CN104509701B - The preparation method of tributyrin microcapsules - Google Patents
The preparation method of tributyrin microcapsules Download PDFInfo
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- CN104509701B CN104509701B CN201510012138.8A CN201510012138A CN104509701B CN 104509701 B CN104509701 B CN 104509701B CN 201510012138 A CN201510012138 A CN 201510012138A CN 104509701 B CN104509701 B CN 104509701B
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- tributyrin
- acid
- parts
- emulsifying agent
- microcapsules
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- UYXTWWCETRIEDR-UHFFFAOYSA-N Tributyrin Chemical compound CCCC(=O)OCC(OC(=O)CCC)COC(=O)CCC UYXTWWCETRIEDR-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000003094 microcapsule Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 17
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 14
- 229930195729 fatty acid Natural products 0.000 claims abstract description 14
- 239000000194 fatty acid Substances 0.000 claims abstract description 14
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 12
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 11
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 11
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000000839 emulsion Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000002535 acidifier Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000004571 lime Substances 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 10
- -1 butyric acid glycerine Ester Chemical class 0.000 claims description 8
- 235000021314 Palmitic acid Nutrition 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 229920000223 polyglycerol Polymers 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims 1
- 229920000053 polysorbate 80 Polymers 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 235000019730 animal feed additive Nutrition 0.000 abstract description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 16
- 235000011116 calcium hydroxide Nutrition 0.000 description 14
- 238000001035 drying Methods 0.000 description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 6
- 241001465754 Metazoa Species 0.000 description 6
- 239000011575 calcium Substances 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 230000000968 intestinal effect Effects 0.000 description 3
- 150000004668 long chain fatty acids Chemical class 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000004652 butanoic acids Chemical class 0.000 description 2
- 210000001072 colon Anatomy 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 150000002943 palmitic acids Chemical class 0.000 description 2
- 210000002784 stomach Anatomy 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000252983 Caecum Species 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- PASOAYSIZAJOCT-UHFFFAOYSA-N butanoic acid Chemical compound CCCC(O)=O.CCCC(O)=O PASOAYSIZAJOCT-UHFFFAOYSA-N 0.000 description 1
- FYPVXEILSNEKOO-UHFFFAOYSA-L calcium;butanoate Chemical compound [Ca+2].CCCC([O-])=O.CCCC([O-])=O FYPVXEILSNEKOO-UHFFFAOYSA-L 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 210000004534 cecum Anatomy 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000024245 cell differentiation Effects 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 210000004913 chyme Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000037406 food intake Effects 0.000 description 1
- 210000004051 gastric juice Anatomy 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- MFBOGIVSZKQAPD-UHFFFAOYSA-M sodium butyrate Chemical compound [Na+].CCCC([O-])=O MFBOGIVSZKQAPD-UHFFFAOYSA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Fodder In General (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a kind of preparation method of tributyrin microcapsules, it is prepared from by 100 parts of raw fatty acid, 50 ~ 100 parts of tributyrin, 1 ~ 10 part of emulsifying agent, 13 ~ 15 parts of calcium hydroxide：By the fusing of tributyrin, aliphatic acid and emulsifying agent Hybrid Heating, then add it to and stirred in 80 ± 5 DEG C of warm water, form emulsion；By calcium hydroxide it is soluble in water be made 10 ~ 20% lime slurry；The emulsion that first two steps are obtained is mixed, reaction generation solid particle；Moisture is filtered out, and the tributyrin microcapsules finished product flowed freely at room temperature can be formed after filtration cakes torrefaction.The advantage of the invention is that production cost is low, technique is simple, and equipment is inexpensive, is conducive to industrialized production, and the obtained solid particle finished product with free-running property is more convenient when being used as animal feed additive.
Description
Technical field
The present invention relates to animal feed additive, more particularly, to a kind of preparation method of tributyrin microcapsules.
