NO326063B1 - Impregnated salts, preservatives and processes for the preparation and use of said salts and preservatives. - Google Patents
Impregnated salts, preservatives and processes for the preparation and use of said salts and preservatives. Download PDFInfo
- Publication number
- NO326063B1 NO326063B1 NO20001174A NO20001174A NO326063B1 NO 326063 B1 NO326063 B1 NO 326063B1 NO 20001174 A NO20001174 A NO 20001174A NO 20001174 A NO20001174 A NO 20001174A NO 326063 B1 NO326063 B1 NO 326063B1
- Authority
- NO
- Norway
- Prior art keywords
- salts
- acid
- impregnated
- salt
- carboxylic acid
- Prior art date
Links
- 150000003839 salts Chemical class 0.000 title claims abstract description 117
- 239000003755 preservative agent Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims description 14
- 238000002360 preparation method Methods 0.000 title description 7
- 150000001735 carboxylic acids Chemical class 0.000 claims abstract description 30
- 150000001734 carboxylic acid salts Chemical class 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 241001465754 Metazoa Species 0.000 claims abstract description 11
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- 239000010985 leather Substances 0.000 claims abstract description 4
- 239000004460 silage Substances 0.000 claims abstract description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 42
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 32
- 239000002253 acid Substances 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 26
- 239000003223 protective agent Substances 0.000 claims description 22
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 21
- 235000019253 formic acid Nutrition 0.000 claims description 21
- 239000011230 binding agent Substances 0.000 claims description 18
- 235000019260 propionic acid Nutrition 0.000 claims description 16
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 16
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- 230000002335 preservative effect Effects 0.000 claims description 13
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- 230000002776 aggregation Effects 0.000 claims description 11
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 150000001413 amino acids Chemical class 0.000 claims description 4
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- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 2
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C1/00—Chemical treatment prior to tanning
- C14C1/02—Curing raw hides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
- A23K30/10—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs of green fodder
- A23K30/15—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs of green fodder using chemicals or microorganisms for ensilaging
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
Foreliggende oppfinnelse vedrører impregnerte salter, konserveringsmiddel og fremgangsmåte for fremstilling og anvendelse av nevnte salter og konserveringsmiddel. The present invention relates to impregnated salts, preservatives and methods for the production and use of said salts and preservatives.
Foreliggende oppfinnelse angår følgelig impregnerte salter kjennetegnet ved at de omfatter minst ett salt av én eller flere karboksylsyrer som er blitt impregnert med fra 0,5 til 30 vekt%, basert på karboksylsyresaltet, av minst én flytende karboksylsyre. The present invention therefore relates to impregnated salts characterized in that they comprise at least one salt of one or more carboxylic acids which have been impregnated with from 0.5 to 30% by weight, based on the carboxylic acid salt, of at least one liquid carboxylic acid.
Videre omfatter foreliggende oppfinnelse konserveringsmiddel kjennetegnet ved at det omfatter et impregnert salt ifølge krav 1. Furthermore, the present invention comprises a preservative characterized in that it comprises an impregnated salt according to claim 1.
Oppfinnelsen angår videre en fremgangsmåte for fremstilling av de impregnerte salter ifølge krav 1, kjennetegnet ved at den omfatter impregnering av minst ett salt av en karboksylsyre eller en blanding av karboksylsyrer med minst én flytende karboksylsyre til konsentrasjonen er 30 vekt%, basert på karboksylsyresaltet. The invention further relates to a method for producing the impregnated salts according to claim 1, characterized in that it comprises the impregnation of at least one salt of a carboxylic acid or a mixture of carboxylic acids with at least one liquid carboxylic acid until the concentration is 30% by weight, based on the carboxylic acid salt.
Foreliggende oppfinnelse vedrører videre en fremgangsmåte for fremstilling av et konserveringsmiddel ifølge krav 6, kjennetegnet ved at den omfatter blanding av impregnerte salter ifølge krav 1, med én eller flere bærere og/eller utformnings-hjelpemidler, og agglomerering med eller uten tilsetting av minst ett bindemiddel. The present invention further relates to a method for producing a preservative according to claim 6, characterized in that it comprises mixing impregnated salts according to claim 1, with one or more carriers and/or shaping aids, and agglomeration with or without the addition of at least one binder .
Oppfinnelsen vedrører også anvendelse av de impregnerte salter ifølge krav 1, eller av konserveringsmidlet ifølge krav 6, for syrebehandling, for konservering av menneske- og dyreføde, eller for anvendelse i silofor eller for lærbehandling. The invention also relates to the use of the impregnated salts according to claim 1, or of the preservative according to claim 6, for acid treatment, for the preservation of human and animal food, or for use in silage or for leather treatment.
Kortkjedede organiske syrer så som maursyre, eddiksyre eller propionsyre anvendes for surgjøring og konservering av menneske- og dyreføde. Ulemper med disse syrer er for eksempel deres flytende aggregasjonstilstand ved romtemperatur, den skarpe eller stikkende lukt som kommer av det lave damptrykk, samt deres korrosivitet. Short-chain organic acids such as formic acid, acetic acid or propionic acid are used for acidification and preservation of human and animal food. Disadvantages of these acids are, for example, their liquid state of aggregation at room temperature, the sharp or pungent smell that comes from the low vapor pressure, as well as their corrosiveness.
De flytende organiske syrer kan dessuten bare med betydelig teknisk kompleksitet innarbeides i konsentrert form, for eksempel i dyreføde. Furthermore, the liquid organic acids can only be incorporated in concentrated form, for example in animal feed, with considerable technical complexity.
DE 28 33 727 A1 beskriver et partikkelformig fungicid materiale som omfatter propionsyre og et bærermateriale. Det sies at med dette materiale er det ingen økning i antallet muggsoppkolonier på lagrede landbruks-innhøstnings-produkter selv etter inkubering i flere dager. Det har imidlertid vist seg at materiale av denne type i seg selv ikke er stabilt ved lagring (tap av syre); og den maksimale mengde av propionsyre som kan påføres, avhenger i stor grad av det anvendte bærermateriale. Det oppstår dessuten ubehagelige lukter med dette materiale, på grunn av avdamping av propionsyren. DE 28 33 727 A1 describes a particulate fungicidal material comprising propionic acid and a carrier material. It is said that with this material there is no increase in the number of mold colonies on stored agricultural harvest products even after incubation for several days. However, it has been shown that material of this type in itself is not stable during storage (loss of acid); and the maximum amount of propionic acid that can be applied depends largely on the carrier material used. Unpleasant odors also occur with this material, due to evaporation of the propionic acid.
