JP4140741B2 - Method for producing dry chitin powder or dry chitosan powder - Google Patents
Method for producing dry chitin powder or dry chitosan powder Download PDFInfo
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- JP4140741B2 JP4140741B2 JP18130298A JP18130298A JP4140741B2 JP 4140741 B2 JP4140741 B2 JP 4140741B2 JP 18130298 A JP18130298 A JP 18130298A JP 18130298 A JP18130298 A JP 18130298A JP 4140741 B2 JP4140741 B2 JP 4140741B2
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- Prior art keywords
- powder
- chitosan
- chitin
- dry
- dried
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Description
【0001】
【発明の属する技術分野】
キチンはキトサン製造用及び関節炎治療剤として期待されているグルコサミン製造用等の原料として使用され、又、皮膚の損傷保護剤として使用される極めて重要な物質である。キトサンは水質浄化用の凝集剤として使用され、近年では、難消化性により食物繊維の効果が期待され、中でも多くのアミノ基をもつことにより、消化管内で胆汁酸を吸着し、血清コレステロ−ル低下作用を示すことから、今後、キトサンは降コレステロ−ル作用を活用した機能性食品への応用が期待されている。又、生分解性ポリマー、ダイエット補助食品等への開発が進められている。本発明は乾燥キチン粉末又は乾燥キトサン粉末の製造方法に関する。
【0002】
【従来の技術】
粉末キチン又は粉末キトサンは従来、例えば、カニ、エビ又はシャコ等の甲皮等又はイカの軟骨を脱蛋白処理、脱カルシウム処理した後、必要により脱アセチル化し、水洗して乾燥した後に粗粉砕し、更に粉砕機で粉砕して粉末キチン及び粉末キトサンを得ていた。
【0003】
【発明が解決しようとする課題】
しかし、含水キチン又は含水キトサンを含水率10%以下の乾燥キチン又は乾燥キトサンにするには乾燥機が必要であり、又、かなりの乾燥時間が必要であった。更に、乾燥物の粉砕による物性劣化が激しく、物性劣化の低減が求められていた。
【0004】
このように、乾燥キチン粉末又は乾燥キトサン粉末を得るためには、膨大な製造設備と多大な製造時間が必要であり、乾燥キチン粉末又は乾燥キトサン粉末の安価で生産効率のよい製造方法が望まれていた。
【0005】
【課題を解決するための手段】
そこで本発明者らは種々検討した結果、難粉砕性のキチン又はキトサンを乾燥しないで含水状態のキチン又はキトサンを直接粉砕機に投入して粉砕することで、含水率10%以下に乾燥されたキチン粉末又はキトサン粉末が得られることを見い出した。更に、含水状態で粉砕することで粉砕による物性劣化が縮小することを見い出した。その結果、乾燥設備が不用となり乾燥のみを行う工程が無くなるため、安価で高効率の製造方法となった。本発明は上記知見に基づいて完成されたものである。
【0006】
即ち、本発明は、
(1) 粉砕前の含水率が20〜80%であり、且つ平均粒子径が300μm〜1cmである含水キチン又は含水キトサンを粉砕機で粉砕して、粉砕機で粉砕すると同時に乾燥を行うことで平均粒子径30〜200μmの乾燥キチン粉末又は乾燥キトサン粉末を得ることを特徴とする乾燥キチン粉末又は乾燥キトサン粉末の製造方法、
(2) 含水キチン又は含水キトサンを粉砕する粉砕機が気流式のジェットミルである(1)に記載の方法、
(3) 粉砕後の乾燥キチン粉末又は乾燥キトサン粉末の含水率が10%以下である(1)又は(2)に記載の方法、
に関する。
【0007】
本発明においてキチンは、通常、例えば、カニ、エビ等の甲殻類の甲皮等を原料とし、それを希アルカリ又は酵素で脱蛋白し、さらに希酸で脱カルシウムして灰分を取り除き、反応終了後、数回水洗することによって得られるが、特にこの方法に限定されない。含水キチンは、例えば、前述の方法により水洗して得られた含水物でもよいし、又、乾燥したものに水を加えて含水させたものでもよい。キトサンは、例えば、キチンを水酸化ナトリウム、水酸化カリウム等の強アルカリ剤中で脱アセチル化した後、数回水洗することによって得られるが、特にこの方法に限定されない。含水キトサンは、例えば、前述の方法により水洗して得られた含水物でもよいし、又、乾燥したものに水を加えて含水させたものでもよい。
【0008】
本発明の粉砕機は、特に限定されず、例えば大量の空気の使用を伴う粉砕機を用いて含水粉砕するのが好ましく、特に気流式ジェットミルが良い。粉砕前の含水キチン又は含水キトサンの含水率は、通常、20〜80%の範囲が好ましく、製造時に水洗して得られる50〜70%の含水キチン又は含水キトサンが特に好ましい。粉砕前の含水キチン又は含水キトサンの平均粒子径は、300μm以上、1cm以下が好ましく、特に好ましくは1〜5mm程度である。粉砕後の乾燥キチン粉末又は乾燥キトサン粉末の含水率は、10%以下が好ましく、特に好ましくは0.5〜5%である。粉砕後の乾燥キチン粉末又は乾燥キトサン粉末の平均粒子径は、300μm以下が好ましく、より好ましくは30〜200μmであり、特に好ましくは、50〜120μmである。粉砕による物性劣化は、通常、乾燥物での気流式ジェットミル粉砕前後の粘度保持率は15〜35%程度であるが、含水状態(例えば、含水キチン又は含水キトサンの含水率が20〜80%)での気流式ジェットミル粉砕前後の粘度保持率は25〜45%に向上して物性劣化が小さくなる。