Background technology
Butyric acid is significant to the enteral nutrition of animal, 1. it not still animal colon cellular energy it is main come
Source, and be the matrix that cell membrane synthesizes lipid, in the growth of promotion alimentary canal cell, Cell differentiation inducing activity, influence gene table
Reach, play an important roll in inducing cell apoptosis.2. butyric acid can make the reduction of intestinal environment pH value, suppress harmful bacteria growing, therefore
In feedstuff industry, butyric acid and its salt are able to extensive use as a kind of multifunctional feed additive.However, because butyric acid is in normal temperature
It is down liquid, and has pole niff, using very inconvenient, so butyrate such as sodium butyrate or calcium butyrate need to be typically made
Use.
Butyric acid is small molecular organic compounds, can be absorbed quickly in stomach and alimentary canal leading portion, it is difficult to reach after alimentary canal
Section such as caecum and colon play a role.By being coated with sustained release to butyrate butyrate can be made to reach alimentary canal back segment.But butyric acid
Salt is that butyric acid neutralizes later product, big contribution is had no to reduction gut pH, so coated butyrate can only be played
State effect 1. and effect 2. can not be played.
Tributyrin is the derivative of butyric acid, is not decomposed in hydrochloric acid in gastric juice, fourth can be slowly decomposed into intestinal environment
Acid and glycerine.Although tributyrin can play two above effect simultaneously, because tributyrin is liquid, use
It is inconvenient.Chinese patent application（Application number 201410298903.2）《Tributyrin solid granulates type preparation and its system
Preparation Method and application》Disclose it is a kind of prepare the method for solid pharmaceutical preparation with white carbon silica gel absorption tributyrin, but adopt
Tributyrin is simply adsorbed with inorganic adsorbent and there are many defects：When inorganic adsorbent absorption tributyrin is more
When, adsorbent surface is more moist, easily caking, no free-running property；Simultaneously because tributyrin boiling point is high, it is impossible to using conventional
Dry particle is made in method such as heat drying, so as to influence the commodity form of product.
The content of the invention
It is an object of the invention to provide a kind of side that tributyrin microcapsules are prepared by membrane material of fatty acid calcium
Method.
To achieve the above object, the present invention can take following technical proposals：
The preparation method of tributyrin microcapsules of the present invention, it is by raw fatty acid, three butyric acid glycerine
Ester, emulsifying agent, calcium hydroxide are matched according to following weight parts and step is prepared from：
Proportioning：100 parts of aliphatic acid, 50 ~ 100 parts of tributyrin, 1 ~ 10 part of emulsifying agent, 13 ~ 15 parts of calcium hydroxide；
Concretely comprise the following steps：
The first step, tributyrin, aliphatic acid and emulsifying agent Hybrid Heating is melted, then add it to 5 ~ 10 times of amounts
Stirred in 80 ± 5 DEG C of warm water, form emulsion；
Second step, the lime slurry that water is made 10 ~ 20% is dissolved in by calcium hydroxide；
3rd step, the emulsion that the first step and second step are obtained is mixed, reaction generation solid particle；
4th step, moisture is filtered out, and 0.2 ~ 1.0mm of diameter is formed after gained filtration cakes torrefaction, has free-flowing at room temperature
The tributyrin microcapsules finished product of property.The content of tributyrin reaches in obtained tributyrin microcapsules finished product
30~50%。
The aliphatic acid is the chain saturated fatty acids of animal and plant fat, preferably stearic acid or palmitic acid.
Described emulsifying agent is tristerin or/and polyglycerol fatty glyceride or/and sucrose ester or/and told
Temperature 80, it is preferred that emulsifying agent can use HLB value for 8 ~ 10 three polyglyceryl fatty acid esters.
Wherein the drying means of the 4th step includes pneumatic conveying drying, fluidized bed drying or drying room low temperature drying.
