• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A new animal feed additive which is active as a preservative is shown. Said animal feed additive comprises 30-80% by weight of propionic acid, 20-70% by weight of glyceryl propionates and optionally 1-10% by weight of an alkali metal salt. The product is non-corrosive and effective as, for example, mold inhibitor.
    公开号:SE535688C2
    申请号:SE1100413
    申请日:2011-05-24
    公开日:2012-11-06
    发明作者:Johan Rehnstroem
    申请人:Perstorp Ab；
    IPC主号:
    专利说明:

    The present invention provides, in a further aspect, a process for the preparation of said animal feed additive wherein a mixture comprising 70-90% by weight of propionic acid and 10-30% by weight of glycerol is reacted at a temperature of 50-70 ° C until a reaction equilibrium is reached.
    Said reaction may optionally be carried out in the presence of an acid catalyst, such as sulfuric acid, in an amount of, for example, 0.05-0.5% by weight, calculated on the total amount of reactants. Said process may also optionally comprise diluting the resulting reaction mixture with additional propionic acid to obtain a composition comprising propionic acid and glyceryl propionates in the aforementioned ratios and / or mixing said alkali metal salt. The acid catalyst used can be suitably neutralized by adding a stoichiometric amount of an alkaline compound, such as ammonia and / or an alkali metal hydroxide. The reaction mixture or composition thus obtained can be advantageously used as a mold-inhibiting additive in animal feed.
    The animal feed additive according to the dosage forms of the present invention can of course be diluted to a suitable concentration of active components by the addition of, for example, water, formic acid, propionic acid, butyric acid and / or other mold inhibiting compounds. The feed additive can of course also be supplemented by the addition of other feed additives, preservatives, nutrients and pharmaceutical preparations, such as compatible antibiotics and vitamins.
    The following preferred embodiments are to be considered as illustrative only and not in any way limiting of the remaining description. In the following, Examples 1-3 relate to the preparation of animal feed additives according to embodiments of the present invention and Examples 4-7 to the evaluation of products obtained in comparison with commercially available propionic acid-based feed additives. Evaluation results are given in attached tables 1-3.
    Example 1 70 kg of propionic acid, 30 kg of glycerol and 200 g of sulfuric acid as catalyst were mixed and heated to 70 ° C in a reaction vessel. A reaction equilibrium was obtained after 8 hours and the resulting reaction mixture was cooled to room temperature and a stoichiometric amount of ammonia was added to said sulfuric acid.
    The resulting reaction mixture showed the following composition: Propionic acid 61.3% by weight Glyceryl monopropionate 6.2% by weight Glyceryl dipropionate 15.7% by weight Glyceryl tripropionate 7.3% by weight Glycerol 0.5% by weight 535 688 Example 2 Example 2 was repeated with the difference that 2% by weight of sodium formate is finally added to the resulting reaction mixture.
    Example 3 Example 2 was repeated with the difference that 3% by weight of sodium formate was finally added to the resulting reaction mixture.
    Example 4 The product obtained in Example 1 was spayed, in application rates corresponding to 35, 46 and 59% of recommended application rates * for aerobic preservation with propionic acid of moist grain, on granules with a moisture content of 34% and the sprayed grain samples were stored in glass jars under normal storage conditions. grain preservation was simulated.
    The product of Example 1 was compared with pure propionic acid and Lupro-Grain® (BASF, Germany). The treated samples were stored in glass jars simulating normal storage conditions during grain preservation at 18-22 ° C. Mold growth was observed and noted weekly. The tests were performed by the Swedish University of Agricultural Sciences and were graded according to the following grading system 0 = no visible mold growth 1 = 1-3 visible small mold colonies 2 = visible mold growth on <10% of the surface 3 = visible mold growth on 10-30% of the surface 4 = visible mold growth on 30-50% of the surface 5 = visible mold growth of> 50% of the surface and is reported in table 1 as mean values for 15 samples / product.
    * Recommended application rate was calculated as follows: Recommended application rate (ml / kg moist grain) = (moisture content x 0.375) - 1,125 Ekström, N., Thyselius, L., Johansson, S. & Thomke, S., 1973, Acid treatment of cereals .
    Dosage, feed value, economy (Acid Treatment of Grain. Application, Nutrative Quality and Economy), JTI message # 352, JTI (www.jti.se), Uppsala, Sweden (in Swedish with English summary). Example 5 30 g of the product obtained in Example 2 were weighed into an open 100 ml beaker and stored for 65 days at room temperature. The remaining samples were calculated as% by weight by interval weighing. A comparative sample with Lupro-Grain® was tested under the same conditions.
