoxidans. A catalytic amount of nitroxyl is preferably 0.1 to 2.5 wt.% on the basis of primary alcohol or 0.1 to 2.5 mol % in relation to the primary alcohol.

Percolate can be any paracanoe acid, such as peracetic acid, phenpropionate acid, Pelourinho acid, etc., substituted alkanoate acid, such as peroxiderythromycin acid, optionally substituted aromatic percolate, such as derbentina acid or m-chloroperbenzoic acid, or inorganic percolate, such as personna acid or permanganate acid. Percolate can be formed in situ from a precursor, such as an appropriate aldehyde, carboxylic acid, acid anhydride, ester or acid amide, such as tetr the-acetylethylenediamine (TAED), with a suitable devoid of halogen oxidizing agent such as hydrogen peroxide or oxygen, either before oxidation reaction, or during the oxidation reaction, or perborate, or percarbonate or similar compounds, in the presence of alleluya agents, such as TAED. Percolate re-oxidizes spent nitroxyl in situ to obtain ion nitracline, which is an effective oxidizing agent in the purification method of the invention. Percolate usually used in a concentration in the cleaning liquid 25 to 2500 ppm (from about 25 mg to 2.5 g per 1 liter). Percolate can be used by themselves or in the form of suitable salts, especially alkali metal salt. A suitable form of personnel acid is, for example, Oxone® (2KHSO5·KHSO4·K2SO4), which is commercially available.

Re-oxidation of the spent nitroxyl in situ can also be done using gidroperekisi or metal complex, or, preferably, both of these compounds, and the metal complex is an intermediate oxidant. The metal complex may include, for example, vanadium, manganese, iron, cobalt, Nickel or copper complexing agent, in particular polyamines, such as 2,2'-bipyridyl, phenanthroline, tetramethylethylenediamine, pentamer Diethylenetriamine and their cyclic equivalents, such as 1,4,7-trimethyl-1,4,7-triazone, and histidine and its oligomers. Hydropeaking can represent hydrogen or alkyl and Gidropress ar(ALK)silt (such as hydropeaking tert-butyl), preferably hydrogen peroxide.

It was found that processing of membrane filters and other equipment, TAMRA and percolate, such as personna acid, or hydropredict, leads to the cleansing action that equal to or better than the effect of treatment with hypochlorite/bromide, as described in WO 97/45523, and has the additional advantage that, according to the estimations using a measurement of the strength of the membrane, the membrane filters are not attacked by the cleaning agents prior to any detectable level. In addition, the absence of halogen represents a significant advantage for environmental reasons, but also in relation to the strength of the processing equipment, especially in the case of membranes.

Nitroxyl can also be oxidized in a separate reaction for the formation of ion nitroxide ex situ. This can be accomplished with the use of metal complexes as described above, such as copper/bipyridyl and oxygen or hydrogen peroxide, or oxidative enzyme such as lacasa, in the presence of oxygen. These methods are described in WO 00/50388 and WO 00/50621, which are included in this description as the e links. This embodiment has the significant advantage that the re-oxidizing agents, such as enzymes, metal complexes, hydrogen peroxide and similar agents, do not come into contact with filters or other equipment subject to the clearing.

The method of the invention can be used for cleaning the filters used in the food industry and feed industry, and equipment used in water treatment. Such equipment can, in particular, to use in the production of dairy products, beer, wine, fruit juices and other beverages and liquids used in food processing. Suitable examples of such equipment include pipes of different diameters, the capillaries, the mixing device and, in particular, filters. The filter may be of any type, including polymer membrane in which the polymer can be a polyvinylpyrrolidone, a polysulfone, polyethersulfone and certain types of polyamides, and ceramic membrane made, for example, from silicon dioxide, aluminum oxide, etc.

