CN1193892A - 基于有机酸的可自由流动的颗粒、其制备方法及用途 - Google Patents
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Abstract
本发明公开了一种由芯和覆盖层组成的自由流动颗粒,其中芯材包含一种有机酸和一种多孔载体,覆盖层具有20℃下水溶的或水溶胀的包覆材料。
Description
本发明涉及由芯和覆盖层组成的可自由流动的颗粒,其中芯材包含一种有机酸和一种多孔载体,覆盖层具有可水溶的或可水溶胀的包覆材料。
本发明还涉及基于有机酸且可自由流动的低异味颗粒的制备方法,所述有机酸优选甲酸、乙酸和/或丙酸,本发明还涉及这种颗粒在食品加工及动物饲料加工中的应用,涉及它们在青贮饲料中的应用。
诸如甲酸、乙酸或丙酸的短链有机酸常用于食品和动物饲料的酸化与保存。这些酸的缺点是:(a)在室温时为液体;(b)因低的蒸气压导致刺鼻的异味;(c)腐蚀性。
此外,为将浓缩形式的液体有机酸加至动物饲料中,必须采用相当复杂的技术过程。
DE 28 33 727 A1公开了一种包含丙酸和载体的颗粒性杀菌材料。该材料可用于防止贮存的农产品中的大量霉菌菌落,使它们即使在几天的培养时间后仍不增加。但是,业已发现,这种材料本身在贮存时是不稳定的(失酸),能够采用的丙酸的最大用量很大程度上取决于所用的载体。另外,由于丙酸自身的挥发性,这种材料会产生令人不愉快的异味。
本发明的目的是提供用于食品-及动物饲料加工的可自由流动且低异味的颗粒,从而为用户提供显著改善的加工性能。本发明的注意力集中于制备以被吸附物形式的固体有机酸,所说的被吸附物与简单浸渍产品的区别之处在于:(a)无论载体如何,均可使固体含酸量大于30%(重量),因而活性成分含量非常高;(b)从被吸附物中释放的有机酸被减至最低,因此活性成分含量得以保持。粉状的终产品应具有优良的贮存性能、流动性能和加工性能。
业已发现,上述目的可以通过由芯和覆盖层组成的自由流动颗粒来实现,其中芯材包含一种有机酸和一种多孔载体,覆盖层具有20℃时可水溶的或可水溶胀的包覆材料。
该新颗粒的优点是:尽管是固体制剂,但强烈的刺鼻性异味减少,而酸可容易且快速地从固体粉末中释放。
进而,本发明涉及含有机酸和多孔载体的颗粒的制备方法,该方法包括,用液体有机酸浸渍载体,然后,用室温下为固体的包覆材料对其进行附聚,包覆材料的用量应使形成的颗粒被覆盖,此外,如果需要的话,通过加入香料进一步提供气味;如果需要的活,通过用细分的隔离剂进行撒粉处理,以确保附聚物的可自由流动性能。
在一个优选的实施方案中,新颗粒在其覆盖层表面上具有隔离剂。芯优选包含约30-90%(重量)、更优选50-80%(重量)的有机酸。有机酸优选是由一种或多种C1-C6的一元羧酸或二元羧酸组成,特别是甲酸、乙酸和/或丙酸。
适宜的载体为多孔的有机或无机载体,其粒径为1-1000μm,优选5-100μm。芯也可包含另一种固体,例如适宜作饲料添加剂的固体如丙酸钙。
水溶性聚合物、有机酸及其盐或低熔点的无机盐可用作包覆材料。
优选采用谷糠、硅酸盐、珍珠岩或硅石作为载体,以芯重量计,其用量为10-70%(重量)、优选20-40%(重量)。
优选使用的包覆材料为聚乙二醇、聚乙烯吡咯烷酮或C3-C14,优选C3-C6的有机酸和其盐,特别是柠檬酸、富马酸、琥珀酸、己二酸、苯甲酸和其盐,或氨基酸和其盐。
在新方法的一个优选实施方案中,首先将载体置于混合机,用有机酸浸渍,然后用包覆材料进行附聚和覆盖。
将疏松且浸渍过的载体颗粒与包覆材料(粘合液体)混合,粘合液体通常是由室温(20℃)下为固体的可水溶性或可水溶胀性物质的高浓度溶液或熔融物组成。这种粘合液体优选以加热状态包覆到浸渍的载体颗粒上,并与载体颗粒混合。粘合液体在浸渍过的载体颗粒的表面上固化。适宜的混合机加工参数使不同的颗粒附聚而得到更大的颗粒。
通过混合过程的工艺参数以及随后经筛分或研磨,得到所需颗粒尺寸。优选颗粒的平均直径小于3mm,更优选0.3-1.3mm。如果需要的话,残余水可在用于覆盖和附聚的粘合液体中存在。在附聚完成后,这部分水可通过无水且微细的隔离剂经撒粉过程而结合。所述撒粉过程也可以防止随后的附聚物的粘连,此外,可用所述有机酸的盐(如丙酸钠或丙酸钙)包覆附聚物。进而,如果需要的话,在撒粉步骤中可加入诸如香兰素、柠檬醛或果味素的香料或风味物质产生附加的异味掩蔽作用,并保证例如动物饲料消费更有兴趣。
原则上,所有耐酸的有机或无机多孔载体均适用于制备这种可自由流动的低异味的附聚物。其具体实例包括:谷糠、珍珠岩、粘土、硅酸盐和硅石,由于无机载体的性能更易于控制,因而它们是优选的。
优选使用的粘合液体是室温下为固体的水溶性或水溶胀性物质。这使其能省去随后的干燥步骤,其中,除了溶剂和附加的水外,在某些情形下有机酸也被蒸出。
为了防止附聚物在相对较高的贮存温度下形变,特别适宜的、用于附聚和覆盖过程的包覆材料(粘合液体)为软化温度大于30℃、优选大于60℃的那些材料。优选采用的包覆材料应对吸附有机酸的pH降低作用无相反影响,如果需要的话,甚至应能加强这种作用。
适宜的粘合液体为为高浓度的热糖溶液或碱金属/碱土金属甲酸盐/乙酸盐/丙酸盐溶液。最后的撒粉步骤可吸收残余的水。优选采用的粘合液体为低熔点的聚乙二醇、柠檬酸、己二酸、富马酸或苯甲酸或其盐的熔融物,高浓度氨基酸和这些酸的混合物的溶液。以颗粒重量计,粘合液体的用量为5-80(重量),优选10-25%(重量)。