    The result is reported in Table 2.
    Example 6 Corrosion on steel panels was evaluated for products according to Examples 1, 2 and 3.
    Corrosion testing was performed according to UN Test Methods Part III Section 37. The results, expressions such as weight loss of the steel panels in% by weight and depth of penetration in μm, are reported in Table 3.
    Example 7 Skin initiation tests were performed according to OECD Guideline No 404, "Acute Dennal Irritation / Corrosion", April 2002 and were evaluated according to Commission Directive 2001/59 / EC.
    The test result using product obtained in Example I showed that said product was not skin irritating. 535 G88 5 Table 1 Appl. amount 35% Appl. amount 46% Appl. amount 59% PA LG Ex. 1 PA LG Ex. l PA LG Ex. 1 28 days 1.3 3.8 1.8 0 0 0 0 0 0 56 days 4.0 5.0 4.5 1.0 1.8 0.3 0 0 O 84 days 5.0 5.0 5 .0 2.5 2.8 0.3 0 0 0 112 days 5.0 5.0 5.0 4.3 4.3 0.3 0 O 0 PA = Propionic acid LG = Lupro-Grain ”Ex. l = Product according to Example 1 Table 2 Example 2, residual weight% Lupro-Grain®, residual weight% 1 day 98.3 96.7 2 days 92.5 88.2 5 days 82.4 70.9 9 days 73.9 53.3 14 days 68.1 35.5 27 days 66 16.4 37 days 63.9 4.9 65 days 62.2 0.1 Table 3 weight loss, weight% Penetration depth, um Example 1 - Panel 1.76 Example 1 - Panel 2 2.50 250 Example 1 - Panel 3 3.84 Example 2 - Panel 1 1.64 Example 2 - Panel 2 1.64 80 Example 2 - Panel 3 0.64 Example 3 - Panel 1.49 Example 3 - Panel 2 1.45 <50 Example 3 - Panel 3 0.37
    权利要求:
    Claims (18)
    [1] 1. 0. An animal feed additive effective as preservative c h a r a c t e ri s e d i n, that it comprises 30-80% by Weight of propionic acid, 20-70%by Weight of glyceryl propionates and less than 4% by Weight of glycerol, balance to100% by Weight being Water.
    [2] 2. An animal feed additive according to Claim lc h a r a c t e ri s e d i n, that it comprises 40-60%, by weight ofpropionic acid, 30-50%by weight of glyceryl propionates.
    [3] 3. An animal feed additive according to Claim lc h a r a c t e ri s e d i n, that it comprises 35-65%, by Weight ofpropionic acid, 35-55%by weight of glyceryl propionates.
    [4] 4. An animal feed additive according to any of the Claims l-3c h a r a c t e ri s e d i n, that it comprises less than 2% by weight ofglycerol.
    [5] 5. An animal feed additive according to any of the Claims l-3c h a r a c t e ri s e d in, that it comprises 0.5-1%, by Weight of glycerol.
    [6] 6. An animal feed additive according to any of the Claims l-5 c h a r a c t e ri s e d i n, that said glyceryl propionates is a mixture comprising l0-30%by Weight of glyceryl monopropionate, 40-70% by Weight of glyceryl dipropionate andl0-30% by weight of glyceryl tripropionate, balance being 100% by weight.
    [7] 7. An animal feed additive according to any of the Claims 1-6c h a r a c t e r i s e d i n, that it additionally comprises at least one alkali metal salt added in an amount of 1-10% by Weight.
    [8] 8. An animal feed additive according to any of the Claims 1-6c h a r a c t e r i s e d i n, that it comprises at least one alkali metal salt added in an amount of l-5% by Weight.
    [9] 9. An animal feed additive according to Claim 7 or 8c h a r a c t e ri s e d i n, that said alkali metal salt is potassium or sodium formate.
    [10] 10. An animal feed additive according to any of the Claims 1-9c h a r a c t e r i s e d i n, that it is diluted with Water, forrnic acid, propionic acid and/orbutyric acid.
    [11] 11.
    [12] 12.
    [13] 13.
    [14] 14.
    [15] 15.
    [16] 16.
    [17] 17.
