CN101703148A - Long-acting low-corrosiveness feed mould inhibitor - Google Patents

Long-acting low-corrosiveness feed mould inhibitor Download PDF

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CN101703148A
CN101703148A CN200910213037A CN200910213037A CN101703148A CN 101703148 A CN101703148 A CN 101703148A CN 200910213037 A CN200910213037 A CN 200910213037A CN 200910213037 A CN200910213037 A CN 200910213037A CN 101703148 A CN101703148 A CN 101703148A
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feed
acid
corrosiveness
long
mould inhibitor
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CN101703148B (en
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李永富
孙震
史锋
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Jiangnan University
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Jiangnan University
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Abstract

The invention relates to a long-acting low-corrosiveness feed mould inhibitor. The physical and chemical reaction is carried out on propanoic acid and ammonium bicarbonate, and then reaction products are compounded with synergistic agents of acetic acid, benzoic acid, sorbic acid, citric acid and alcohol, and finally a liquid state product or a solid state product is prepared. The feed mould inhibitor can effectively inhibit moulds in feed from growing and breeding and can prevent the generation of mycotoxin if added in the feed. The feed mould inhibitor has the advantages of good mould proof effect, long mould proof time, weak volatileness, little corrosion to equipment, little thrill to production staffs, environmental protection and the like, and the pH value is close to that of the feed.