The method of the invention can be made by oxidation and/or solubilization of hydrocarbons and other primary alcohols with high molecular weight, such as protein materials, polyphenolic compounds in the residues to be removed from fil the ditch. Such procedures purification is preferably carried out by the processing equipment in an aqueous solution of nitroxyl compounds and percolate. The concentration of nitroxyl compounds can mainly be in the range from 1 to 100 mg per 1 g, in particular from 3 to 30 mg/ml, and the concentration of percolate may be in the range from 0.025 to 10 g per 1 l, in particular 0.25 to 2.5 g/L. the Method of the invention can be performed in a static way, i.e. by processing batches of equipment in a suitable container containing a processing fluid, during the period from several seconds to several hours, in particular from 3 min to 1 h Method can also provide a dynamic way, i.e. the way in which permanent or semi-permanent flow of the processing liquid is passed over the equipment or through it, for example, with a speed of 5 ml to 10 l/min, depending on the size of the equipment. After processing nitroxyl and percolate equipment should be washed with washing liquid which can be water or neutralizing an aqueous liquid, or an organic solvent, such as alcohol, or their mixture, or their sequential combination. Further details on catalyzed by nitroxyl processing filters and other equipment in the food industry can be found in WO 97/45523, which included the present description by reference. In WO 99/15256, which is included in the description by reference, provides further details on the catalyzed nitroxyl processing filters in water treatment.

Example 1:Cleaning filters using hypochlorite/TAMRO

The filtration membrane (hollow tube containing 40 hollow fiber membrane (pore size 0.5 Ám) with a total surface area of 0.04 m2(reminiscent of the modules R-100 x-ray flux used in large-scale installations) used to filter beer. Membranes were contaminated using the technique of dead-end filtration until the pores are not blocked, resulting in minimal penetration or current.

A solution containing 1000 ppm of hypochlorite and 35 ppm of TAMRO, within half an hour was used to clean the membranes. the pH of the reaction solution was brought to 10. The cold water flow (PVC) unused membranes amounted to 6000 l/h/m2. PVC after cleaning was also 6000 l/h/m2.

Example 2:Cleaning filters using hypochlorite/bromide/TAMRO

A solution containing 1000 ppm of hypochlorite 60 ppm of bromide and 35 ppm of TAMRO, within half an hour used to clean membranes, contaminated in accordance with example 1. the pH of the reaction solution was brought to 10. The cold water flow (PVC) unused membranes amounted to 6000 l/h/m2. PVC on the Le purification was also 6000 l/h/m 2.

Example 3:Cleaning filters using peroxisomal acid/TAMRO

A solution containing 1000 ppm peroxisomal acid and 35 ppm of TAMRO, within half an hour used to clean membranes, contaminated in accordance with example 1. the pH of the reaction solution was brought to 8. The cold water flow (PVC) unused membranes amounted to 6000 l/h/m2. PVC after cleaning was also 6000 l/h/m2.

Example 4:Cleaning filters using manganese complex/hydrogen peroxide/TAMRO

Purified membrane contaminated in accordance with example 1. To clean the membranes used the following sequence of manipulations: cleanup started pre-treatment by washing the membranes with 0.5 M sodium hydroxide for 10 min, followed by washing with a solution containing 2000 ppm of hydrogen peroxide (or 2000 ppm peracetic acid), 100 ppm of TAMRA and 50 ppm Mn complex with 1,4,7-trimethyl-1,4,7-triazone, within half an hour. the pH of the reaction solution was brought to 10. The cold water flow (PVC) unused membranes amounted to 6000 l/h/m2. PVC after cleaning was also 6000 l/h/m2.

Example 5:The data stability of membranes

(a) Stability in water:

6 membranes (type MF05 M2 1.5 mm), obtained from a module unused membranes (type RX 300), POM is looking in the vessel, containing water at ambient temperature for 2 months. At the end of the experiment measured the force required to fracture membranes, with the tester, material to the company Stable Micro Systems type TA-HD, equipped cell 50 N. the Results are presented in table 1.

Table 1

The maximum force required for fracture membrane
MembraneThe maximum power of destruction (N)
19,31
29,12
39,82
49,77
5of 9.21
68,88
Average 9,35 N

The standard deviation of 0.37

(b) the Effect of sodium hypochlorite:

7 membranes (type MF05 M2 1.5 mm), obtained from a module unused membranes (type RX 300), was placed in a vessel containing a cleaning solution (35 ppm, TAMRA, 1000 ppm sodium hypochlorite at pH 10 and ambient temperature). The cleaning solution was refreshed every week for 2 months. At the end of the experiment measured the force required to fracture membranes, using a tester material from Stable Micro Systems type TA-HD, equipped cell 50 N. the Results are presented in table 2.

