JPS6317902A - Production of chitosan granule - Google Patents
Production of chitosan granuleInfo
- Publication number
- JPS6317902A JPS6317902A JP16093086A JP16093086A JPS6317902A JP S6317902 A JPS6317902 A JP S6317902A JP 16093086 A JP16093086 A JP 16093086A JP 16093086 A JP16093086 A JP 16093086A JP S6317902 A JPS6317902 A JP S6317902A
- Authority
- JP
- Japan
- Prior art keywords
- chitosan
- concentration
- aqueous solution
- acid
- granules
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 93
- 239000008187 granular material Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000002245 particle Substances 0.000 claims abstract description 46
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- 238000001694 spray drying Methods 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003463 adsorbent Substances 0.000 abstract description 6
- 238000004587 chromatography analysis Methods 0.000 abstract description 2
- 238000002347 injection Methods 0.000 abstract description 2
- 239000007924 injection Substances 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 2
- 239000003937 drug carrier Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 230000006196 deacetylation Effects 0.000 description 7
- 238000003381 deacetylation reaction Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000011260 aqueous acid Substances 0.000 description 5
- 239000000969 carrier Substances 0.000 description 5
- 239000011859 microparticle Substances 0.000 description 5
- 239000012736 aqueous medium Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000010253 intravenous injection Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- 241000238557 Decapoda Species 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 230000000850 deacetylating effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229940127554 medical product Drugs 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 241000238424 Crustacea Species 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 230000003308 immunostimulating effect Effects 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
Landscapes
- Medicinal Preparation (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はキトサン粒体の製造方法に関し、更に詳しくは
、医療品担体、注射薬材料、クロマトグラフィー用吸着
材、バイオリアクタ担体等として有用な種々の粒径の高
純度キトサン粒体の提供を目的とする。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for producing chitosan granules, more specifically, chitosan particles useful as carriers for medical products, materials for injections, adsorbents for chromatography, carriers for bioreactors, etc. The purpose is to provide high purity chitosan particles of various particle sizes.
（従来の技術）
従来、キチンを脱アセチル化して得られるキトサンは公
知であり、そのユニークな性質からして各種の吸着材、
医療品担体、医療材料としての研究が行なわれている。(Prior art) Chitosan, which is obtained by deacetylating chitin, has been known, and due to its unique properties, it has been used as a variety of adsorbents,
Research is being conducted on its use as a carrier for medical products and as a medical material.
例えば、各種担体として利用する場合には、キトサンを
粒状化する技術が重要であり、このような粒状化技術と
しては、キトサンが酸の水溶液に可溶であり、アルカリ
によって凝固するという性質を利用して、キトサンの水
溶液を調製し、これをアルカリにより中和して粒状化す
る技術が最も多く提案されている。For example, when using chitosan as a variety of carriers, it is important to have a technology to granulate chitosan, and this granulation technology takes advantage of the property that chitosan is soluble in aqueous acid solutions and solidified by alkali. The most commonly proposed technique is to prepare an aqueous solution of chitosan, neutralize it with an alkali, and granulate it.
これらの粒状化方法によれば、平均粒径が数ｍｍから数
１００μｍ程度の粒状キトサンが提供される。According to these granulation methods, granular chitosan having an average particle size of about several mm to several 100 μm is provided.
（発明が解決しようとしている問題点）上記の公知の方
法は、いずれも水性媒体中において、キトサンの凝固を
行うものであり、比較的平均粒径の大なる粒状キトサン
は得られるものの、例えば、数１０μｍ程度のキトサン
粒体を得るのは非常に困難であり、更に数μｍ程度のキ
トサン粒体な得ることはできない。これは、キトサンの
粒状化を水性媒体中で行う結果、キトサン粒子が微小で
あるとそれらが水性媒体中で凝集を生じ易いこと、およ
び、このような微小な状態で凝集を生じることなく乾燥
するのは極めて困難なためである。(Problems to be Solved by the Invention) The above-mentioned known methods all involve coagulating chitosan in an aqueous medium, and although granular chitosan with a relatively large average particle size can be obtained, for example, It is very difficult to obtain chitosan particles with a size of about several tens of micrometers, and it is even impossible to obtain chitosan particles with a size of about several micrometers. This is because chitosan is granulated in an aqueous medium, and if the chitosan particles are minute, they tend to aggregate in the aqueous medium, and it is difficult to dry them in such a minute state without causing aggregation. This is because it is extremely difficult.