Description

Long-acting low-corrosiveness feed mould inhibitor
Technical field
The present invention relates to field of fodder, be specifically related to a kind of Midew preventive for feed that is applicable to single feed, additive premix, concentrated feed, mixed feed and concentrate supplement.
Background technology
Worldwide, cereal and feed all exist serious mould contamination.Feed mold can cause its nutritional labeling to reduce, and can not obtain corresponding nutritional amt after animal searches for food; Feed mold also causes the feed palatability to descend minimizing of searching for food property or the apocleisis of animal; Cause the mould of feed mold also can produce a large amount of mycotoxins, the animal production capacity of searching for food is descended, heavy then cause the death of the animal that searches for food; Many mycotoxins have very high residual rate in animal body, not only can directly cause murder by poisoning to animal, also can transfer to the human body from animal by food chain, and human body is produced injury.At present, prevent that going mouldy mainly of feed from realizing by adding Midew preventive for feed.
The mould inhibitor that uses in the feed is based on propionic acid and its esters at present.The propionic acid anti-mold effect is good, but high volatility, the mildew-resistant duration is short, and big to production equipment corrosivity, big to producers' health hazard, the price of propionic acid is higher in addition, and in order to reach anti-mold effect preferably, needing increases consumption, and feed cost is improved; Though the propionate compound volatility is low, its anti-mold effect is not as propionic acid.
The content of invention
At the above-mentioned deficiency of existing propionic acid and propionate compound Midew preventive for feed, the applicant has carried out improving research, and a kind of long-acting low-corrosiveness feed mould inhibitor is provided, and not only anti-mold effect is stronger, and cost is also lower.
Technical scheme of the present invention is as follows:
A kind of long-acting low-corrosiveness feed mould inhibitor, the component of prescription comprises propionic acid and carbonic hydroammonium, the mass fraction of described two components is:
Propionic acid 10~60
Carbonic hydroammonium 1~40
Above-mentioned two components are placed the reactor of 50~85 ℃ of temperature,, obtain liquid product in speed of agitator 50~200 commentaries on classics/min reaction 2~6 hours down.
Its further technical scheme is: the component in the described prescription also comprises synergist, and described synergist comprises acetate, benzoic acid, sorbic acid, citric acid and ethanol, and the mass fraction of described each component is:
Propionic acid 10~60
Carbonic hydroammonium 1~40
Acetate 0.1~10
Benzoic acid 0.1~15
Sorbic acid 0.1~10
Citric acid 0.1~15
Ethanol 0.1~15
The carbonic hydroammonium that by propionic acid and mass fraction is 1~30 part reacted 2~6 hours in the reactor of 50~85 ℃ of temperature, speed of agitator 50~200 commentaries on classics/min, the each component that adds remaining ammonium hydrogencarbonate and described synergist then, continue reaction 1~5 hour, obtain liquid product.
Its further technical scheme is: the pH value of resulting product is 4.5~6.5.
Its further technical scheme is: the described liquid product that will obtain adds in the inserts, make solid-state long-acting low-corrosiveness feed mould inhibitor, described inserts is at least a in vermiculite, white carbon, rice chaff, the zeolite powder, and the mass fraction of described liquid product and inserts is:
Liquid product 300~500
Inserts 500~700.
Useful technique effect of the present invention is:
(1) the present invention reacts propionic acid and carbonic hydroammonium, generates the stable propionic acid and the system of ammonium, greatly reduces the volatility of propionic acid; (2) the pH value and the feed of product are close, and have reduced the buffering of feed to mould inhibitor, have significantly improved anti-mold effect; (3) price of carbonic hydroammonium has significantly reduced the cost of mould inhibitor less than 1/5th of propionic acid; (4) add synergist acetate, benzoic acid, sorbic acid, citric acid and ethanol in the system of propionic acid and ammonium, strengthened the mildew-resistant fungistatic effect of goods, enlarged scope of restraining fungi, goods are applied widely; (5) original form of product is a liquid, can directly mix workshop section at feed and add, and can effectively reduce the surface tension of moisture, and water fully is penetrated in the feed, reduces water activity, and feed is difficult for going mouldy; (6) add the liquid mould inhibitor and also can reduce the friction of feed in pelletization, prolong the ring mould life-span, reduce power consumption, save the pellet processing cost.
Description of drawings
Fig. 1 is the contrast figure of Escherichia coli growth curve.
Fig. 2 is the contrast figure of Listeria monocytogenes growth curve.
The specific embodiment