除了多孔载体外,适宜的隔离剂为细分的研磨过的有机酸或其盐如甲酸钠,和无机酸盐或Aerosil硅胶。隔离剂的用量小于10%(重量),优选为0.5-5%(重量)。
一般说来,多孔载体首先加至混合机(如Eirich混合机)中,只需少量的能量输入即可用有机酸对其进行浸渍。而在另一过程中,也可以先将液体放入混合机中,再计量加入载体。在这种情况下,需要的能量输入较高。
必须确保均匀浸渍并避免局部过湿,否则会发生结块现象。在浸渍完成后,会出现可自由流动的且轻微堆积的颗粒。为了在喷射粘合液体时使液滴尺寸分布优良,粘合液体的粘度应通过适当地选择温度而确定,以使其小于1000、优选小于100mPa.S。由于在热的粘合液体与较冷的浸渍载体间存在温度差,在这种优选的实施方案中,粘合液体的液滴首先会迅速固化。在进一步的附聚过程中,由于机械和热能的输入,床层温度会增加10-30℃,这取决于粘合液体的类型。进而,粘合液体的液滴会积聚在已形成的附聚物上,这些液滴中的一些会与另一些发生聚结。在附聚过程中,能量输入会增加约20%。
最后,如前所述,可与隔离剂一起加入细分的赋予风味的物质。原则上,大多数香料和风味物质均可用于此目的,它们可根据附聚物的最后应用状况进行选择。以颗粒重量计,这些香料的用量小于1%(重量),优选为0.05-0.5%(重量)。所产生的附聚物具有低的粉含量,异味很小,其所含有机酸易于溶于水。
新的颗粒适用于加工食品和动物饲料及用于青贮饲料。具体而言,食品和动物饲料可理解为收获的产品,如干草、青贮饲料、湿谷物、豆类植物或谷类植物,以及奶代用品、液体产品、混合的矿物质饲料、鱼青饲料或鱼肉。
新的颗粒可以包含其它添加剂,如矿物质、维生素、抗生素或蛋白质强化剂。
实施例
(所用的甲酸含量=99%/所用丙酸含量=99%)
A.比较实施例
比较实施例1
将100g的小麦糠首先放置在一种家用混合机中,用100g甲酸进行浸渍。酸易于被吸收;产品表现出粘附性能,但它们易于分开,并且具有强烈的甲酸气味。
比较实施例2
将100g的Sipernat(微细硅石,来自Degussa)首先放置在一种家用混合机中,用100g的由等量甲酸和丙酸组成的酸性混合物进行浸渍。酸性混合物易于被吸收;形成一种疏松的可自由流动的产品。该产品具有强烈的令人不愉快的甲酸/丙酸气味。
比较例2
将100g的珍珠岩首先放置在一种家用混合机中,如实施例1用100g甲酸进行浸渍。甲酸易于被吸收;但产品表现出强烈的结块趋势并具有强烈的令人不愉快的甲酸气味。
B.浸渍、附聚和覆盖试验
实施例1
将460g Sipernat(微细硅石,来自Degussa)首先放置在一种Eirich混合机(RO2)中并用905g甲酸进行浸渍;甲酸含量为67%。然后,将来自热贮存容器作为粘合液体的80℃下的200g甲酸钠熔融物经一个二元喷嘴喷射进包含1000g该混合物的混合空间中。形成的附聚物用44g Sipernat进行撒粉处理。游离酸的含量为54%。形成的产品可自由流动,且其异味很小。
实施例2
将400g Sipernat(微细硅石,来自Degussa)首先放置在一种Eirich混合机(RO2)中并用1000g甲酸进行浸渍(甲酸含量为71%)。然后,将来自热贮存容器作为粘合液体的80℃下的180g浓葡聚糖溶液经一个二元喷嘴喷射进混合空间中。形成的附聚物用45g Sipernat和12g柠檬醛进行撒粉处理。酸含量为61%。形成的产品可自由流动。在浸渍后的能量消耗≈400W。在覆盖层后能量消耗≈500W。在附聚步骤中,速度从340rpm增至460rpm。
实施例3
将400g Sipernat首先放置在一种Eirich混合机中,与实施例2类似,用1100g甲酸进行浸渍,甲酸含量为71%。然后,将来自热贮存容器作为粘合液体的170℃下的260g柠檬酸熔融物经一个二元喷嘴喷射进混合空间中。形成的附聚物用44g Sipernat和8g香兰素进行撒粉处理。总酸含量≈74%。形成的附聚物基本消除了甲酸的异味。
实施例4
将8.7kg Sipernat首先放置在一种犁铧(ploughshare)混合机(Lo 130)中,用24kg甲酸(98%)进行浸渍(甲酸含量为71%)。为附聚和覆盖,将来自热贮存容器的170℃下的5.5kg柠檬酸熔融物经一个二元喷嘴喷射进混合空间中。形成的附聚物用650g Sipernat和24g香兰素进行撒粉处理。总酸含量≈74%。形成的附聚物基本消除了甲酸的异味并可自由流动。
Claims (11)
1、一种由芯和覆盖层组成的可自由流动颗粒,其中,芯材包含一种有机酸和一种多孔载体,覆盖层具有20℃下可水溶的或可水溶胀的包覆材料。
2、根据权利要求1的颗粒,其中在覆盖层的表面上还具有一种隔离剂。
3、根据权利要求1的颗粒,其中芯料包含30-90%(重量)的有机酸。
4、根据权利要求1的颗粒,其中有机酸为C1-C6的一元羧酸或二元羧酸或其混合物。
5、根据权利要求1的颗粒,其中所用的载体为多孔的有机或无机载体,其粒径为1-1000μm,优选5-100μm。
6、根据权利要求1的颗粒,其中所用的包覆材料为水溶性聚合物、有机酸、其盐或低熔点的无机盐。