EP-A-0 590 856 og EP-A-0 608 975 beskriver blandinger av faste karboksylsyresalter og faste karboksylsyrer med lavere pKa enn karboksylsyren i de anvendte salter. Når denne blanding oppløses i vann, frigjøres karboksylsyrene fra saltene ved hjelp av karboksylsyren med den lavere pKa i en fortrengningsreaksjon. De resulterende nye salter med karboksylsyren med den lavere pKa er med fordel uløselige i vann og utfelles fra løsningen. En ulempe med disse blandinger er at det fremdeles er nødvendig å anvende forskjellige karboksylsyrer med forskjellige pKa-verdier for fremstilling av konserveringsmidlene. For å sikre at karboksylsyrene er fullstendig frigjort fra utgangs-karboksylsyresaltene (for eksempel fra kalsiumpropionat) ved oppløsing i vann, må karboksylsyrene med den lavere pKa (for eksempel maleinsyre) tilsettes i minst ekvimolare mengder, basert på karboksylgruppene som finnes i syrene. Dette begrenser innholdet av den individuelle aktive karboksylsyresubstans. Hvis uløselige karboksylsyresalter dannes ved denne frigjøring, må de i tillegg fjernes i en påfølgende reaksjon. EP-A-0 590 856 and EP-A-0 608 975 describe mixtures of solid carboxylic acid salts and solid carboxylic acids with a lower pKa than the carboxylic acid in the salts used. When this mixture is dissolved in water, the carboxylic acids are released from the salts by means of the carboxylic acid with the lower pKa in a displacement reaction. The resulting new salts with the carboxylic acid with the lower pKa are advantageously insoluble in water and precipitate from the solution. A disadvantage of these mixtures is that it is still necessary to use different carboxylic acids with different pKa values for the preparation of the preservatives. To ensure that the carboxylic acids are completely freed from the starting carboxylic acid salts (for example from calcium propionate) when dissolved in water, the carboxylic acids with the lower pKa (for example maleic acid) must be added in at least equimolar amounts, based on the carboxyl groups present in the acids. This limits the content of the individual active carboxylic acid substance. If insoluble carboxylic acid salts are formed by this release, they must also be removed in a subsequent reaction.
Det er et formål med foreliggende oppfinnelse å tilveiebringe nye preparater for behandling av menneske- og dyreføde, som ikke har de ovennevnte ulemper, og som uten vanskelighet kan blandes av brukeren i menneske- og dyreføden som skal behandles. Hovedmålet var å fremstille et fast materiale som har et maksimalt innhold av aktiv substans og som oppviser meget lite lukt, hvis noen. Det faste sluttprodukt bør ha gode lagrings-, strømnings- og bearbeidelsesegenskaper. It is an object of the present invention to provide new preparations for the treatment of human and animal food, which do not have the above-mentioned disadvantages, and which can be mixed by the user in the human and animal food to be treated without difficulty. The main aim was to produce a solid material which has a maximum content of active substance and which exhibits very little, if any, odour. The solid end product should have good storage, flow and processing properties.
Vi har funnet at dette formål oppnås ved hjelp av de nye impregnerte salter omfattende minst ett salt av én eller flere karboksylsyrer, hvilket salt er blitt impregnert med fra 0,5 til 30 vekt%, basert på karboksylsyresaltet, av minst én flytende karboksylsyre. We have found that this purpose is achieved by means of the new impregnated salts comprising at least one salt of one or more carboxylic acids, which salt has been impregnated with from 0.5 to 30% by weight, based on the carboxylic acid salt, of at least one liquid carboxylic acid.
Oppfinnelsen angår dessuten konserveringsmidler omfattende et impregnert salt av ovennevnte materiale. Konserveringsmidlene kan dessuten med fordel omfatte minst én bærer og/eller utformningshjelpemiddel, og kan, hvor hensiktsmessig, være belagt med et beskyttende middel og/eller et strøpulver. The invention also relates to preservatives comprising an impregnated salt of the above-mentioned material. The preservatives can also advantageously include at least one carrier and/or design aid, and can, where appropriate, be coated with a protective agent and/or a dusting powder.
Oppfinnelsen angår dessuten en fremgangsmåte for fremstilling av de impregnerte salter, som omfatter impregnering av minst ett salt av en karboksylsyre eller av en blanding av karboksylsyrer med minst én flytende karboksylsyre til konsentrasjonen er 30 vekt%, basert på karboksylsyresaltet. The invention also relates to a method for producing the impregnated salts, which comprises impregnation of at least one salt of a carboxylic acid or of a mixture of carboxylic acids with at least one liquid carboxylic acid until the concentration is 30% by weight, based on the carboxylic acid salt.
Oppfinnelsen angår dessuten fremstilling av konserveringsmidler omfattende et impregnert salt av ovennevnte produkt, som omfatter impregnerte salter omfattende minst ett salt av én eller flere karboksylsyrer, hvilket salt er blitt impregnert med fra 0,5 til 30 vekt% av minst én flytende karboksylsyre, som, hvor hensiktsmessig, blandes med minst én bærer og/eller minst ett utformningshjelpemiddel, og som agglomereres med eller uten tilsetting av ett eller flere bindemidler, og deretter blir konserveringsmidlene med fordel forsynt med et beskyttende middel som størkner ved romtemperatur (23°C), idet det beskyttende middel tilsettes i en mengde slik at de resulterende konserveringsmidler belegges, og hvor hensiktsmessig, bevirkes ytterligere odorisering for eksempel ved tilsetting av duftmidler. Konserveringsmidlene dannet på denne måte kan med fordel også belegges med et findispergert strøpulver for forbedring av konserveringsmidlenes strømningsegenskaper. The invention also relates to the production of preservatives comprising an impregnated salt of the above-mentioned product, which comprises impregnated salts comprising at least one salt of one or more carboxylic acids, which salt has been impregnated with from 0.5 to 30% by weight of at least one liquid carboxylic acid, which, where appropriate, is mixed with at least one carrier and/or at least one shaping aid, and which is agglomerated with or without the addition of one or more binders, and then the preservatives are advantageously provided with a protective agent which solidifies at room temperature (23°C), as the protective agent is added in an amount so that the resulting preservatives are coated, and where appropriate, further odorization is effected, for example by the addition of fragrances. The preservatives formed in this way can advantageously also be coated with a finely dispersed bedding powder to improve the flow properties of the preservatives.
De nye impregnerte salter eller konserveringsmidler har den fordel at syrens meget stikkende lukt reduseres. De impregnerte salter omfatter med fordel et innhold av aktiv substans på fra 68 til 75 vekt%, fortrinnsvis 70-73 vekt%, spesielt foretrukket 70-72 vekt%, totalt, basert på den totale mengde av karboksylsyrer som finnes i saltet og som er tilsatt. Både de nye impregnerte salter og konserveringsmidlene frigjør syreinnholdet effektivt og hurtig fra faststoffet og har gode lag-rings-, strømnings- og bearbeidelsesegenskaper. The new impregnated salts or preservatives have the advantage that the very pungent smell of the acid is reduced. The impregnated salts advantageously comprise a content of active substance of from 68 to 75% by weight, preferably 70-73% by weight, particularly preferably 70-72% by weight, in total, based on the total amount of carboxylic acids found in the salt and which are added. Both the new impregnated salts and the preservatives release the acid content efficiently and quickly from the solid and have good storage, flow and processing properties.
Flytende organiske syrer egnet for impregnering av karboksylsyresaltene er syrer eller blandinger av syrer som er flytende eller blir flytende ved bearbeidelsestemperaturene, fortrinnsvis ned til 40°C eller lavere. Liquid organic acids suitable for impregnation of the carboxylic acid salts are acids or mixtures of acids which are liquid or become liquid at the processing temperatures, preferably down to 40°C or lower.
