CN102728079A - Drying method of water-soluble low molecular weight chitosan - Google Patents
Drying method of water-soluble low molecular weight chitosan Download PDFInfo
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- CN102728079A CN102728079A CN201210207226XA CN201210207226A CN102728079A CN 102728079 A CN102728079 A CN 102728079A CN 201210207226X A CN201210207226X A CN 201210207226XA CN 201210207226 A CN201210207226 A CN 201210207226A CN 102728079 A CN102728079 A CN 102728079A
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- soluble low
- weight chitosan
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Abstract
The invention relates to a drying method of chitosan, and concretely relates to a drying method of water-soluble low molecular weight chitosan. The provided drying method of the water-soluble low molecular weight chitosan has the advantages of high drying efficiency, high stability, simple operation and the like, and allows drying equipment cleaning to be convenient. An auxiliary material is added to an aqueous solution of the water-soluble low molecular weight chitosan, is dissolved, and is dried through using a centrifuge spray drier, wherein the mass percentage of the aqueous solution of the water-soluble low molecular weight chitosan is 10-30%; the addition amount of the auxiliary material is 0.1-1% of the solid mass of the water-soluble low molecular weight chitosan; and the auxiliary material is one selected from starch, a gelatin, polyvinylpyrrolidone, Arabic gum powder, beta-cyclodextrin, methyl cellulose, hydroxyethylmethyl cellulose, hydroxyethyl cellulose and the like.
Description
Technical field
The present invention relates to a kind of drying means of shitosan, especially relate to a kind of drying means of water-soluble low molecular weight chitosan.
Background technology
The molecular weight of water-soluble low molecular weight chitosan is generally 2000～6000, and is water-soluble strong, is absorbed and used easily, shows the physiologically active and the functional character of many uniquenesses, for example activation and proliferation Bifidobacterium in human body intestinal canal; Improve the macrophage phagocytic ability; Promote the growth of spleen antibody, suppress growth of tumour cell; Bring high blood pressure down, blood sugar, blood fat, the absorption cholesterol; In microenvironment, have the strong bacteriostasis and the wettability power etc. of significantly preserving moisture.
At present, the drying means of water-soluble low molecular weight chitosan mainly contains freeze-drying, organic solvent precipitation method and spray drying process etc.Freeze drying efficient is low, and cost is higher, but can access high-quality product; Organic solvent precipitation method is to utilize organic solvent that the low-molecular weight chitoglycan product is precipitated out, and carries out drying under reduced pressure again, use a large amount of organic solvents, and efficient is low, pollutes greatly, and energy consumption is big, and yield is also lower; Spray drying process has that drying cost is low, the drying efficiency advantages of higher, is drying means the most frequently used in the present large-scale production, can reach low-molecular weight chitoglycan quick-drying requirement in batches.But existing low-molecular weight chitoglycan spray drying process mainly adopts direct drying method; All adopt like Chinese patent 200710053139.2,200810154871.3 and directly solution to be carried out spray-dired method and carry out drying; The shortcoming of this drying means is the low-molecular weight chitoglycan easy oxidizing brown stain of spraying under the hot conditions; Generally to be controlled at and collect powder in the 20min, prolong the collection powder time interval, cause reducing drying efficiency otherwise can only take to reduce baking temperature.Simultaneously, the powder-product flowability that obtains is relatively poor.In addition, spray-dired powder-product sticks easily on the wall of spray dryer, then forms gel behind the chance water, stops powder further to dissolve, and has a strong impact on equipment cleaning efficient.Because above shortcoming, cause present low-molecular weight chitoglycan manufacturing enterprise majority still to adopt organic dissolving precipitated method to carry out drying, so the dry low-molecular weight chitoglycan of research and utilization spray drying process is for realizing that its large-scale production is of great immediate significance.
Summary of the invention
The object of the present invention is to provide a kind ofly have not only that drying efficiency is higher, stability better, simple operation and other advantages, and the drying means of the water-soluble low molecular weight chitosan of convenient and dry equipment cleaning.
Concrete steps of the present invention are following:
In the water-soluble low molecular weight chitosan aqueous solution, add auxiliary material, utilize drying machine with centrifugal spray to carry out drying after the dissolving.