また、従来方法の場合には、水性媒体中における凝固方
法を使用する結果、操作が煩雑で且つ条件設定が困難で
あるため、一定の粒度および品質の粒体を得るのが困難
であった。更に、キトサンの粒状化に際しては、アルカ
リ等の凝固剤、界面活性剤等の懸濁剤等が必要であるた
め、これらの各種補助剤が、得られるキトサン粒体中に
混入し、不純物を含んだキトサン粒体となるという問題
がある。この問題は、キトサン粒体を医療分野で使用し
ようとする時には非常に重要であり、従来方法によるキ
トサン粒体は殆ど医療分野では利用することができなか
った。Further, in the case of the conventional method, as a result of using a coagulation method in an aqueous medium, the operation is complicated and the setting of conditions is difficult, so it is difficult to obtain granules with a constant particle size and quality. Furthermore, when granulating chitosan, coagulating agents such as alkalis and suspending agents such as surfactants are required, so these various auxiliary agents are mixed into the resulting chitosan granules and are free from impurities. However, there is a problem that it becomes chitosan granules. This problem is very important when trying to use chitosan granules in the medical field, and chitosan granules produced by conventional methods could hardly be used in the medical field.
また、最近では、キトサンが免疫活性効果があること、
また生理活性物の徐放性担体としての利用可能性等が報
告されているが、このような用途においては、キトサン
の平均粒径はμｍオーダーであること、および不純物を
含有しないことが要求されるため、従来技術によるキト
サン粒体は殆ど利用可能性が見い出し得ないものであっ
た。In addition, recently, chitosan has been shown to have an immunostimulating effect.
In addition, it has been reported that chitosan can be used as a sustained release carrier for physiologically active substances, but for such uses, chitosan is required to have an average particle size on the μm order and to be free of impurities. Therefore, chitosan granules according to the prior art could hardly be used.
従って、その平均粒径が１０μｍ以下のものから任意の
平均粒径の球状のキトサン粒体を提供できる方法が強く
要望されている。Therefore, there is a strong demand for a method that can provide spherical chitosan particles having an arbitrary average particle size of 10 μm or less.
（問題点を解決するための手段）
本発明者は上記の如き従来技術の問題点を解決し、上記
の要望に応えるべく鋭意研究の結果、本発明を完成した
。(Means for Solving the Problems) The present inventor has completed the present invention as a result of intensive research to solve the problems of the prior art as described above and to meet the above demands.
すなわち、本発明は、キトサンの酸水溶液をアンモニア
雰囲気中で噴霧乾燥することを特徴とするキトサン粒体
の製造方法である。That is, the present invention is a method for producing chitosan granules, which comprises spray-drying an acid aqueous solution of chitosan in an ammonia atmosphere.
次に本発明を更に詳細に説明する。本発明者は従来から
キトサンの粒状化について鋭意研究のところ、キトサン
を酸の水溶液に適当な濃度で溶解し、従来技術の如く、
凝固浴中に加えて凝固させるのではなく、得られたキト
サン水溶液を種々の条件で加熱アンモニア雰囲気中に噴
霧して乾燥する、すなわちスプレードライ方式で乾燥す
る時は、噴霧乾燥条件に従って種々の平均粒径のキトサ
ン粒体が極めて容易に得られることを知見したものであ
る。しかも、このようにして得られる種々の平均粒径の
キトサン粒体は、その形状が殆ど角のない球状であり、
しかも、乾燥時固体になるような凝固剤等を使用しない
ため、得られるキトサン粒体は非常に高純度であり、吸
着材等の一般的用途は勿論、平均粒径が１０μｍ以下の
ものは特に医療分野における担体材料等として非常に適
しているものであった。Next, the present invention will be explained in more detail. The present inventor has been conducting extensive research on the granulation of chitosan, and has discovered that chitosan is dissolved in an aqueous acid solution at an appropriate concentration, and as in the prior art,
Instead of adding it to a coagulation bath and coagulating it, the obtained chitosan aqueous solution is dried by spraying it in a heated ammonia atmosphere under various conditions, that is, when drying by spray drying method, various average It was discovered that chitosan particles having the same particle size can be obtained extremely easily. Moreover, the chitosan particles of various average particle sizes obtained in this way are spherical in shape with almost no corners,
Moreover, since no coagulant or the like that becomes solid upon drying is used, the chitosan particles obtained are of extremely high purity, and can be used not only for general purposes such as adsorbents, but also for those with an average particle size of 10 μm or less. It was extremely suitable as a carrier material in the medical field.