By the following examples the present invention is specifically described.
Embodiment 1:
Take by weighing propionic acid 1200g, ammonium hydrogencarbonate 200g by mass fraction, join in the reactor, temperature is controlled at 80 ℃, mixing speed 120 commentaries on classics/min.Behind reaction 4h, add carbonic hydroammonium 100g, acetate 15g, benzoic acid 20g, sorbic acid 15g, citric acid 20g, ethanol 25g, continue reaction 3h, obtain the Midew preventive for feed goods.Said products is a liquid, and the pH value is 5, and the consumption that directly is added in the feed is a 400g/ ton feed.After 300g flowing product and the mixing of 500g rice chaff, the amount ratio in feed is a 1000g/ ton feed.
The mensuration of embodiment 1 goods fungistatic effect
1, the mensuration of embodiment 1 goods minimal inhibitory concentration (MIC):
Get bacterium (staphylococcus aureus, Escherichia coli, salmonella, bacillus subtilis), mould (mould, aspergillus) respectively, each bacterium 1mL (bacteria containing amount 10 6CFU/mL) add 10 milliliters test tube respectively 1~No. 9, insert the 9mL nutrient solution in each test tube.In vitro add the Midew preventive for feed flowing product that the different embodiment 1 that measure obtain at 1~No. 8, make the volumetric concentration of No. 1 pipe to No. 8 interior mould inhibitor flowing product of pipe be respectively 0.5 ‰ (v/v), 1.0 ‰ (v/v), 1.5 ‰ (v/v), 2.0 ‰ (v/v), 2.5 ‰ (v/v), 3.0 ‰ (v/v), 3.5 ‰ (v/v), 4.0 ‰ (v/v), No. 9 Guan Weiwu mould inhibitor flowing product pipes, No. 10 pipe is sterile tube.Mould in above-mentioned each test tube (mould, aspergillus) was cultivated 48 hours in 28 ℃ incubator, bacterium in above-mentioned each test tube (staphylococcus aureus, Escherichia coli, salmonella, bacillus subtilis) was cultivated 24 hours in 37 ℃ incubator, and measurement result sees Table 1-1.
Table 1-1 embodiment 1 goods are to the MIC measurement result of bacterium and mould
Figure G2009102130371D0000031
Annotate :+expression testing result is positive, promptly detects;-expression testing result is negative, does not promptly measure; ± expression testing result is a probable positive, and is promptly suspicious, but can not determine, down together.
Table 1-1 result show: embodiment 1 goods are 1 ‰ (v/v) for the MIC of Escherichia coli, salmonella and staphylococcus aureus, are 1.5 ‰ (v/v) for bacillus subtilis.For mould and aspergillus, MIC is 2 ‰ (v/v).
2, embodiment 1 goods adopt the Oxford agar diffusion method to carry out the mensuration of fungistatic effect:
Adopt the Oxford agar diffusion method, getting mould, aspergillus, head mold respectively is coated on the corresponding culture medium, the Oxford cup is positioned on the culture medium, add the Midew preventive for feed goods 1mL that embodiment 1 obtains in each Oxford cup, volumetric concentration is respectively 0.8% (v/v), 1.2% (v/v), 1.6% (v/v), and that measures above-mentioned Midew preventive for feed goods respectively presses down the mould effect; And compare with the mould effect that presses down that adds SPSS in the cup of Oxford.Above-mentioned mould, aspergillus, head mold were cultivated 48 hours in 28 ℃ incubator, and that measures mould inhibitor and physiological saline presses down the mould result, and measurement result sees Table 1-2.
The test of table 1-2 embodiment 1 goods anti-mold effect
Annotate: data are the diameter of inhibition zone in the table, and unit is mm, down together.
Table 1-2 result shows that embodiment 1 goods all have good result to the fungistatic effect of mould, aspergillus, head mold.
Embodiment 2:
Take by weighing propionic acid 2500g, ammonium hydrogencarbonate 900g by mass fraction, join in the reactor, temperature is controlled at 75 ℃, mixing speed 100 commentaries on classics/min.Behind reaction 4h, add carbonic hydroammonium 600g, acetate 200g, benzoic acid 400g, sorbic acid 200g, citric acid 400g, ethanol 400g, continue reaction 4h, obtain the Midew preventive for feed goods.Said products is a liquid, and the pH value is 5, and the consumption that directly is added in the feed is a 450g/ ton feed.After 350g flowing product, 100g white carbon and the mixing of 450g vermiculite, the amount ratio in feed is 1500/ ton of feed.
The mensuration of embodiment 2 goods fungistatic effects
1, the mensuration of embodiment 2 goods minimal inhibitory concentrations (MIC): its method of testing is described identical with embodiment 1, and measurement result sees Table 2-1.
Table 2-1 embodiment 2 goods are to the MIC measurement result of bacterium and mould
Figure G2009102130371D0000051
2, embodiment 2 goods adopt the Oxford agar diffusion method to carry out the mensuration of fungistatic effect: its method of testing is described identical with embodiment 1, and measurement result sees Table 2-2.
The test of table 2-2 embodiment 2 goods anti-mold effects
Figure G2009102130371D0000052
Embodiment 3:
Take by weighing propionic acid 3500g, ammonium hydrogencarbonate 1600g by mass fraction, join in the reactor, temperature is controlled at 85 ℃, mixing speed 120 commentaries on classics/min.Behind reaction 4h, add carbonic hydroammonium 900g, acetate 500g, benzoic acid 800g, sorbic acid 500g, citric acid 800g, ethanol 800g, continue reaction 3h, obtain the Midew preventive for feed goods.Said products is a liquid, and the pH value is 5.5, and the consumption that directly is added in the feed is a 500g/ ton feed.After 400g flowing product, 100 rice chaffs and the mixing of 500g zeolite powder, the amount ratio in feed is a 1000g/ ton feed.
The mensuration of embodiment 3 goods fungistatic effects
1, the mensuration of embodiment 3 goods minimal inhibitory concentrations (MIC): its method of testing is described identical with embodiment 1, and measurement result sees Table 3-1.
Table 3-1 embodiment 3 goods are to the MIC measurement result of bacterium and mould
Figure G2009102130371D0000061
2, embodiment 3 goods adopt the Oxford agar diffusion method to carry out the mensuration of fungistatic effect: its method of testing is described identical with embodiment 1, and measurement result sees Table 3-2.
The test of table 3-2 embodiment 3 goods anti-mold effects
Figure G2009102130371D0000062
Embodiment 4:
Take by weighing propionic acid 5000g, ammonium hydrogencarbonate 2300g by mass fraction, join in the reactor, temperature is controlled at 70 ℃, mixing speed 50 commentaries on classics/min.Behind reaction 2h, add carbonic hydroammonium 1000g, acetate 750g, benzoic acid 1200g, sorbic acid 750g, citric acid 1200g, ethanol 1200g, continue reaction 5h, obtain the Midew preventive for feed goods.Said products is a liquid, and the pH value is 6.5, and the consumption that directly is added in the feed is a 700g/ ton feed.After 450g flowing product, 150g vermiculite, 150g white carbon and the mixing of 350g rice chaff, the amount ratio in feed is 1500/ ton of feed.
The mensuration of embodiment 4 goods fungistatic effects
1, the mensuration of embodiment 4 goods minimal inhibitory concentrations (MIC): its method of testing is described identical with embodiment 1, and measurement result sees Table 4-1.
Table 4-1 embodiment 4 goods are to the MIC measurement result of bacterium and mould
Figure G2009102130371D0000071
2, embodiment 4 goods adopt the Oxford agar diffusion method to carry out the mensuration of fungistatic effect: its method of testing is described identical with embodiment 1, and measurement result sees Table 4-2.
The test of table 4-2 embodiment 4 goods anti-mold effects
Figure G2009102130371D0000072
Embodiment 5:
Take by weighing propionic acid 6000g, ammonium hydrogencarbonate 3000g by mass fraction, join in the reactor, temperature is controlled at 50 ℃, mixing speed 200 commentaries on classics/min.Behind reaction 6h, add carbonic hydroammonium 1000g, acetate 1000g, benzoic acid 1500g, sorbic acid 1000g, citric acid 1500g, ethanol 1500g, continue reaction 1h, obtain the Midew preventive for feed goods.Said products is a liquid, and the pH value is 4.5, and the consumption that directly is added in the feed is a 300g/ ton feed.After 500g flowing product, 100g vermiculite, 100g white carbon, 150g rice chaff and the mixing of 350g zeolite powder, the amount ratio in feed is 2000/ ton of feed.
The mensuration of embodiment 5 goods fungistatic effects
1, the mensuration of embodiment 5 goods minimal inhibitory concentrations (MIC): its method of testing is described identical with embodiment 1, and measurement result sees Table 5-1.
Table 5-1 embodiment 5 goods are to the MIC measurement result of bacterium and mould
Figure G2009102130371D0000081
2, embodiment 5 goods adopt the Oxford agar diffusion method to carry out the mensuration of fungistatic effect: its method of testing is described identical with embodiment 1, and measurement result sees Table 5-2.
The test of table 5-2 embodiment 5 goods anti-mold effects
Figure G2009102130371D0000082
Embodiment 6:
The anti-mold effect control experiment:
Adding volumetric concentration in culture medium respectively is above embodiment 1, embodiment 3, embodiment 5 goods of 2 ‰ (v/v), be contrast with the physiological saline group that adds with volumetric concentration, measure the growth curve of Escherichia coli and Listeria monocytogenes respectively with AAS, by measuring the absorbance of measured matter at 625mm wavelength place, measurement result is seen Fig. 1 and Fig. 2 respectively.
Fig. 1 is the contrast figure of Escherichia coli growth curve.Fig. 2 is the contrast figure of Listeria monocytogenes growth curve.Abscissa is the time among the figure, and ordinate is the absorbance of the 625mm wavelength light that records of spectrophotometer.The result of Fig. 1 and Fig. 2 shows that the goods of embodiment 1, embodiment 3, embodiment 5 can effectively suppress the propagation of these two kinds of bacteriums, and fungistatic effect is strong, and adopts the fungistatic effect of physiological saline very weak.
The used bacterium of the various embodiments described above, mould and culture medium thereof are the commercial goods, and wherein culture medium is respectively a bacterium: cultured solution of broth, mould: potato culture, aspergillus and head mold: husky formula culture medium.