The quality percentage composition of the said water-soluble low molecular weight chitosan aqueous solution can be 10%～30%; The addition of said auxiliary material can be 0.1%～1% of water-soluble low molecular weight chitosan solid masses; Said auxiliary material can be selected from a kind of in starch, gelatin, polyvinylpyrrolidone, gum arabic powder, beta cyclodextrin, methylcellulose, HEMC, the hydroxyethylcellulose etc.; Said dissolving can adopt mechanical agitator to be stirred to dissolving fully; The EAT of the spray drying tower of said drying machine with centrifugal spray can be 160～200 ℃, and outlet temperature can be 60～90 ℃, and hot air flow can be 70%～100% (about 3220～4600m
3/ L), the peristaltic pump flow can be 10～25L/h; Said drying machine with centrifugal spray is LT-50 type drying machine with centrifugal spray (can available from Wuxi Li Yida drying equipment Manufacturing Co., Ltd).
The present invention utilizes the interpolation high polymer adjuvant to carry out mode spray-drying low-molecular-weight (molecular weight is generally 3000～6000) chitosan aqueous solution that the film on the molecular level encapsulates, and with respect to direct spray-dired technology, the present invention has the following advantages:
1) the present invention encapsulates through the film that the interpolation high polymer adjuvant carries out on the molecular level, high efficiency rapid draing water-soluble low molecular weight chitosan, and the product flowability of the present invention's preparation improves greatly, helps the exploitation of product formulation.
2) powder-product is difficult for glutinous wall, and spray drying device cleans easily.
3) dissolution velocity of product is faster, is easy to absorb.
4) can under higher EAT, carry out drying, the feed liquid flow increases, and spray-dired efficient significantly improves.
5) acquisition time of product powder prolongs more than 2 times at interval, reduces spray-drying personnel's working strength.
6) heat resistance of product improves, and makes product more stable, is easy to preserve, and has solved water-soluble low molecular weight chitosan quick-drying technical barrier in batches.
The specific embodiment
Following examples will be further described the present invention.
Embodiment 1
Get the quality percentage composition and be 10% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.2%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 160 ℃, and outlet temperature is 60 ℃, hot air flow 70% (about 3220m
3/ L), peristaltic pump flow 10L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 10～13kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 2
Get the quality percentage composition and be 12% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.5%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 180 ℃, and outlet temperature is 75 ℃, hot air flow 85% (about 3910m
3/ L), peristaltic pump flow 11L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 10～13kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 3
Get the quality percentage composition and be 15% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.7%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 200 ℃, and outlet temperature is 90 ℃, hot air flow 100% (about 4600m
3/ L), peristaltic pump flow 12L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 10～13kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 4
Get the quality percentage composition and be 18% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.3%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 170 ℃, and outlet temperature is 65 ℃, hot air flow 72% (about 3312m
3/ L), peristaltic pump flow 16L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can dry 20～22kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 5
Get the quality percentage composition and be 20% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.1%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 180 ℃, and outlet temperature is 75 ℃, hot air flow 88% (about 4048m
3/ L), peristaltic pump flow 16L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 20～22kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 6
Get the quality percentage composition and be 23% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 1%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 200 ℃, and outlet temperature is 90 ℃, hot air flow 90% (about 4140m
3/ L), peristaltic pump flow 17L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 20～22kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 7
Get the quality percentage composition and be 25% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.8%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 160 ℃, and outlet temperature is 60 ℃, hot air flow 95% (about 4370m
3/ L), peristaltic pump flow 20L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 38～42kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 8
Get the quality percentage composition and be 28% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.4%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 175 ℃, and outlet temperature is 70 ℃, hot air flow 98% (about 4508m
3/ L), peristaltic pump flow 23L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 38～42kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 9
Get the quality percentage composition and be 30% low-molecular weight chitoglycan solution, add the polyvinylpyrrolidone with respect to water-soluble low molecular weight chitosan solid masses 0.6%, the mechanical agitator vigorous stirring utilizes LT-50 type spray dryer dry to dissolving fully.The setup parameter of spray dryer is following: the drying tower EAT is 190 ℃, and outlet temperature is 85 ℃, hot air flow 100% (about 4600m
3/ L), peristaltic pump flow 25L/h.