Because tributyrin is water insoluble but can be dissolved each other with long chain fatty acids, therefore by tributyrin, long-chain fat
Added after fat acid and emulsifier for mixing in warm water, aliphatic acid, which may be homogenously dispersed in, forms micro emulsion in water, due to tributyrin
Polarity is small, inside micro emulsion, and long chain fatty acids, which are distributed on the outside of tributyrin drop, forms micro-capsule, now in system
Calcium hydroxide aqueous solution is added, long chain fatty acids form fatty acid calcium with calcium hydroxide reaction and quickly solidify to form the micro- of stabilization
Capsule.
The advantage of the invention is that：（1）By the microencapsulation in aqueous phase, obtained at room temperature it is stable have it is wandering
Property tributyrin microcapsules solid powder, be easy to use；When these microcapsules through animal ingestion enter stomach, in acid
Fatty acid calcium is dissociated into aliphatic acid in property environment, and microcapsule structure is transformed into fat-soluble soft particle, enters enteron aisle with chyme, in intestines
Aliphatic acid is progressively absorbed in road, is absorbed while tributyrin is gradually dissociated into intestinal environment after butyric acid；（2）Make
Aliphatic acid and tributyrin compatibility for the matrix material of microcapsules is good, and can be digested and assimilated by animal, is animal life
It is long that energy is provided；（3）Production cost is low, and technique is simple, equipment is inexpensive, is conducive to industrialized production, and what is obtained has free-running property
Solid particle finished product it is more convenient when being used as animal feed additive.
Embodiment
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1
1st, 100kg stearic acid, 55kg tributyrins, the polyglycerol fatty acids of 5kg tri- are added in 500L reactors
Ester, heating fusing makes material temperature stable at 80 ± 5 DEG C；
2nd, 80 ± 5 DEG C of 1000kg hot water is added in 2000L reactors, the oil phase thing melted in the 1st step is beaten
Enter, stir 3 ~ 10min, be dispersed in water oil phase；
3rd, the calcium hydroxide and 100kg water for weighing 13kg are mixed to form milk of lime, are squeezed into simultaneously with pump from the bottom of reactor
Stirring, milk of lime continues to stir 10 minutes after adding, blowing, with 200 mesh filter screen drainages, and filter cake dries 20 in 50 DEG C of drying rooms ~
40h, obtains tributyrin fatty acid calcium microcapsules 173kg, wherein tributyrin content 31.8%.
Embodiment 2
1st, 100kg palmitic acids, 100kg tributyrins, the polyglyceryl fatty acid esters of 2kg tri- are added in 500L reactors,
2kg Tween 80s, heating fusing makes material temperature stable at 80 ± 5 DEG C；
2nd, 1300 kg, 80 ± 5 DEG C of hot water are added in 2000L reactors, the oil phase thing melted in the 1st step is squeezed into,
3 ~ 10min is stirred, oil phase is dispersed in water；
3rd, 15kg calcium hydroxides are weighed and 100kg water is mixed to form milk of lime, is squeezed into and is stirred with pump from the bottom of reactor
To mix, milk of lime continues to stir 10 minutes after adding, blowing, with 200 mesh filter screen drainages, filter cake dries 20 in 50 DEG C of drying rooms ~
40h, obtains tributyrin fatty acid calcium microcapsules 220kg, tributyrin content 45.5%.
Embodiment 3
1st, 100kg palmitic acids, 70kg tributyrins, the polyglyceryl fatty acid esters of 5kg tri- are added in 500L reactors,
Heating fusing makes material temperature stable at 80 ± 5 DEG C；
2nd, 80 ± 5 DEG C of hot water of 1000kg are added in 2000L reactors, the oil phase thing melted in the 1st step is squeezed into,
3 ~ 10min is stirred, oil phase is dispersed in water；
3rd, 15kg calcium hydroxides are weighed and 100kg water is mixed to form milk of lime, is squeezed into and is stirred with pump from the bottom of reactor
To mix, milk of lime continues to stir 10 minutes after adding, blowing, with 200 mesh filter screen drainages, filter cake dries 20 in 50 DEG C of drying rooms ~
40h, obtains tributyrin fatty acid calcium microcapsules 190kg, tributyrin content 36.8%.