Ci-C8-mono- og/eller dikarboksylsyrer og saltene av disse Ci-C8-mono-og/eller dikarboksylsyrer anvendes med fordel for fremstilling av de impregnerte salter eller for fremstilling av konserveringsmidlene. Alkalimetall-, jordalkalimetall-eller ammoniumsalter er egnet. Syrer så som maursyre, eddiksyre og/eller propionsyre og deres ammonium-, kalsium, litium-, natrium-, magnesium- og/eller kaliumsalter anvendes fortrinnsvis. Kalsium-, natrium- eller ammoniumsaltene anvendes med fordel. I prinsippet er imidlertid andre syrer så som aminosyrer, hydroksykarboksylsyrer, oksosyrer eller mineralsyrer så som HCI eller H2SO4 og deres salter også egnet, idet mineralsyrer er minst foretrukket. Det er mulig å anvende enkeltsalter eller blandinger av forskjellige salter av én karboksylsyre eller flere karboksylsyrer som er blitt impregnert med én eller flere syrer under dannelse av de impregnerte salter. De impregnerte salter består med fordel av saltene av en karboksylsyre som er blitt impregnert med den samme karboksylsyre. De impregnerte salter består fortrinnsvis av saltet av en karboksylsyre som er blitt impregnert med den samme karboksylsyre. Salter av maursyre og/eller propionsyre som er blitt impregnert med maursyre og/eller propionsyre i en form som er så konsentrert som mulig, for eksempel med maursyre med 99% styrke, er spesielt foretrukket. Ci-C8 mono- and/or dicarboxylic acids and the salts of these Ci-C8 mono- and/or dicarboxylic acids are advantageously used for the preparation of the impregnated salts or for the preparation of the preservatives. Alkali metal, alkaline earth metal or ammonium salts are suitable. Acids such as formic acid, acetic acid and/or propionic acid and their ammonium, calcium, lithium, sodium, magnesium and/or potassium salts are preferably used. The calcium, sodium or ammonium salts are used with advantage. In principle, however, other acids such as amino acids, hydroxycarboxylic acids, oxo acids or mineral acids such as HCI or H 2 SO 4 and their salts are also suitable, mineral acids being the least preferred. It is possible to use single salts or mixtures of different salts of one carboxylic acid or several carboxylic acids which have been impregnated with one or more acids to form the impregnated salts. The impregnated salts advantageously consist of the salts of a carboxylic acid which has been impregnated with the same carboxylic acid. The impregnated salts preferably consist of the salt of a carboxylic acid which has been impregnated with the same carboxylic acid. Salts of formic acid and/or propionic acid that have been impregnated with formic acid and/or propionic acid in a form that is as concentrated as possible, for example with formic acid at 99% strength, are particularly preferred.
Impregnerte salter fremstilt ut fra maursyre og saltene av maursyre er meget spesielt foretrukket. Impregnated salts prepared from formic acid and the salts of formic acid are very particularly preferred.
Røntgenstrukturanalyse av de nye impregnerte salter viser et ytterligere bånd ved sammenlikning med normale karboksylsyresalter. X-ray structural analysis of the new impregnated salts shows a further band when compared with normal carboxylic acid salts.
De impregnerte salter kan, for forbedring av håndteringen, med fordel blandes med andre substanser, for eksempel med en bærer, og/eller de kan bestrøs med et strøpulver. To improve handling, the impregnated salts can advantageously be mixed with other substances, for example with a carrier, and/or they can be sprinkled with a dusting powder.
Betegnelsen impregnering angir påføring av minst én karboksylsyre, som er flytende ved 40°C eller lavere, på det (de) faste karboksylsyresalt(er) slik at den (de) flytende karboksylsyre(r) trenger inn i saltkrystallen(e). Som regel finner dette sted med svak varmeutvikling. For impregneringen påføres minst én karboksylsyre i en mengde på opp til 30 vekt%, basert på karboksylsyresaltet (-saltene), på saltet (saltene), med påføring av karboksylsyren(e) fortrinnsvis i en mengde på fra 0,5 til 30 vekt%, spesielt foretrukket med påføring av fra 15 til 25 vekt%, meget spesielt foretrukket med påføring av fra 15 til 20 vekt%, basert på saltkomponenten, for fremstilling av en fast substans som reaksjonsprodukt. Med mer enn 30 vekt% syre begynner saltkrystallene å klebes sammen; under disse betingelser er fri karboksylsyre tilstede i en viss utstrekning i tillegg til de impregnerte salter. Disse krystaller som er klebet sammen, kan skilles fra hverandre ved tilsetting av et frigjøringsmiddel, og den frie karboksylsyre kan tas opp av frigjøringsmidlet. Med mer enn 35 vekt% syre kleber produktene så sterkt sammen at det fås en pastaaktig konsistens som følge av den frie karboksylsyre. Disse produkter med pastaaktig konsistens kan bearbeides til granuler, for eksempel i et annet bearbeidingstrinn ved tilsetting av et frigjøringsmiddel og behandling for eksempel i en blander. Siden ytterligere bearbeidingstrinn og større mengder av et frigjøringsmiddel er nødvendig hvis mer enn 30 vekt% av fri syre er tilsatt, er disse utførelsesformer mindre foretrukket av økonomiske grunner. Det er imidlertid mulig i prinsippet å forbedre strømningsegenskapene hos de impregnerte salter ved tilsetting av små mengder av et frigjøringsmiddel selv med mindre enn 30 vekt% karboksylsyre. Eksempler på egnede og fordelaktige frigjøringsmidler er Sipernater, Aerosiler og/eller Tixosiler. The term impregnation indicates the application of at least one carboxylic acid, which is liquid at 40°C or lower, to the solid carboxylic acid salt(s) so that the liquid carboxylic acid(s) penetrates into the salt crystal(s). As a rule, this takes place with weak heat development. For the impregnation, at least one carboxylic acid is applied in an amount of up to 30% by weight, based on the carboxylic acid salt(s), to the salt(s), with the application of the carboxylic acid(s) preferably in an amount of from 0.5 to 30% by weight , particularly preferred with the application of from 15 to 25% by weight, very particularly preferred with the application of from 15 to 20% by weight, based on the salt component, for the production of a solid substance as reaction product. With more than 30% by weight of acid, the salt crystals start to stick together; under these conditions free carboxylic acid is present to a certain extent in addition to the impregnated salts. These crystals which are stuck together can be separated from each other by the addition of a releasing agent, and the free carboxylic acid can be taken up by the releasing agent. With more than 35% acid by weight, the products stick together so strongly that a paste-like consistency is obtained as a result of the free carboxylic acid. These products with a paste-like consistency can be processed into granules, for example in another processing step by adding a release agent and processing for example in a mixer. Since additional processing steps and larger amounts of a release agent are required if more than 30% by weight of free acid is added, these embodiments are less preferred for economic reasons. However, it is possible in principle to improve the flow properties of the impregnated salts by adding small amounts of a release agent even with less than 30% by weight of carboxylic acid. Examples of suitable and beneficial release agents are Sipernates, Aerosils and/or Tixosils.
Ved den nye fremgangsmåte for fremstilling av de impregnerte salter blir således minst ett salt av en karboksylsyre eller av en blanding av karboksylsyrer impregnert med minst én karboksylsyre som er flytende ved 40°C eller lavere, til konsentrasjonen er 30 vekt%, basert på karboksylsyresaltet (-saltene). In the new method for producing the impregnated salts, at least one salt of a carboxylic acid or of a mixture of carboxylic acids is thus impregnated with at least one carboxylic acid which is liquid at 40°C or lower, until the concentration is 30% by weight, based on the carboxylic acid salt ( -the salts).