7、根据权利要求5的颗粒,其中所用的载体为谷糠、硅酸盐、珍珠岩或硅石,其用量为10-70%(重量),优选20-40%(重量)。
8、根据权利要求6的颗粒,其中,所用的包覆材料为聚乙二醇、聚乙烯吡咯烷酮或C3-C14,优选C3-C6的有机酸或其盐,特别是柠檬酸、富马酸、琥珀酸、己二酸、苯甲酸、山梨酸或其盐、或氨基酸或其盐。
9、一种含有机酸和多孔载体的颗粒的制备方法,该方法包括,用液体有机酸浸渍载体,然后,用室温下固化的液化包覆材料使载体进行附聚,包覆材料的用量应使形成的颗粒被覆盖,此外,如果需要的话,通过加入香料进一步提供气味;如果需要的活,通过用细分的隔离剂进行撒粉处理,以确保附聚物的可自由流动性能。
10、根据权利要求9的方法,其中首先将载体置于混合机中,用有机酸浸渍,然后用包覆材料附聚和覆盖。
11、权利要求1的颗粒在食品和动物饲料以及青贮饲料的酸处理和防腐中的应用。
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DE19531782.3 | 1995-08-30 | ||
DE19531782A DE19531782A1 (de) | 1995-08-30 | 1995-08-30 | Rieselfähiges Granulat auf Basis organischer Säuren, Verfahren zu seiner Herstellung und seine Verwendung |
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CN1193892A true CN1193892A (zh) | 1998-09-23 |
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EP (1) | EP0847243A1 (zh) |
JP (1) | JPH11511969A (zh) |
KR (1) | KR19990044266A (zh) |
CN (1) | CN1193892A (zh) |
AU (1) | AU706207B2 (zh) |
BR (1) | BR9609990A (zh) |
CA (1) | CA2227282A1 (zh) |
CZ (1) | CZ49998A3 (zh) |
DE (1) | DE19531782A1 (zh) |
EA (1) | EA000874B1 (zh) |
GE (1) | GEP20002062B (zh) |
HU (1) | HUP9802322A3 (zh) |
IL (1) | IL122355A (zh) |
NO (1) | NO980861L (zh) |
NZ (1) | NZ316933A (zh) |
PL (1) | PL325169A1 (zh) |
SK (1) | SK22898A3 (zh) |
TR (1) | TR199800344T1 (zh) |
WO (1) | WO1997007687A1 (zh) |
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CN100381070C (zh) * | 2002-01-08 | 2008-04-16 | Can科技公司 | 通过用脂质和疏水性高熔点化合物的混合物包覆而进行的包囊化 |
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DE19710127A1 (de) * | 1997-03-12 | 1998-09-17 | Herbert Dr Widulle | Mittel zur Keimverminderung im Trinkwasser, Tränkewasser u. Waschwasser für Gemüse |
DE19933906A1 (de) * | 1999-07-22 | 2001-01-25 | Eckhard Eltz | Verfahren und Anordnung zur Behandlung von Futtermitteln |
DE10055390A1 (de) * | 2000-11-09 | 2002-05-29 | Nutrinova Gmbh | Einsatz eines Säurepräparates als Futtermittelzusatz in der Nutztieraufzucht |
KR100451545B1 (ko) * | 2002-03-18 | 2004-10-06 | 김유용 | 염산과 규산염광물질을 함유한 자돈사료첨가용 혼합조성물의 제조방법, 상기 혼합조성물 및 사료 |
DE10231891A1 (de) * | 2002-07-12 | 2004-01-22 | Basf Ag | Zubereitungen, enthaltend Diformiate |
SE528410C2 (sv) * | 2004-06-30 | 2006-11-07 | Kemira Grow How Ab | Antimikrobiell surgörande foderprodukt och förfarande för dess framställning |