    [18] 18. A method of producing an animal feed additive according to any of the Claims 1-9 c h a r a c t e r i s e d i n, that a mixture comprising 70-90% by Weight of propionic acidand l0-30% by weight of glycerol is subjected to reaction at a temperature of 50-70°Cuntil a reaction equilibrium is obtained and that at least one alkali metal salt optionally isadded to yielded reaction mixture in an amount of l-10% by Weight. A method according to Claim 11c h a r a c t e r i s e d i n, that said reaction is performed in presence of an acidic catalyst. A method according to Claim 12c h a r a c t e ri s e d i n, that said acidic catalyst is sulphuric acid. A method according to Claim 12 or 13c h a r a c t e r i s e d i n, that said acidic catalyst is present in an amount of 0.05-0.5 %by weight calculated on total amount of reactants. A method according to any of the Claims 12-14c h a r a c t e r i s e d i n, that said acidic catalyst is neutralised by addition of a stoechiometric amount of an alkaline compound. A method according to any of the Claim 15c h a r a c t e r i s e d i n, that said alkaline compound is ammonium hydroxide and/oran alkali metal hydroxide. A method according to any of the Claims 11-16c h a r a c t e r i s e d i n, that yielded reaction mixture is diluted with an additionalamount of propionic acid to obtain a composition comprising 30-80% by weight of propionic acid and 20-70% by weight of glyceryl propionates. Use of a feed additive according to any of the Claims 1-10 as mould inhibitor.
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    同族专利:
    公开号 | 公开日
    SE1100413A1|2012-11-06|
    CN103648294B|2015-05-27|
    EP2713769A4|2014-12-24|
    EP2713769B1|2016-09-14|
    CN103648294A|2014-03-19|
    EP2713769A1|2014-04-09|
    DK2713769T3|2016-10-24|
    HUE029643T2|2017-02-28|
    WO2012161633A1|2012-11-29|
    PL2713769T3|2017-01-31|
    ES2605846T3|2017-03-16|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    WO2017200479A1|2016-05-20|2017-11-23|Perstorp Ab|Animal feed additive effective as broad-spectrum preservative|US2005371A|1934-08-18|1935-06-18|Eastman Kodak Co|Process for the manufacture of tripropionin|
    US3394009A|1964-07-24|1968-07-23|Atlas Chem Ind|Preparation of baked products|
    SU701631A1|1978-05-03|1979-12-05|Казахский Филиал Всесоюзного Научно- Исследовательского Института Комбикормовой Промышленности|Method of the preservation of feed|
    CA1168078A|1980-09-09|1984-05-29|Gerhard J. Haas|Intermediate moisture food preservation|
    US4847067A|1984-05-02|1989-07-11|Thomas Richard D|Mold and dust inhibiting product and method|
    HU0001509A3|1997-03-21|2001-11-28|Basf Ag|Propionic acid, ammonia, propanediol and water solutions and the use thereof|
    US7169424B2|2003-02-28|2007-01-30|Kemin Industries, Inc.|Mold inhibitor having reduced corrosiveness|
    IT1393045B1|2009-03-16|2012-04-11|Cantini|COMPOSITIONS CONTAINING MONOGLICERIDES OF ORGANIC ACIDS FROM C1 TO C7 AND GLYCEROL, THEIR PREPARATION AND USE AS ANTIBACTERIALS IN THE ZOOTECHNY.|
    BRPI0902564A2|2009-08-17|2011-05-03|Auster Nutricao Animal Ltda|composed of 1 monopropionine and its isomer 3 monopropionine as preservatives of animal feed, grain and flour|
    CN101691525B|2009-10-12|2011-11-30|河南兴泰科技实业有限公司|Glycerin fatty acid ester and preparation method thereof|SE541250C2|2017-05-04|2019-05-14|Perstorp Ab|Method for reduction of deoxynivalenol levels in feed|
    EP3809869A1|2018-06-22|2021-04-28|Basf Se|Compositions for animals and uses thereof|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    SE1100413A|SE1100413A1|2011-05-24|2011-05-24|Animal feed additive which acts as a preservative|SE1100413A| SE1100413A1|2011-05-24|2011-05-24|Animal feed additive which acts as a preservative|
    DK12790221.1T| DK2713769T3|2011-05-24|2012-05-14|ANIMAL FEEDING Additive EFFECTIVE AS PRESERVATIVE|
    ES12790221.1T| ES2605846T3|2011-05-24|2012-05-14|Effective animal feed additive as a preservative|
    EP12790221.1A| EP2713769B1|2011-05-24|2012-05-14|Animal feed additive effective as preservative|
    PL12790221T| PL2713769T3|2011-05-24|2012-05-14|Animal feed additive effective as preservative|
    PCT/SE2012/000073| WO2012161633A1|2011-05-24|2012-05-14|Animal feed additive effective as preservative|
    CN201280025197.3A| CN103648294B|2011-05-24|2012-05-14|Animal feed additive effective as preservative|
    HUE12790221A| HUE029643T2|2011-05-24|2012-05-14|Animal feed additive effective as preservative|
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