Ved den nye fremgangsmåte for fremstilling av de impregnerte salter er det også mulig å tilsette minst ett salt av én eller flere karboksylsyrer til minst én karboksylsyre. Denne fremstillingsmåte er mindre gunstig enn tilsetting til saltet (saltene) slik at under disse betingelser, for eksempel når det anvendes en blander for fremstilling, er det nødvendig med en øket energitilførsel. In the new method for producing the impregnated salts, it is also possible to add at least one salt of one or more carboxylic acids to at least one carboxylic acid. This method of preparation is less favorable than addition to the salt(s) so that under these conditions, for example when a mixer is used for preparation, an increased energy input is required.
Den nye fremgangsmåte for fremstilling av impregnerte salter utføres med fordel ved en temperatur bestemt ved størkningspunktet for den anvendte karboksylsyre. Fremgangsmåten utføres ved fra 0 til 60°C, fortrinnsvis fra 15 til 50°C, spesielt foretrukket fra 20 til 40°C. The new method for producing impregnated salts is advantageously carried out at a temperature determined by the solidification point of the carboxylic acid used. The method is carried out at from 0 to 60°C, preferably from 15 to 50°C, particularly preferably from 20 to 40°C.
Ved en foretrukket utførelsesform har det nye salt også et beskyttende middel og/eller strøpulver på krystallenes overflate. Størrelsen av de impregnerte saltkrystaller er fortrinnsvis under 2,5 mm, spesielt foretrukket fra 10 |im til 2000 lim, meget spesielt foretrukket fra 300 nm til 1500 (j.m. In a preferred embodiment, the new salt also has a protective agent and/or dusting powder on the surface of the crystals. The size of the impregnated salt crystals is preferably below 2.5 mm, particularly preferred from 10 µm to 2000 lm, very particularly preferred from 300 nm to 1500 (j.m.
De nye konserveringsmidler er konserveringsmidler omfattende impregnerte salter som omfatter minst ett salt av én eller flere karboksylsyrer og er blitt impregnert med minst én flytende karboksylsyre. Disse impregnerte salter kan blandes i konserveringsmidlene med én eller flere bærere og/eller utformnings-hjelpemidler. Det er mulig ved den nye fremgangsmåte for fremstilling av konserveringsmidlene å agglomerere denne blanding med eller uten tilsetting av bindemiddel. Det er så mulig å påføre på disse konserveringsmidler et beskyttende middel som er løselig eller svellbart i vann ved 20°C, og/eller et findispergert strøpulver, slik at de nye konserveringsmidler får et belegg av et beskyttende middel og/eller strøpulver. The new preservatives are preservatives comprising impregnated salts which comprise at least one salt of one or more carboxylic acids and have been impregnated with at least one liquid carboxylic acid. These impregnated salts can be mixed in the preservatives with one or more carriers and/or formulation aids. It is possible with the new method for producing the preservatives to agglomerate this mixture with or without the addition of a binder. It is then possible to apply to these preservatives a protective agent which is soluble or swellable in water at 20°C, and/or a finely dispersed dusting powder, so that the new preservatives get a coating of a protective agent and/or dusting powder.
Bærere som kan anvendes, er porøse, organiske eller uorganiske bærermaterialer hvis partikkelstørrelser er fra 1 til 1000 ^im, fortrinnsvis fra 5 til 100 jirn. Carriers that can be used are porous organic or inorganic carrier materials whose particle sizes are from 1 to 1000 µm, preferably from 5 to 100 µm.
Alle kjente organiske eller uorganiske porøse bærere er, så lenge de er bestandige overfor syre, i prinsippet egnet for fremstilling av slike frittstrømmende agglomerater med redusert lukt. Eksempler er kornkli, perlitt, leirmaterialer, silikater og silikamaterialer, idet uorganiske bærere er foretrukket på grunn av at deres egenskaper lettere kan reguleres. All known organic or inorganic porous carriers are, as long as they are resistant to acid, in principle suitable for the production of such free-flowing agglomerates with reduced odour. Examples are grain bran, perlite, clay materials, silicates and silica materials, inorganic carriers being preferred because their properties can be more easily regulated.
Eksempler på andre bærere som kan anvendes, er diatoméjord, knust sand, leire, nylonpulver, uløselige metalloksider eller uløselige metallsalter, Aerosil, korundum, matt glass, granitt, kvarts eller flint, aluminiumfosfat, kaolin, bentonitt, zeolitter, kalsiumsilikat, talk, titanoksid, aktivt karbon eller benmel. Examples of other carriers that can be used are diatomaceous earth, crushed sand, clay, nylon powder, insoluble metal oxides or insoluble metal salts, Aerosil, corundum, frosted glass, granite, quartz or flint, aluminum phosphate, kaolin, bentonite, zeolites, calcium silicate, talc, titanium oxide , activated carbon or bone meal.
Bærere som fortrinnsvis anvendes, er kornkli, silikater, perlitt eller silkamaterialer i mengder på fra 10 til 70%, fortrinnsvis fra 20 til 40%, basert på vekten av det impregnerte salt. Carriers which are preferably used are grain bran, silicates, perlite or silica materials in amounts of from 10 to 70%, preferably from 20 to 40%, based on the weight of the impregnated salt.
Egnede bindemidler ved den nye fremgangsmåte er vann og/eller syntetiske eller naturlige polymerer, for eksempel albumin, kasein, soyaprotein, stivelse, syntetiske cellulosederivater så som karboksymetylcellulose, metylcellulose, hydroksymetyl-, hydroksyetyl- og/eller -propylcellulose, polyetylenglykol, polyvinylalkohol, polyvinylpyrrolidon, gelatin, karagenan, kitosan, dekstrin, alginater, agar-agar, gummi arabicum, trangantgummi eller guargummi, eller blandinger av disse. Suitable binders in the new method are water and/or synthetic or natural polymers, for example albumin, casein, soy protein, starch, synthetic cellulose derivatives such as carboxymethyl cellulose, methyl cellulose, hydroxymethyl-, hydroxyethyl- and/or -propyl cellulose, polyethylene glycol, polyvinyl alcohol, polyvinyl pyrrolidone , gelatin, carrageenan, chitosan, dextrin, alginates, agar-agar, gum arabic, trangant gum or guar gum, or mixtures thereof.
Beskyttelsesmidler som kan anvendes, er vannløselige polymerer så som syntetiske eller naturlige polymerer, for eksempel gelatin, karagenan, alginater eller polyvinylpyrrolidon, organiske syrer og deres salter eller lavtsmeltende uorganiske salter. Protective agents that can be used are water-soluble polymers such as synthetic or natural polymers, for example gelatin, carrageenan, alginates or polyvinylpyrrolidone, organic acids and their salts or low-melting inorganic salts.
Beskyttelsesmidler som fortrinnsvis anvendes, er polyetylenglykoler, polyvinylpyrrolidoner eller organiske C3-Cu-syrer, fortrinnsvis C3-C6-syrer og deres salter, spesielt citronsyre, fumarsyre, ravsyre, adipinsyre, benzosyre og deres salter, eller aminosyrer og deres salter. Preservatives which are preferably used are polyethylene glycols, polyvinylpyrrolidones or organic C3-Cu acids, preferably C3-C6 acids and their salts, especially citric acid, fumaric acid, succinic acid, adipic acid, benzoic acid and their salts, or amino acids and their salts.