EP1846475A1 (en) * | 2005-02-04 | 2007-10-24 | Basf Aktiengesellschaft | Water swellable material |
DE102006021392B4 (de) * | 2006-05-08 | 2013-06-27 | Ligrana Gmbh | Zusammensetzung |
DE102007031039A1 (de) * | 2007-07-04 | 2009-01-08 | Süd-Chemie AG | Verfahren zur schonenden Raffination von Pflanzenölen mit Naturbleicherde |
DE102021115047A1 (de) | 2021-06-10 | 2022-12-15 | André Brendler | Carbonsäure beladener Salzträger und das Verfahren zur Herstellung davon |
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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NL149989B (nl) * | 1967-03-08 | 1976-07-15 | Philips Nv | Korrelvormig preparaat. |
CH484625A (de) * | 1969-04-03 | 1970-01-31 | Libavia Ag | Verfahren zur Herstellung granulierter Futtermittel |
AR206283A1 (es) * | 1971-01-27 | 1976-07-15 | Chinoin Gyogyszer Es Vegyeszet | Una composicion para la conservacion de productos de procedencia animal o vegetal |
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 |
DE3103623A1 (de) * | 1979-08-03 | 1982-09-16 | Siegfried Dr. 8069 Sünzhausen Moser | "mineralstoffreiches ergaenzungsfutter und dessen verwendung" |
IT1185550B (it) * | 1985-04-12 | 1987-11-12 | Dox Al Italia Spa | Miscele non polverose di sfarinati o farine con principi attivi per mangimistica |
IT1229930B (it) * | 1988-10-14 | 1991-09-16 | Dox Al Italia Spa | Procedimento per la preparazione di miscele per uso alimentare e mangimistico comprendenti sostanze attive distribuite in modo uniforme |
US5082675A (en) * | 1989-07-29 | 1992-01-21 | Bp Chemicals Limited | Ensiling composition |
DE4117399A1 (de) * | 1990-06-14 | 1992-01-09 | Micro Plus Konzentrate Gmbh | Wasserhaltiges mittel zur konditionierung feinkoerniger mineralischer futtermittel |
DE4217971C1 (de) * | 1992-05-30 | 1993-10-21 | Boehringer Ingelheim Vetmed | Verfahren und Wirbelbettapparatur zum Granulieren und/oder Umhüllen |
EP0612843A1 (en) * | 1993-02-22 | 1994-08-31 | Unilever N.V. | Granular acidic cleaners |
IT1265290B1 (it) * | 1993-12-17 | 1996-10-31 | Dox Al Italia Spa | Miscele ad elevato contenuto di sostanze attive idonee ad essere distribuite in modo omogeneo nei mangimi per animali. |