Table 2

The maximum force required for fracture membrane
MembraneThe maximum power of destruction (N)
1to 4.98
26,40
34,85
4of 6.49
55,80
65,16
75,96
Average 5,66 N

The standard deviation 0,673

(C) Effect of sodium hypochlorite/sodium bromide:

8 membranes (type MF05 M2 1.5 mm), obtained from a module unused membranes (type RX 300), was placed in a vessel containing a cleaning solution (35 ppm, TAMRA, 1000 ppm of sodium hypochlorite and 60 ppm sodium bromide at pH 10 and ambient temperature). The cleaning solution was refreshed every week for 2 months. At the end of the experiment measured the force required to fracture membranes, with the tester, material to the company Stable Micro Systems type TA-HD, equipped cell 50 N. the Results are presented in table 3.

5,03
Table 3

The maximum force required for fracture membranes
MembraneThe maximum power of destruction (N)
1
25,98
36,03
44,24
5of 5.83
66,55
73,36
84,58
Average 5,20 N

The standard deviation 1,085

(d) the Effect of peroxisomal acid:

6 membranes (type MF05 M2 1.5 mm), obtained from a module unused membranes (type RX 300), was placed in a vessel containing a cleaning solution (35 ppm, TAMRA, 1000 ppm peroxisomal acid at pH 8 and ambient temperature). The cleaning solution was refreshed every week for 2 months. At the end of the experiment measured the force required to fracture membranes, with the tester, material to the company Stable Micro Systems type TA-HD, equipped cell 50 N. the Results are presented in table 4.

tr>
Table 4

The maximum force required for fracture membranes
MembraneThe maximum power of destruction (N)
19,50
28,79
3was 9.33
48,60
5for 9.47
68,48
The average value of 9, 30 N

The standard deviation 0,46

You should make a conclusion that the membrane susceptible to destruction when oxidants such as hypochlorite/bromide (hypohalite), used in combination with TAMRA as a cleaning agent. The standard deviation of the forces required to fracture membranes, increases significantly due to the addition of bromide to a solution of hypochlorite/TAMRO. Therefore, the chance of destroying the membranes during the full-scale filter (e.g., beer) was significantly higher when the bromide is added to the cleaning solution (AMRO/hypochlorite).

In addition, the use peroxisomal acid in combination with TAMRA seems, has a very small effect on the membrane from the point of view of destruction. Use peroxisomal acid in combination with TAMRA as a cleaning agent is more favorable than hypohalite/TAMRO, due to the fact that the waste does not contain Halogens. Another important advantage peroxisomal acid is that, compared to hypohalite combinations, no corrosion filtration equipment.

1. Free from halogen-free way of cleaning equipment for food processing, including the introduction of equipment in contact with

(a) cyclically what nitroxyl and re-oxidant in the form of percolate or a salt thereof, or

(b) cyclic nitroxyl and re-oxidant in the form of gidroperekisi, or

(C) nitrosonium connection.

2. The method according to claim 1 where the re-oxidizing agent is percolate or its salt.

3. The method according to claim 2, where percolate is a peracetic acid.

4. The method according to claim 2, where percolate is persero acid.

5. The method according to any of claim 2 to 4, where percolate receive in situ from hydrogen peroxide or a compound releasing hydrogen peroxide.

6. The method according to claim 1, where Gidropress represents hydrogen peroxide in the presence of a metal complex or oxidative enzyme.

7. The method according to any of claim 2 to 4, where again the oxidizing agent used in aqueous solution at a concentration of 25-2500 ppm

8. The method according to any one of claims 1 to 4 or 6, where the cyclic nitroxyl compound is a 2,2,6,6-tetramethylpiperidine-N-oxyl (TEMPO) or 4-hydroxy-, 4-acyloxy - or 4-acylamino derived.

9. The method according to claim 1, where nitrosonium compound was obtained previously using a metal complex or oxidative enzyme.

10. The method according to any one of claims 1 to 4 or 6, where the equipment includes a membrane filter.



 

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