Ved en foretrukket utførelsesform av den nye fremgangsmåte for fremstilling av konserveringsmidlene innføres karboksylsyresaltet i en blandeinnretning, impregnert med den organisk syre, en bærer iblandes hvor hensiktsmessig, og deretter utføres agglomerering og belegging med beskyttelsesmidlet, i nærvær eller fravær av et bindemiddel. In a preferred embodiment of the new method for producing the preservatives, the carboxylic acid salt is introduced into a mixing device, impregnated with the organic acid, a carrier is mixed where appropriate, and then agglomeration and coating with the protective agent is carried out, in the presence or absence of a binder.
De impregnerte salter og/eller bærerpartikler blandes med beskyttelsesmidlet, idet sistnevnte vanligvis består av en sterkt konsentrert løsning eller smelte av substanser som er løselige eller svellbare i vann og størkner ved romtemperatur (23°C). Dette beskyttelsesmiddel påføres fortrinnsvis i oppvarmet tilstand på de impregnerte salt- og/eller bærerpartikler og blandes med sistnevnte. I løpet av dette størkner beskyttelsesmidlet på overflaten av de impregnerte salter og/eller bærerpartikler. Egnede driftsparametere for blandeinnretningen resulterer i agglomerering av forskjellige partikler til større granuler. The impregnated salts and/or carrier particles are mixed with the protective agent, the latter usually consisting of a highly concentrated solution or melt of substances that are soluble or swellable in water and solidify at room temperature (23°C). This protective agent is preferably applied in a heated state to the impregnated salt and/or carrier particles and mixed with the latter. During this, the protective agent solidifies on the surface of the impregnated salts and/or carrier particles. Suitable operating parameters for the mixing device result in agglomeration of different particles into larger granules.
Størrelsen av granulene kan justeres ved hjelp av The size of the granules can be adjusted using
bearbeidelsesparametere, for eksempel under blandingen eller under virvelsjikt-granuleringen, og ved mengden og typen bindemiddel eller ellers ved påfølgende sikting eller maling. Granulene har fortrinnsvis en gjennomsnittlig diameter på under 3 mm, spesielt 0,3-1,3 mm. Det er mulig, hvor hensiktsmessig, at residualvann kan være tilstede i beskyttelsesmidlet som anvendes for belegging og agglomerering. Etter agglomereringsprosessen eller direkte etter fremstillingen av de impregnerte salter kan restvann bindes ved hjelp av en bestrøingsprosess med et tørt og findispergert strøpulver. Det er mulig ved denne bestrøingsprosess også å forhindre at agglomeratene eller de impregnerte salter kleber sammen senere, og dessuten for eksempel å påføre saltet av den anvendte organisk syre (f.eks. natrium- eller kalsiumformiat eller -propionat) på agglomeratet eller saltene. Det er videre mulig, hvor hensiktsmessig, å tilsette et luktmiddel eller smaksstoff, f.eks. vanillin, tecu-smaksstoff, citral eller fructin, som gjør det mulig å oppnå en ytterligere luktmaskerende virkning som for eksempel gjør det tiltrekkende for dyr å fortære maten. processing parameters, for example during mixing or during fluidized bed granulation, and by the amount and type of binder or otherwise by subsequent screening or grinding. The granules preferably have an average diameter of less than 3 mm, especially 0.3-1.3 mm. It is possible, where appropriate, that residual water may be present in the protective agent used for coating and agglomeration. After the agglomeration process or directly after the production of the impregnated salts, residual water can be bound by means of a sprinkling process with a dry and finely dispersed sprinkling powder. It is also possible with this sprinkling process to prevent the agglomerates or the impregnated salts from sticking together later, and furthermore, for example, to apply the salt of the organic acid used (e.g. sodium or calcium formate or propionate) to the agglomerate or the salts. It is also possible, where appropriate, to add an odorant or flavouring, e.g. vanillin, tecu flavouring, citral or fructin, which makes it possible to achieve a further odor-masking effect which, for example, makes it attractive for animals to consume the food.
Beskyttelsesmidler som fortrinnsvis anvendes, så som bindemiddelvæsker, er substanser som er løselige eller svellbare i vann og som størkner ved romtemperatur. Dette gjør det mulig å unngå et påfølgende tørketrinn hvor, bortsett fra et løsningsmiddel eller det ytterligere vann, en del av den organisk syre også vil fordampe. Protective agents which are preferably used, such as binder liquids, are substances which are soluble or swellable in water and which solidify at room temperature. This makes it possible to avoid a subsequent drying step where, apart from a solvent or the additional water, part of the organic acid will also evaporate.
Spesielt egnede beskyttelsesmidler for agglomereringsprosessen og beleggingen er slike som har en mykningstemperatur på over 30°C, fortrinnsvis over 60°C, for unngåelse av deformasjon av agglomeratene hvis lagringstemperaturen er forholdsvis høy. Beskyttelsesmidlene som fortrinnsvis anvendes, motvirker dessuten ikke den pH-nedsettende virkning av den adsorberte organisk syre, eller til og med, hvor hensiktsmessig, understøtter eller forøker de denne. Particularly suitable protective agents for the agglomeration process and the coating are those which have a softening temperature of over 30°C, preferably over 60°C, to avoid deformation of the agglomerates if the storage temperature is relatively high. The protective agents which are preferably used also do not counteract the pH-lowering effect of the adsorbed organic acid, or even, where appropriate, support or increase this.
Eksempler på egnede beskyttelsesmidler er sterkt konsentrerte varme sukkerløsninger eller alkalimetall-/jordalkalimetallformiat/-acetat/-propionat-løsninger. Rest-vanninnholdet i dem kan tas opp ved det endelige bestrøingstrinn. Lavtsmeltende polyetylenglykoler så som PEG 4000, smelter av citronsyre, av adipinsyre, fumarsyre eller benzosyre eller deres salter, sterkt konsentrerte løsninger av aminosyrer eller blandinger av disse syrer er egnet og foretrukket som bindemiddelvæsker. Mengden av anvendt bindemiddelvæske er fra 0,5 til 80%, fortrinnsvis fra 10 til 25%, men spesielt foretrukket fra 5 til 15%, basert på vekten av granulene. Examples of suitable protective agents are highly concentrated hot sugar solutions or alkali metal/alkaline earth metal formate/acetate/propionate solutions. The residual water content in them can be taken up in the final sprinkling step. Low-melting polyethylene glycols such as PEG 4000, melts of citric acid, of adipic acid, fumaric acid or benzoic acid or their salts, highly concentrated solutions of amino acids or mixtures of these acids are suitable and preferred as binder liquids. The amount of binder liquid used is from 0.5 to 80%, preferably from 10 to 25%, but particularly preferably from 5 to 15%, based on the weight of the granules.
Egnede strøpulvere er, i tillegg til selve de porøse bærermaterialer, fin-dispergerte, malte organiske syrer eller deres salter, f.eks. natriumformiat, og uorganiske salter, Sipernater, Tixosiler eller Aerosiler. Mengden av tilsatte strøpulvere er 10 vekt%, fortrinnsvis fra 0,1 til 5 vekt%. Suitable bedding powders are, in addition to the porous carrier materials themselves, finely dispersed, ground organic acids or their salts, e.g. sodium formate, and inorganic salts, Sipernates, Thixosils or Aerosils. The amount of added bedding powder is 10% by weight, preferably from 0.1 to 5% by weight.