The gained spray-dried powders utilizes the fixed funnel method to measure angle of repose α: 30～36 °, 1h can the dry low-molecular weight chitoglycan aqueous solution 38～42kg, and sample can effectively be preserved 2 years under shady and cool drying condition at least.
Embodiment 10
Change the auxiliary material polyvinylpyrrolidone in the foregoing description in starch, gelatin, gum arabic powder, beta cyclodextrin, methylcellulose, HEMC, the hydroxyethylcellulose a kind of, all the other operations, technological parameter and result are identical with the foregoing description 1～9.
Claims (7)
1. the drying means of water-soluble low molecular weight chitosan is characterized in that its concrete steps are following:
In the water-soluble low molecular weight chitosan aqueous solution, add auxiliary material, utilize drying machine with centrifugal spray to carry out drying after the dissolving.
2. the drying means of water-soluble low molecular weight chitosan as claimed in claim 1, the quality percentage composition that it is characterized in that the said water-soluble low molecular weight chitosan aqueous solution is 10%～30%.
3. the drying means of water-soluble low molecular weight chitosan as claimed in claim 1, the addition that it is characterized in that said auxiliary material is 0.1%～1% of a water-soluble low molecular weight chitosan solid masses.
4. the drying means of water-soluble low molecular weight chitosan as claimed in claim 1 is characterized in that said auxiliary material is selected from a kind of in starch, gelatin, polyvinylpyrrolidone, gum arabic powder, beta cyclodextrin, methylcellulose, HEMC, the hydroxyethylcellulose.
5. the drying means of water-soluble low molecular weight chitosan as claimed in claim 1 is characterized in that said dissolving is to adopt mechanical agitator to be stirred to dissolving fully.
6. the drying means of water-soluble low molecular weight chitosan as claimed in claim 1, the EAT that it is characterized in that the spray drying tower of said drying machine with centrifugal spray is 160～200 ℃, outlet temperature is 60～90 ℃.
7. the drying means of water-soluble low molecular weight chitosan as claimed in claim 1, the hot air flow that it is characterized in that the spray drying tower of said drying machine with centrifugal spray is 70%～100%, the peristaltic pump flow is 10～25L/h.
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| CN201210207226XA CN102728079A (en) | 2012-06-21 | 2012-06-21 | Drying method of water-soluble low molecular weight chitosan |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6320302A (en) * | 1986-07-11 | 1988-01-28 | Dainichi Color & Chem Mfg Co Ltd | Production of chitosan particle |
| CN1689557A (en) * | 2004-04-23 | 2005-11-02 | 中国科学院过程工程研究所 | Method for preparing hollow minisphere for lung administration |
| CN1748550A (en) * | 2004-09-14 | 2006-03-22 | 重庆市畜牧科学研究院 | Multifunctional new feed additive of Chinese herbal medicine for pig |
| CN101732259A (en) * | 2009-12-29 | 2010-06-16 | 广东药学院 | Chitosan micron particle as well as preparation method and application thereof |
| CN102010512A (en) * | 2010-10-12 | 2011-04-13 | 广东药学院 | Preparation method and application of water-soluble chitosan micro-particles |
-
2012
- 2012-06-21 CN CN201210207226XA patent/CN102728079A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6320302A (en) * | 1986-07-11 | 1988-01-28 | Dainichi Color & Chem Mfg Co Ltd | Production of chitosan particle |
| CN1689557A (en) * | 2004-04-23 | 2005-11-02 | 中国科学院过程工程研究所 | Method for preparing hollow minisphere for lung administration |
| CN1748550A (en) * | 2004-09-14 | 2006-03-22 | 重庆市畜牧科学研究院 | Multifunctional new feed additive of Chinese herbal medicine for pig |
| CN101732259A (en) * | 2009-12-29 | 2010-06-16 | 广东药学院 | Chitosan micron particle as well as preparation method and application thereof |
| CN102010512A (en) * | 2010-10-12 | 2011-04-13 | 广东药学院 | Preparation method and application of water-soluble chitosan micro-particles |
Non-Patent Citations (1)
| Title |
|---|
| 韩磊等: "含糖类物料的喷雾干燥", 《林产化学与工业》 * |
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Application publication date: 20121017 |