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- 1995-08-30 DE DE19531782A patent/DE19531782A1/de not_active Withdrawn
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1996
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- 1996-08-26 GE GEAP19964214A patent/GEP20002062B/en unknown
- 1996-08-26 WO PCT/EP1996/003757 patent/WO1997007687A1/de not_active Application Discontinuation
- 1996-08-26 EP EP96930104A patent/EP0847243A1/de not_active Withdrawn
- 1996-08-26 TR TR1998/00344T patent/TR199800344T1/xx unknown
- 1996-08-26 IL IL12235596A patent/IL122355A/xx not_active IP Right Cessation
- 1996-08-26 HU HU9802322A patent/HUP9802322A3/hu unknown
- 1996-08-26 KR KR1019980701502A patent/KR19990044266A/ko not_active Application Discontinuation
- 1996-08-26 PL PL96325169A patent/PL325169A1/xx unknown
- 1996-08-26 BR BR9609990A patent/BR9609990A/pt not_active Application Discontinuation
- 1996-08-26 SK SK228-98A patent/SK22898A3/sk unknown
- 1996-08-26 JP JP9509846A patent/JPH11511969A/ja active Pending
- 1996-08-26 CN CN96196578A patent/CN1193892A/zh active Pending
- 1996-08-26 EA EA199800229A patent/EA000874B1/ru not_active IP Right Cessation
- 1996-08-26 AU AU69286/96A patent/AU706207B2/en not_active Ceased
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Cited By (1)
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CN100381070C (zh) * | 2002-01-08 | 2008-04-16 | Can科技公司 | 通过用脂质和疏水性高熔点化合物的混合物包覆而进行的包囊化 |
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BR9609990A (pt) | 1999-07-06 |
TR199800344T1 (xx) | 1998-05-21 |
HUP9802322A3 (en) | 2001-08-28 |
KR19990044266A (ko) | 1999-06-25 |
JPH11511969A (ja) | 1999-10-19 |
SK22898A3 (en) | 1998-12-02 |
EA199800229A1 (ru) | 1998-12-24 |
DE19531782A1 (de) | 1997-03-06 |
IL122355A0 (en) | 1998-04-05 |
NZ316933A (en) | 1999-01-28 |
WO1997007687A1 (de) | 1997-03-06 |
CZ49998A3 (cs) | 1998-08-12 |
HUP9802322A2 (hu) | 1999-01-28 |
CA2227282A1 (en) | 1997-03-06 |
EA000874B1 (ru) | 2000-06-26 |
NO980861D0 (no) | 1998-02-27 |
GEP20002062B (en) | 2000-05-10 |
MX9801399A (es) | 1998-05-31 |
AU706207B2 (en) | 1999-06-10 |
AU6928696A (en) | 1997-03-19 |
PL325169A1 (en) | 1998-07-06 |
IL122355A (en) | 2000-08-31 |
EP0847243A1 (de) | 1998-06-17 |
NO980861L (no) | 1998-02-27 |
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