Vanligvis innføres minst ett salt av én eller flere organiske syrer i en blandeinnretning, f.eks. en blandeinnretning av typen Eirich, og impregneres med minst én organisk syre med små mengder tilført energi. Fremgangsmåten kan imidlertid også være slik at væsken innføres i blandeinnretningen, og saltene av karboksylsyrene måles inn. Høyere mengder tilført energi er nødvendig i sistnevnte tilfelle. Usually at least one salt of one or more organic acids is introduced into a mixing device, e.g. a mixing device of the Eirich type, and is impregnated with at least one organic acid with small amounts of added energy. However, the procedure can also be such that the liquid is introduced into the mixing device, and the salts of the carboxylic acids are measured in. Higher amounts of added energy are required in the latter case.
Man må passe på å sikre jevn impregnering og å unngå for høy lokal fukting, som fører til klumpdannelse. Etter impregneringen inneholder blandeinnretningen et frittstrømmende karboksylsyresalt i form av et krystallinsk faststoff. Viskositeten av bindemiddelvæsken som deretter innmåles hvor hensiktsmessig, bør justeres ved passende valg av temperatur, slik at den blir under 1000 mPa, fortrinnsvis < 100 mPa, for oppnåelse av en fin dråpestørrelsesfordeling ved sprøytingen. Ved denne foretrukne utførelsesform vil dråpene av bindemiddelvæske, på grunn av temperaturforskjellen mellom den varme bindemiddelvæske og det kaldere impregnerte salt, i begynnelsen størkne hurtig. Etter hvert som agglomereringsprosessen skrider fram, øker temperaturen i sjiktet på grunn av innføringen av den mekaniske og termiske energi, med fra 10 til 30°C, avhengig av beskaffenheten av bindemiddelvæsken. Ytterligere dråper av bindemiddelvæske blir festet til de tidligere dannede agglomerater, og noen av dem løper sammen. Tilført energimengde øker under agglomereringen. Care must be taken to ensure uniform impregnation and to avoid excessive local wetting, which leads to lump formation. After the impregnation, the mixing device contains a free-flowing carboxylic acid salt in the form of a crystalline solid. The viscosity of the binder liquid, which is then measured where appropriate, should be adjusted by appropriate selection of temperature, so that it is below 1000 mPa, preferably < 100 mPa, to achieve a fine droplet size distribution during spraying. In this preferred embodiment, the drops of binder liquid will, due to the temperature difference between the hot binder liquid and the colder impregnated salt, initially solidify quickly. As the agglomeration process progresses, the temperature in the layer increases due to the introduction of the mechanical and thermal energy, by 10 to 30°C, depending on the nature of the binder liquid. Additional drops of binder liquid are attached to the previously formed agglomerates, and some of them run together. Added amount of energy increases during agglomeration.
Det er mulig til slutt å tilsette et odoriseringsmiddel sammen med strøpulveret, som beskrevet ovenfor. Et stort antall duftmidler og smaksstoffer som kan velges avhengig av den påfølgende anvendelse av agglomeratet, er i prinsippet egnet til dette. Innholdet i disse duftmidler kan være < 1%, fortrinnsvis fra 0,05 til 0,5%, basert på vekten av granulene. Agglomeratene dannet på denne måte inneholder lite støv og har redusert lukt, og deres innhold av organisk syre er lett løselig i vann. Finally, it is possible to add an odorising agent together with the bedding powder, as described above. A large number of fragrances and flavors which can be selected depending on the subsequent use of the agglomerate are in principle suitable for this. The content of these fragrances can be < 1%, preferably from 0.05 to 0.5%, based on the weight of the granules. The agglomerates formed in this way contain little dust and have reduced odour, and their organic acid content is easily soluble in water.
De nye impregnerte salter og/eller konserveringsmidler er egnet for syrebehandling og/eller konservering av menneske- og dyreføde, for anvendelse i silofor og for lærbehandling. Menneske- og dyreføde er spesielt gress, landbruks-produkter og/eller kompoundert dyreføde, samt materialene som anvendes til fremstilling av dem, så som høy, bygg, hvete, havre, rug, mais, ris, soyabønner, sukkerrør-rester, sukkerrør, raps, jordnøtter, solsikkefrø, bokhvetehakkels, silofor, våtkorn («wet grains»), belgfrukter eller kornavlinger, men også melke-erstat-ningsprodukter, flytende, sammensatte og mineral-fér, fiske-silofor eller fisk, kjøtt eller benmel. The new impregnated salts and/or preservatives are suitable for acid treatment and/or preservation of human and animal food, for use in silage and for leather treatment. Human and animal food is especially grass, agricultural products and/or compounded animal food, as well as the materials used in their production, such as hay, barley, wheat, oats, rye, maize, rice, soybeans, sugar cane residues, sugar cane, rapeseed, peanuts, sunflower seeds, buckwheat groats, silo forage, wet grains ("wet grains"), legumes or cereal crops, but also milk substitutes, liquid, compound and mineral fertilizers, fish silo forage or fish, meat or bone meal.
De nye konserveringsmidler kan også inneholde andre additiver så som mineraler, vitaminer, antibiotika eller proteinadditiver. Konserveringsmidlene kan spesielt inneholde andre additiver med fungicide eller baktericide egenskaper, så som formalin, maursyre, eddiksyre, propionsyre, benzosyre, sorbinsyre eller bisulfitter. The new preservatives may also contain other additives such as minerals, vitamins, antibiotics or protein additives. The preservatives may in particular contain other additives with fungicidal or bactericidal properties, such as formalin, formic acid, acetic acid, propionic acid, benzoic acid, sorbic acid or bisulphites.
De nye impregnerte salter og/eller konserveringsmidler tilsettes med fordel til materialet som skal konserveres, i hvert tilfelle i en mengde på fra 0,1 til 25 kg, fortrinnsvis fra 0,5 til 20 kg, spesielt foretrukket fra 5 til 15 kg, pr. tonn materiale som skal konserveres. The new impregnated salts and/or preservatives are advantageously added to the material to be preserved, in each case in an amount of from 0.1 to 25 kg, preferably from 0.5 to 20 kg, particularly preferably from 5 to 15 kg, per . tonnes of material to be conserved.
Eksempler Examples
(Renhet av den anvendte maursyre og propionsyre = 99%) (Purity of the formic acid and propionic acid used = 99%)
A. Maursyre A. Formic acid
Eksempel 1 Example 1
100 g natriumformiat ble innført i en husholdningsblander (Braun), og 15 vekt% maursyre ble tilsatt. Temperaturen steg fra 22 til 40°C ved opptak av syren. Det resulterende produkt (= impregnert salt) var frittstrømmende og luktfritt. 100 g of sodium formate was introduced into a household mixer (Braun), and 15% by weight of formic acid was added. The temperature rose from 22 to 40°C when the acid was absorbed. The resulting product (= impregnated salt) was free-flowing and odorless.