以上の如き本発明方法は次の如くして行われ種々の平均
粒径のキトサン粒体が提供される。The method of the present invention as described above is carried out as follows, and chitosan particles having various average particle sizes are provided.
本発明において使用するキトサンとは、カニやエビの甲
殻類の外皮中に存在するキチンを脱アセチル化して得ら
れるものであり、それ自体としては周知の材料であり、
種々の脱アセチル化度、種々の分子量ものが市場から入
手できるし、また容易に製造し得るものである。本発明
において使用するキトサンは、これらの公知のキトサン
中で、酸の水溶液に溶解できるものはいずれの脱アセチ
ル化度でもいずれの分子量のものでも使用できる。The chitosan used in the present invention is obtained by deacetylating chitin present in the outer skin of crustaceans such as crabs and shrimp, and is a well-known material in itself.
Products with various degrees of deacetylation and various molecular weights are commercially available and can be easily produced. The chitosan used in the present invention may have any degree of deacetylation and any molecular weight among these known chitosan as long as it can be dissolved in an aqueous acid solution.
キトサンを溶解するための酸の水溶液は、酢酸、乳酸等
の有機酸および塩酸等の無機酸のいずれの水溶液でもよ
い。The aqueous acid solution for dissolving chitosan may be any aqueous solution of organic acids such as acetic acid and lactic acid, and inorganic acids such as hydrochloric acid.
酸の水溶液の酸濃度は、溶解するキトサンの濃度にもよ
るが、＝一般的には０．１〜１０重量％重量％機度が好
ましく、またキトサンの濃度はいずれの濃度でもよいが
、一般的には０．０５〜２０重量％、好ましくは０．１
〜１０重量％重量％機る。濃度が上記範囲未満であると
経済性が劣り、また上記濃度を越えると、キトサン水溶
液の粘度が高くなり、取扱不便となる。このようなキト
サンの濃度を調製することによって、サブミクロンのも
のから１００μｍオーダーの種々のキトサン粒体を提供
することができる。The acid concentration of the aqueous acid solution depends on the concentration of chitosan to be dissolved, but is generally preferably 0.1 to 10% by weight, and the concentration of chitosan may be any concentration, but generally Generally 0.05 to 20% by weight, preferably 0.1
~10% by weight. If the concentration is less than the above range, the economic efficiency will be poor, and if it exceeds the above concentration, the viscosity of the chitosan aqueous solution will increase, making handling inconvenient. By adjusting the concentration of chitosan in this way, it is possible to provide various chitosan particles ranging from submicron to 100 μm order.
上記のキトサンの水溶液はキトサンの溶解によってｐＨ
は７に近くなるが、更に無害な塩基性物質を加えてｐＨ
を更に７に近づけることによって、−層容易にキトサン
粒体を得ることができる。またキトサンが凝固しない程
度にアルコール等の有機溶剤を添加してもよい。更に、
キトサン水溶液中には予め有用な薬剤、例えば、酵素、
生理活性物質等を適当量添加させておくこともできる。The above chitosan aqueous solution has a pH of
becomes close to 7, but by adding a harmless basic substance, the pH
By making the value even closer to 7, chitosan particles can be easily obtained. Further, an organic solvent such as alcohol may be added to an extent that chitosan does not coagulate. Furthermore,
Useful drugs such as enzymes, enzymes, etc. are added to the chitosan aqueous solution in advance.
A suitable amount of a physiologically active substance or the like may also be added.
本発明で使用する噴霧乾燥方法自体は、アンモニア雰囲
気中行うことを除き公知の方法であり、いずれの公知の
噴霧乾燥装置も有用である。The spray drying method itself used in the present invention is a known method except that it is carried out in an ammonia atmosphere, and any known spray drying apparatus is useful.