【0009】
【発明の効果】
本発明は、含水キチン又は含水キトサンを粉砕機で粉砕して、乾燥工程を別途に設けることなく、高品質の乾燥キチン粉末又は乾燥キトサン粉末を得る極めて有効な製造方法である。
【0010】
【実施例】
以下に実施例を挙げて本発明を具体的に説明するが、本発明はこれらに限定されるものではない。
実施例1
乾燥物の粘度が780mPa・s、脱アセチル化度97%、平均粒子径2.5mm、含水率が4.3%、22.2%、44.5%、56.0%、77.0%の5つのキトサンを用い、気流式ジェットミル((株)躍進機械製作所、KV−15型)で粉砕し乾燥キトサン粉末を得た。乾燥キトサン粉末の粘度、平均粒子径、含水率、脱アセチル化度を表1に示す。
【0011】
【表1】
粉砕前含水率 粘 度 平均粒子径 含水率 脱アセチル化度
(%) (mPa・s) (μm) (%) (%)
4.3 230 180 6.2 96.0
22.2 260 180 6.9 97.0
44.5 280 180 6.8 97.0
56.0 270 170 7.6 97.0
77.0 250 170 7.9 96.0
【0012】
実施例2
乾燥物の粘度が780mPa・s、脱アセチル化度97%、平均粒子径2.5mm、含水率が4.3%、22.2%、44.5%、56.0%、77.0%の5つのキトサンを用い、気流式ジェットミル(ホソカワミクロン(株)、ACM−10型)で粉砕し乾燥キトサン粉末を得た。乾燥キトサン粉末の粘度、平均粒子径、含水率、脱アセチル化度を表2に示す。
【0013】
【表2】
粉砕前含水率 粘 度 平均粒子径 含水率 脱アセチル化度
(%) (mPa・s) (μm) (%) (%)
4.3 180 160 5.5 97.0
22.2 225 150 5.9 97.0
44.5 208 150 5.4 97.0
56.0 211 140 6.8 97.0
77.0 204 140 7.8 97.0
【0014】
実施例3
乾燥物の粘度が1200mPa・s、平均粒子径3.5mm、含水率が5.0%、50.0%の2つのキチンを用い、気流式ジェットミル(ホソカワミクロン(株)、ウルトラプレックス)で粉砕して乾燥キチン粉末を得た。乾燥キチン粉末の粘度、平均粒子径、含水率、を表3に示す。
【0015】
【表3】
粉砕前含水率 粘 度 平均粒子径 含水率
(%) (mPa・s) (μm) (%)
5.0 380 140 5.8
50.0 430 130 6.0
【0016】
粘度の測定値は、キチン10gに48%苛性ソーダ200mlを加え、95℃で3時間反応して得られたキトサンの粘度である。
【0017】
実施例4
乾燥物の粘度が310mPa・s、脱アセチル化度92%、平均粒子径3.2mm、含水率が6%、60%の2つのキトサンを用い、気流式ジェットミル(ホソカワミクロン(株)、ACM−10型)で粉砕し、180μmの網で篩過して乾燥キトサン粉末を得た。乾燥キトサン粉末の粘度、平均粒子径、含水率、脱アセチル化度を表4に示す。
【0018】
【表4】
粉砕前含水率 粘 度 平均粒子径 含水率 脱アセチル化度
(%) (mPa・s) (μm) (%) (%)
6.0 120 140 3.5 92.0
60.0 140 120 3.4 92.0[0001]
BACKGROUND OF THE INVENTION
Chitin is an extremely important substance that is used as a raw material for the production of chitosan and for the production of glucosamine, which is expected as an agent for treating arthritis. Chitosan is used as a flocculant for water purification, and in recent years, it is expected to have an effect of dietary fiber due to indigestibility, and by having many amino groups, it absorbs bile acids in the digestive tract, and serum cholesterol Since it shows a lowering action, chitosan is expected to be applied to functional foods utilizing the cholesterol action. Development into biodegradable polymers, dietary supplements, and the like is underway. The present invention relates to a method for producing dry chitin powder or dry chitosan powder.