Claims (4)

1. long-acting low-corrosiveness feed mould inhibitor, it is characterized in that: the component of prescription comprises propionic acid and carbonic hydroammonium, the mass fraction of described two components is:
Propionic acid 10~60
Carbonic hydroammonium 1~40
Above-mentioned two components are placed the reactor of 50~85 ℃ of temperature,, obtain liquid product in speed of agitator 50~200 commentaries on classics/min reaction 2~6 hours down.
2. according to the described long-acting low-corrosiveness feed mould inhibitor of claim 1, it is characterized in that: the component in the described prescription also comprises synergist, and described synergist comprises acetate, benzoic acid, sorbic acid, citric acid and ethanol, and the mass fraction of described each component is:
Propionic acid 10~60
Carbonic hydroammonium 1~40
Acetate 0.1~10
Benzoic acid 0.1~15
Sorbic acid 0.1~10
Citric acid 0.1~15
Ethanol 0.1~15
The carbonic hydroammonium that by propionic acid and mass fraction is 1~30 part reacted 2~6 hours in the reactor of 50~85 ℃ of temperature, speed of agitator 50~200 commentaries on classics/min, the each component that adds remaining ammonium hydrogencarbonate and described synergist then, continue reaction 1~5 hour, obtain liquid product.
3. according to claim 1 or 2 described long-acting low-corrosiveness feed mould inhibitors, it is characterized in that: the pH value of resulting product is 4.5~6.5.
4. according to claim 1 or 2 described long-acting low-corrosiveness feed mould inhibitors, it is characterized in that: the described liquid product that will obtain adds in the inserts, make solid-state long-acting low-corrosiveness feed mould inhibitor, described inserts is at least a in vermiculite, white carbon, rice chaff, the zeolite powder, and the mass fraction of described liquid product and inserts is:
Liquid product 300~500
Inserts 500~700.
CN2009102130371A 2009-11-10 2009-11-10 Long-acting low-corrosiveness feed mould inhibitor Expired - Fee Related CN101703148B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103168974A (en) * 2013-03-25 2013-06-26 重庆民泰香料化工有限责任公司 Liquid mildewproof agent for feed and method for avoiding mildew of feed
CN104970258A (en) * 2015-07-17 2015-10-14 四川农业大学 Compound feed additive with antioxidant function capable of relieving mycotoxicosis of piggy
CN105341360A (en) * 2015-12-07 2016-02-24 重庆华睿隆生物科技有限公司 Carrier-free propionic acid solid feed mildew preventive and preparation and use thereof
CN109647339A (en) * 2019-01-25 2019-04-19 中国科学院兰州化学物理研究所 The method for preparing mold toxin sorbent using semicoke

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1059454A (en) * 1991-09-06 1992-03-18 蒋石磊 Long-lasting fungicide for composite feed
CN1284266A (en) * 2000-07-19 2001-02-21 谢艳蓉 Mildew-proof preservative and preparation method and application thereof
CN100442992C (en) * 2006-11-30 2008-12-17 上海交通大学 Mold-proof oxidation-resistant compound additive

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103168974A (en) * 2013-03-25 2013-06-26 重庆民泰香料化工有限责任公司 Liquid mildewproof agent for feed and method for avoiding mildew of feed
CN103168974B (en) * 2013-03-25 2014-06-11 重庆民泰香料化工有限责任公司 Liquid mildewproof agent for feed and method for avoiding mildew of feed
CN104970258A (en) * 2015-07-17 2015-10-14 四川农业大学 Compound feed additive with antioxidant function capable of relieving mycotoxicosis of piggy
CN105341360A (en) * 2015-12-07 2016-02-24 重庆华睿隆生物科技有限公司 Carrier-free propionic acid solid feed mildew preventive and preparation and use thereof
CN109647339A (en) * 2019-01-25 2019-04-19 中国科学院兰州化学物理研究所 The method for preparing mold toxin sorbent using semicoke

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