Eksempel 2 Example 2
100 g kalsiumformiat ble innført i en husholdningsblander, og 15 vekt% maursyre ble tilsatt. Det resulterende produkt hadde en litt stikkende lukt av maursyre og oppviste sammenhengings-oppførsel, dvs. at det resulterende impregnerte salt var litt fuktig og ikke frittstrømmende. 100 g of calcium formate was introduced into a household mixer, and 15% by weight of formic acid was added. The resulting product had a slightly pungent odor of formic acid and exhibited cohesive behavior, ie the resulting impregnated salt was slightly moist and not free-flowing.
Eksempel 3 Example 3
100 g natriumformiat ble innført i en husholdningsblander, og 10 vekt% maursyre ble tilsatt. Temperaturen steg fra 23 til 45°C ved opptak av syren. Det impregnerte salt hadde en litt stikkende lukt og viste en liten tendens til å bli granuløst. 100 g of sodium formate was introduced into a household blender, and 10% by weight of formic acid was added. The temperature rose from 23 to 45°C when the acid was absorbed. The impregnated salt had a slightly pungent odor and showed a slight tendency to become granular.
B. Propionsyre B. Propionic acid
Eksempel 4 Example 4
100 g fumarsyre ble innført i en husholdningsblander, og 15 vekt% propionsyre ble tilsatt. Produktet var meget sammenhengende og hadde en intens lukt. 100 g of fumaric acid was introduced into a household mixer, and 15% by weight of propionic acid was added. The product was very cohesive and had an intense smell.
Eksempel 5 Example 5
100 g natriumformiat ble innført i en husholdningsblander, og 15 vekt% propionsyre ble tilsatt, som i de foregående eksempler. Produktet var sterkt sammenhengende og hadde en intens lukt. 100 g of sodium formate was introduced into a household mixer, and 15% by weight of propionic acid was added, as in the previous examples. The product was strongly cohesive and had an intense smell.
Eksempel 6 Example 6
100 g kalsumformiat ble innført i en husholdningsblander, og 15 vekt% propionsyre ble tilsatt. Temperaturen steg litt mens syren ble opptatt. Produktet hadde en intens lukt og oppviste sterk sammenhengingsoppførsel. 100 g of calcium formate was introduced into a household mixer, and 15% by weight of propionic acid was added. The temperature rose slightly while the acid was absorbed. The product had an intense odor and exhibited strong cohesive behavior.
Eksempel 7 Example 7
100 g kalsumpropionat ble innført i en husholdningsblander, og 15 vekt% propionsyre ble tilsatt. Temperaturen steg fra 23 til 29°C ved opptak av syren. Produktet var frittstrømmende og hadde en intens lukt. 100 g of calcium propionate was introduced into a household mixer, and 15% by weight of propionic acid was added. The temperature rose from 23 to 29°C when the acid was absorbed. The product was free-flowing and had an intense smell.
C. Fremstilling av konserveringsmidler C. Manufacture of preservatives
Eksempel 8 Example 8
1000 g natriumformiat ble innført i en Eirich-blander (R02) og impregnert med 15 vekt% maursyre. 200 g natriumformiatsmelte ved 80°C ble sprøytet som bindemiddel fra en oppvarmet lagringsbeholder gjennom en tokomponent-dyse, på 1000 g av denne blanding i blandekammeret. De resulterende agglomerater ble bestrødd med 44 g Sipernat® (=sterkt dispergert silika levert av Degussa). Det resulterende produkt var frittstrømmende og luktfritt. 1000 g of sodium formate was introduced into an Eirich mixer (R02) and impregnated with 15% by weight of formic acid. 200 g of sodium formate melt at 80°C was sprayed as binder from a heated storage container through a two-component nozzle, onto 1000 g of this mixture in the mixing chamber. The resulting agglomerates were sprinkled with 44 g of Sipernat® (=highly dispersed silica supplied by Degussa). The resulting product was free-flowing and odorless.
Eksempel 9 Example 9
1000 g natriumformiat ble innført i en Eirich-blander og impregnert med 15 vekt% maursyre. For agglomerering og belegging ble 180 g av en konsentert glukoseløsning ved 80°C sprøytet som bindemiddel fra en opp-varmet lagringsbeholder gjennom en tokomponent-dyse inn i blandekammeret. De resulterende agglomerater ble bestrødd med 45 g Sipernat® og 12 g citral. Syreinnholdet var da 59,5%. De resulterende agglomerater var frittstrømmende. 1000 g of sodium formate was introduced into an Eirich mixer and impregnated with 15% by weight of formic acid. For agglomeration and coating, 180 g of a concentrated glucose solution at 80°C was sprayed as binder from a heated storage container through a two-component nozzle into the mixing chamber. The resulting agglomerates were sprinkled with 45 g of Sipernat® and 12 g of citral. The acid content was then 59.5%. The resulting agglomerates were free-flowing.
Eksempel 10 Example 10
Som i eksempel 9, ble 500 g natriumformiat innført i en Eirich-blander og impregnert med 15 vekt% maursyre. Deretter ble det tilsatt 500 g perlitt. 260 g citronsyresmelte ved 170°C ble sprøytet inn som bindemiddel fra en oppvarmet lagringsbeholder gjennom en tokomponent-dyse inn i blandekammeret. De resulterende agglomerater ble bestrødd med 44 g Sipernat® og 8 g vanillin. Det totale syreinnhold var 29,7%. De resulterende konserveringsmidler var frittstrømmende og luktfrie. De impregnerte salter beskrevet i eksempler 1 -7 kan også omdannes som i eksempler 8-10 til frittstrømmende konserveringsmidler med redusert lukt eller ingen lukt. As in Example 9, 500 g of sodium formate was introduced into an Eirich mixer and impregnated with 15% by weight formic acid. Then 500 g of perlite was added. 260 g of citric acid melt at 170°C was injected as binder from a heated storage container through a two-component nozzle into the mixing chamber. The resulting agglomerates were sprinkled with 44 g of Sipernat® and 8 g of vanillin. The total acid content was 29.7%. The resulting preservatives were free-flowing and odorless. The impregnated salts described in examples 1-7 can also be converted as in examples 8-10 into free-flowing preservatives with reduced odor or no odor.
Følgende eksempler 11-14 viser lagringsstabilitetstester for et impregnert salt (natriumformiat impregnert med 20 vekt% maursyre) behand-let med forskjellige beskyttelsesmidler og/eller strøpulvere (se tabell 1). Delmengder av de impregnerte salter ble anbrakt i en trommelblander og blandet i ytterligere 10 minutter under tilsetting av additivene (se tabell 1). Produktene ble deretter innført i en stålbeholder (diameter ca. 40 mm) opp til 15-20 mm under kanten av beholderen, lagret i en tørkeovn ved 35°C under belastning (simulert med et metallstempel), idet belastningen svarte til simulert lagring under normale lagringsbetingelser, og testet i de angitte tidsrom. På grunn av testbeholderens lille diameter og lagringen under trykk, er det, for påvisning av om hvorvidt et produkt er frittstrømmende eller ikke, nødvendig å banke på beholderen. Betegnelsene anvendt til å angi resultatet av strømningstesten har følgende betydninger: forsiktig banking 1x, forsiktig banking 2x og banking 1x = produktet er frittstrømmende banking 3x = produktet viser sammenklebning, men er hovedsakelig frittstrømmende banking 4x, banking 5x og banking >5x = produktet er sammenklebet og praktisk talt ikke lenger frittstrømmende. The following examples 11-14 show storage stability tests for an impregnated salt (sodium formate impregnated with 20% by weight formic acid) treated with various protective agents and/or bedding powders (see table 1). Portions of the impregnated salts were placed in a drum mixer and mixed for a further 10 minutes while adding the additives (see Table 1). The products were then introduced into a steel container (diameter approx. 40 mm) up to 15-20 mm below the edge of the container, stored in a drying oven at 35°C under load (simulated with a metal stamp), the load corresponding to simulated storage under normal storage conditions, and tested for the specified periods of time. Due to the small diameter of the test container and the storage under pressure, in order to detect whether a product is free-flowing or not, it is necessary to tap the container. The terms used to indicate the result of the flow test have the following meanings: gentle tapping 1x, gentle tapping 2x and tapping 1x = the product is free-flowing tapping 3x = the product shows sticking but is mainly free-flowing tapping 4x, tapping 5x and tapping >5x = the product is stuck together and practically no longer free-flowing.