Claims (2)
1. a kind of preparation method of tributyrin microcapsules, it is characterised in that：It is by raw fatty acid, three butyric acid glycerine
Ester, emulsifying agent, calcium hydroxide are matched according to following weight parts and step is prepared from：
Proportioning：100 parts of aliphatic acid, 50 ~ 100 parts of tributyrin, 1 ~ 10 part of emulsifying agent, 13 ~ 15 parts of calcium hydroxide；
Concretely comprise the following steps：
The first step, by tributyrin, aliphatic acid and emulsifying agent Hybrid Heating melt, then add it to 5 ~ 10 times amount 80 ±
Stirred in 5 DEG C of warm water, form emulsion；
Second step, the lime slurry that water is made 10 ~ 20% is dissolved in by calcium hydroxide；
3rd step, the emulsion that the first step and second step are obtained is mixed, reaction generation solid particle；
4th step, moisture is filtered out, and 0.2 ~ 1.0mm of diameter is formed after gained filtration cakes torrefaction, has free mobility at room temperature
Tributyrin microcapsules finished product；
The aliphatic acid is stearic acid or palmitic acid.
2. the preparation method of tributyrin microcapsules according to claim 1, it is characterised in that：Described emulsifying agent
For tristerin or/and polyglycerol fatty acid ester or/and sucrose ester or/and Tween 80.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510012138.8A CN104509701B (en) | 2015-01-12 | 2015-01-12 | The preparation method of tributyrin microcapsules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510012138.8A CN104509701B (en) | 2015-01-12 | 2015-01-12 | The preparation method of tributyrin microcapsules |
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| CN104509701A CN104509701A (en) | 2015-04-15 |
| CN104509701B true CN104509701B (en) | 2017-07-11 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107751646A (en) * | 2017-11-08 | 2018-03-06 | 浙江恒兴饲料有限公司 | A kind of special antibacterial additive of aquatic products and its production method |
| CN108642105B (en) * | 2018-04-18 | 2021-03-30 | 江南大学 | A kind of method for enzymatic inclusion of tributyrin |
| CN108770948A (en) * | 2018-05-08 | 2018-11-09 | 江南大学 | It is a kind of using maltodextrin and cyclodextrin as the tributyrin microcapsules of wall material |
| CN108850558A (en) * | 2018-05-23 | 2018-11-23 | 江南大学 | A method of microcapsules tributyrin is prepared using tween emulsifier |
| CN112602841B (en) * | 2020-12-15 | 2022-03-29 | 南京农业大学 | A kind of oxymatrine and tributyrin composite microcapsule and its preparation method and application |
| CN115363135A (en) * | 2021-05-19 | 2022-11-22 | 湖北浩华生物技术有限公司 | High-oil-loading water-dispersible tributyrin feed additive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101301030A (en) * | 2008-05-22 | 2008-11-12 | 新奥（厦门）农牧发展有限公司 | Prescription of particles coated by butanoic acid derivative for feeding and preparing technique thereof |
| IT1392214B1 (en) * | 2008-11-28 | 2012-02-22 | Sila S R L | PROCESS FOR THE PRODUCTION OF A COMPOUND OF N-BUTIRRIC ACID IN MICROCAPSULATED FORM, INTENDED FOR ANIMAL OR HUMAN POWER |
| NL2004557C2 (en) * | 2010-04-15 | 2011-10-18 | Sanluc Internat Nv | COMPOSITION FOR ANIMAL FEED INCLUDING A BUTYRATE SALT. |
| CN103609866A (en) * | 2013-12-04 | 2014-03-05 | 上海美农生物科技股份有限公司 | Micro-capsule type butyrate preparation method |
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