[0002]
[Prior art]
Conventionally, powder chitin or powder chitosan is, for example, deproteinized and decalcified from shells of crabs, shrimp or shrimp, etc. or squid cartilage, deacetylated as necessary, washed with water, dried and then coarsely crushed. Further, it was pulverized by a pulverizer to obtain powdered chitin and powdered chitosan.
[0003]
[Problems to be solved by the invention]
However, a drier is required to convert hydrous chitin or hydrous chitosan into dry chitin or dry chitosan having a water content of 10% or less, and a considerable drying time is required. Furthermore, physical property deterioration due to pulverization of the dried product is severe, and reduction of physical property deterioration has been demanded.
[0004]
Thus, in order to obtain dry chitin powder or dry chitosan powder, enormous production equipment and a great deal of production time are required, and a cheap and efficient production method for dry chitin powder or dry chitosan powder is desired. It was.
[0005]
[Means for Solving the Problems]
Therefore, as a result of various investigations, the present inventors have dried the water content to 10% or less by directly putting the water-containing chitin or chitosan into the pulverizer without crushing the difficult-to-grind chitin or chitosan. It has been found that chitin powder or chitosan powder can be obtained. Furthermore, it has been found that deterioration in physical properties due to pulverization is reduced by pulverization in a water-containing state. As a result, since the drying equipment is not required and there is no step of performing only drying, the manufacturing method is inexpensive and highly efficient. The present invention has been completed based on the above findings.
[0006]
That is, the present invention
(1) By pulverizing hydrous chitin or hydrous chitosan having a water content of 20 to 80% before pulverization and an average particle diameter of 300 μm to 1 cm with a pulverizer, pulverizing with a pulverizer and simultaneously drying. A method for producing a dried chitin powder or a dried chitosan powder, characterized in that the dried chitin powder or dried chitosan powder having an average particle size of 30 to 200 μm is obtained;
(2) The method according to (1), wherein the pulverizer for pulverizing hydrous chitin or hydrous chitosan is an air-jet jet mill,
(3) The method according to (1) or (2), wherein the moisture content of the dried chitin powder or the dried chitosan powder after pulverization is 10% or less,
About.
[0007]
In the present invention, chitin is usually obtained from, for example, crustacean crusts such as crabs and shrimps, deproteinized with dilute alkali or enzyme, further decalcified with dilute acid to remove ash, and the reaction is completed. Thereafter, it is obtained by washing with water several times, but is not particularly limited to this method. The hydrated chitin may be, for example, a hydrated product obtained by washing with water by the method described above, or may be a hydrated product obtained by adding water to a dried product. Chitosan can be obtained, for example, by deacetylating chitin in a strong alkali agent such as sodium hydroxide or potassium hydroxide and then washing with water several times, but is not particularly limited to this method. The hydrated chitosan may be, for example, a hydrated product obtained by washing with water by the method described above, or may be a product obtained by adding water to a dried product.
[0008]
The pulverizer of the present invention is not particularly limited, and for example, it is preferable to perform hydrous pulverization using a pulverizer that involves the use of a large amount of air, and an airflow jet mill is particularly preferable. The water content of the water-containing chitin or water-containing chitosan before pulverization is usually preferably in the range of 20 to 80%, particularly preferably 50 to 70% of water-containing chitin or water-containing chitosan obtained by washing with water during production. The average particle size of hydrous chitin or hydrous chitosan before pulverization is preferably 300 μm or more and 1 cm or less, and particularly preferably about 1 to 5 mm. The moisture content of the dried chitin powder or dried chitosan powder after pulverization is preferably 10% or less, particularly preferably 0.5 to 5%. The average particle size of the dried chitin powder or dried chitosan powder after pulverization is preferably 300 μm or less, more preferably 30 to 200 μm, and particularly preferably 50 to 120 μm. The deterioration of physical properties due to pulverization is usually about 15 to 35% of the viscosity retention before and after airflow jet mill pulverization with a dry product, but the water content (for example, the water content of hydrated chitin or hydrated chitosan is 20 to 80%). ), The viscosity retention before and after the airflow jet mill pulverization is improved to 25 to 45%, and the deterioration of physical properties is reduced.
[0009]
【The invention's effect】
The present invention is a very effective production method for obtaining high-quality dry chitin powder or dry chitosan powder without pulverizing hydrous chitin or hydrous chitosan with a pulverizer and providing a separate drying step.