D. Surgjøring av matvarer D. Acidification of foodstuffs
Eksempel 15 Example 15
En utgangs-matvare av smågris ble behandlet med 10 kg/t eller 20 kg/t av et impregnert salt (natriumformiat/15 vekt% maursyre). Matvarens pH falt fra 6,4 til henholdsvis 5,5 eller 5,1. A starting feed of piglets was treated with 10 kg/h or 20 kg/h of an impregnated salt (sodium formate/15% by weight formic acid). The food's pH dropped from 6.4 to 5.5 or 5.1 respectively.
Claims (16)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19739319A DE19739319A1 (en) | 1997-09-08 | 1997-09-08 | Soaked salts, a process for their preparation, their use |
| PCT/EP1998/005469 WO1999012432A1 (en) | 1997-09-08 | 1998-08-28 | Impregnated salts, a method for producing said salts, and the use of the same |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| NO20001174D0 NO20001174D0 (en) | 2000-03-07 |
| NO20001174L NO20001174L (en) | 2000-03-07 |
| NO326063B1 true NO326063B1 (en) | 2008-09-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO20001174A NO326063B1 (en) | 1997-09-08 | 2000-03-07 | Impregnated salts, preservatives and processes for the preparation and use of said salts and preservatives. |
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| EP (1) | EP1014807B1 (en) |
| AT (1) | ATE207705T1 (en) |
| CZ (1) | CZ292287B6 (en) |
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| ES (1) | ES2167100T3 (en) |
| HU (1) | HUP0004043A3 (en) |
| NO (1) | NO326063B1 (en) |
| PL (2) | PL195154B1 (en) |
| WO (1) | WO1999012432A1 (en) |
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| DE10050246C1 (en) * | 2000-10-11 | 2002-06-20 | Nutrinova Gmbh | Calcium double salts, process for their preparation and their use for preservation |
| DE10055390A1 (en) | 2000-11-09 | 2002-05-29 | Nutrinova Gmbh | Use of an acid preparation as a feed additive in livestock rearing |
| DE10105308A1 (en) * | 2001-02-02 | 2002-08-14 | Nutrinova Gmbh | Sorbic acid as a growth-stabilizing additive to feed for livestock rearing |
| DE10228027B4 (en) * | 2002-06-24 | 2006-04-13 | Bos Gmbh & Co. Kg | Window blind with rattle-free guide |
| DE10231891A1 (en) * | 2002-07-12 | 2004-01-22 | Basf Ag | Coated formulation containing sodium, potassium, cesium and/or ammonium diformate is used in premix for animal feed or additive, as performance and/or growth promoter; acidifier; preservative or silage or in fertilizer |
| LU91250B1 (en) * | 2006-06-14 | 2007-12-17 | Regis Brouet | The informational bonus for food, non-food and fuel products |
| WO2008055990A1 (en) * | 2006-11-10 | 2008-05-15 | Basf Se | Sodium-containing methanoic acid solutions |
| DE102016203477A1 (en) * | 2016-03-03 | 2017-09-07 | Addcon Europe Gmbh | Preparation and use of alkali metal diformates with medium-chain fatty acid derivatives |
| LU500270B1 (en) | 2021-06-10 | 2022-12-12 | Lucas Brendler | Carboxylic Acid Loaded Salt Carrier and the Method for Producing thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH613607A5 (en) * | 1975-06-11 | 1979-10-15 | Lonza Ag | Ensiling agent and process for preparation thereof |
| US4199606A (en) * | 1977-09-22 | 1980-04-22 | Bland Bobby | Propionic acid on a carrier material as a preservative |
| GB8525061D0 (en) * | 1985-10-10 | 1985-11-13 | Bp Chem Int Ltd | Antimicrobial additives |
| DE69305714T2 (en) * | 1992-09-30 | 1997-03-20 | Bp Chem Int Ltd | Removable carboxylic acids |
| GB9301532D0 (en) * | 1993-01-27 | 1993-03-17 | Bp Chem Int Ltd | Releasably bound hydroxycarboxylic acids |
| US5547987A (en) * | 1993-07-19 | 1996-08-20 | Anitox Corporation | Pathogen inhibitor for animal feeds |
| NO300912B1 (en) * | 1995-05-12 | 1997-08-18 | Norsk Hydro As | Animal feed additives and feed containing such additives |
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1997
- 1997-09-08 DE DE19739319A patent/DE19739319A1/en not_active Withdrawn
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1998
- 1998-08-28 ES ES98949979T patent/ES2167100T3/en not_active Expired - Lifetime
- 1998-08-28 PL PL98378471A patent/PL195154B1/en not_active IP Right Cessation
- 1998-08-28 PL PL336591A patent/PL191579B1/en not_active IP Right Cessation
- 1998-08-28 HU HU0004043A patent/HUP0004043A3/en unknown
- 1998-08-28 WO PCT/EP1998/005469 patent/WO1999012432A1/en active IP Right Grant
- 1998-08-28 CZ CZ2000826A patent/CZ292287B6/en not_active IP Right Cessation
- 1998-08-28 EP EP98949979A patent/EP1014807B1/en not_active Expired - Lifetime
- 1998-08-28 DE DE59801993T patent/DE59801993D1/en not_active Expired - Lifetime
- 1998-08-28 AT AT98949979T patent/ATE207705T1/en not_active IP Right Cessation
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2000
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| DE59801993D1 (en) | 2001-12-06 |
| WO1999012432A1 (en) | 1999-03-18 |
| PL191579B1 (en) | 2006-06-30 |
| DE19739319A1 (en) | 1999-03-11 |
| NO20001174D0 (en) | 2000-03-07 |
| CZ292287B6 (en) | 2003-08-13 |
| EP1014807A1 (en) | 2000-07-05 |
| PL336591A1 (en) | 2000-07-03 |
| EP1014807B1 (en) | 2001-10-31 |
| CZ2000826A3 (en) | 2000-06-14 |
| HUP0004043A3 (en) | 2003-02-28 |
| NO20001174L (en) | 2000-03-07 |
| ATE207705T1 (en) | 2001-11-15 |
| HUP0004043A2 (en) | 2001-03-28 |
| ES2167100T3 (en) | 2002-05-01 |
| PL195154B1 (en) | 2007-08-31 |
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