[0010]
【Example】
EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples.
Example 1
The dried product has a viscosity of 780 mPa · s, a deacetylation degree of 97%, an average particle size of 2.5 mm, and a moisture content of 4.3%, 22.2%, 44.5%, 56.0%, and 77.0%. The dry chitosan powder was obtained by pulverizing with an air-flow jet mill (Rikishin Machine Seisakusho, KV-15 type). Table 1 shows the viscosity, average particle diameter, water content, and degree of deacetylation of the dried chitosan powder.
[0011]
[Table 1]
Water content before grinding Viscosity Average particle size Water content Deacetylation degree
(%) (MPa · s) (μm) (%) (%)
4.3 230 180 6.2 96.0
22.2 260 180 6.9 97.0
44.5 280 180 6.8 97.0
56.0 270 170 7.6 97.0
77.0 250 170 7.9 96.0
[0012]
Example 2
The dried product has a viscosity of 780 mPa · s, a deacetylation degree of 97%, an average particle size of 2.5 mm, and a moisture content of 4.3%, 22.2%, 44.5%, 56.0%, and 77.0%. The dry chitosan powder was obtained by pulverizing with an airflow jet mill (Hosokawa Micron Co., Ltd., ACM-10 type). Table 2 shows the viscosity, average particle diameter, water content, and degree of deacetylation of the dried chitosan powder.
[0013]
[Table 2]
Water content before grinding Viscosity Average particle size Water content Deacetylation degree
(%) (MPa · s) (μm) (%) (%)
4.3 180 160 5.5 97.0
22.2 225 150 5.9 97.0
44.5 208 150 5.4 97.0
56.0 211 140 6.8 97.0
77.0 204 140 7.8 97.0
[0014]
Example 3
Grinded with an air-jet jet mill (Hosokawa Micron Corporation, Ultraplex) using two chitins with a dried product viscosity of 1200 mPa · s, an average particle size of 3.5 mm, and a moisture content of 5.0% and 50.0%. As a result, dry chitin powder was obtained. Table 3 shows the viscosity, average particle diameter, and water content of the dried chitin powder.
[0015]
[Table 3]
Water content before grinding Viscosity Average particle size Water content
(%) (MPa · s) (μm) (%)
5.0 380 140 5.8
50.0 430 130 6.0
[0016]
The measured value of the viscosity is the viscosity of chitosan obtained by adding 200 ml of 48% caustic soda to 10 g of chitin and reacting at 95 ° C. for 3 hours.
[0017]
Example 4
Using two chitosans having a dried product viscosity of 310 mPa · s, a degree of deacetylation of 92%, an average particle size of 3.2 mm, a moisture content of 6% and 60%, an air-jet jet mill (Hosokawa Micron Co., Ltd., ACM- 10 type) and sieved through a 180 μm net to obtain dry chitosan powder. Table 4 shows the viscosity, average particle diameter, water content, and degree of deacetylation of the dried chitosan powder.
[0018]
[Table 4]
Water content before grinding Viscosity Average particle size Water content Deacetylation degree
(%) (MPa · s) (μm) (%) (%)
6.0 120 140 3.5 92.0
60.0 140 120 3.4 92.0
Claims (3)
Priority Applications (1)
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JP18130298A JP4140741B2 (en) | 1998-06-29 | 1998-06-29 | Method for producing dry chitin powder or dry chitosan powder |
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JP18130298A JP4140741B2 (en) | 1998-06-29 | 1998-06-29 | Method for producing dry chitin powder or dry chitosan powder |
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JP2000007706A JP2000007706A (en) | 2000-01-11 |
JP4140741B2 true JP4140741B2 (en) | 2008-08-27 |
Family
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JP18130298A Expired - Fee Related JP4140741B2 (en) | 1998-06-29 | 1998-06-29 | Method for producing dry chitin powder or dry chitosan powder |
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CN107266598A (en) * | 2017-05-17 | 2017-10-20 | 宁波拜尔玛生物科技有限公司 | The functional sugar prepared based on nanometer technology and its application in field of medicaments |
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JP5069405B2 (en) * | 2005-06-23 | 2012-11-07 | 大日精化工業株式会社 | Method for producing fine particle chitin |
JP4976662B2 (en) * | 2005-06-24 | 2012-07-18 | 大日精化工業株式会社 | Chitosan fine particles |
CN106432540B (en) * | 2016-09-13 | 2019-05-14 | 浙江大学 | A kind of preparation method of chitin micro mist |
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Cited By (2)
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CN107266598A (en) * | 2017-05-17 | 2017-10-20 | 宁波拜尔玛生物科技有限公司 | The functional sugar prepared based on nanometer technology and its application in field of medicaments |
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