このような噴霧乾燥機中で上記の如きキトサンの水溶液
を５０〜１５０℃程度のアンモニア雰囲気中に噴霧する
ことにより、溶液は微細な液滴が凝固するとともに水分
が蒸発し、本発明方法によるキトサン粒体が得られる。By spraying the chitosan aqueous solution as described above into an ammonia atmosphere at a temperature of about 50 to 150°C in such a spray dryer, fine droplets of the solution coagulate and water evaporates, resulting in chitosan produced by the method of the present invention. Granules are obtained.
使用するアンモニア雰囲気は、いずれの濃度でもよいが
、一般的には約１００〜１１００００ｐｐの濃度である
。アンモニア濃度が低すぎると、キトサンの凝固が遅れ
るため、乾燥温度を高めることが必要となり、その結果
、形成されるキトサン粒体が凝集したり、変質したりす
る可能性が生じるので好ましくない。また上記範囲以上
のアンモニア濃度でも経済性を考慮しなければ何等問題
はない。このようにして得られた本発明のキトサン粒体
は、角の殆ど無い球状体であり、その平均粒径は噴霧乾
燥条件に従って１０μｍ以下のものから１００μｍオー
ダーのものである。得られたキトサン粒体には若干酸と
アンモニアからなる塩が残っていることもあるので、更
に水洗して残っている酸を十分に除去してもよく、少量
の塩が残留しても問題のない用途ではそのままでもよい
。The ammonia atmosphere used may have any concentration, but generally has a concentration of about 100 to 110,000 pp. If the ammonia concentration is too low, the coagulation of chitosan will be delayed, making it necessary to increase the drying temperature, and as a result, the formed chitosan particles may aggregate or change in quality, which is not preferable. Further, even if the ammonia concentration exceeds the above range, there is no problem unless economic efficiency is taken into account. The chitosan particles of the present invention thus obtained are spherical bodies with almost no corners, and the average particle size ranges from 10 μm or less to on the order of 100 μm depending on the spray drying conditions. The obtained chitosan granules may have some salts consisting of acid and ammonia remaining, so they may be further washed with water to sufficiently remove the remaining acids, but there is no problem even if a small amount of salt remains. It can be left as is in applications where there is no such thing.
また得られたキトサン粒体は、用途によフてはポリイソ
シアネート、ポリエポキシ化合物等の架橋剤によフて架
橋処理を行い、その耐水性等を高めてもよい。The obtained chitosan particles may also be crosslinked with a crosslinking agent such as polyisocyanate or polyepoxy compound to improve their water resistance etc., depending on the use.
（作用・結果）
以上の如き本発明方法によれば、従来方法では提供でき
なかった球状のキトサン粒体が提供でき、また噴霧乾燥
条件を変化させることによって平均粒径が１０μｍ以下
の微小のものから１００μｍオーダーの粒体が提供でき
る。従って、本発明方法によるキトサン粒体は、従来公
知の平均粒径の犬なキトサン粒子と同様にゲルクロマト
グラフィー、イオン交換クロマトグラフィー等の交換材
、透析材、イオン交換体、バイオリアクタの担体等とし
て有用であることは勿論、従来技術において球状の形状
が要求される用途においても有用である。更に平均粒径
が１０μｍ以下のキトサン微小粒体の場合には、高純度
であることから、従来では使用できなかった医療分野で
の用途、例えば、生理活性物質の担体や静脈注射剤の材
料等としての有用である。(Action/Result) According to the method of the present invention as described above, spherical chitosan particles, which could not be provided by conventional methods, can be provided, and by changing the spray drying conditions, particles with an average particle size of 10 μm or less can be provided. It is possible to provide particles with a size on the order of 100 μm. Therefore, the chitosan particles produced by the method of the present invention can be used as exchange materials for gel chromatography, ion exchange chromatography, etc., dialysis materials, ion exchangers, carriers for bioreactors, etc., as well as conventionally known chitosan particles with a small average particle size. It is of course useful in applications where a spherical shape is required in the prior art. Furthermore, in the case of chitosan microparticles with an average particle size of 10 μm or less, due to their high purity, they can be used in medical fields that could not be used in the past, such as carriers for physiologically active substances and materials for intravenous injections. It is useful as a.
次に実施例を挙げて本発明を更に具体的に説明する。な
お、文中、部または％とあるのは特に断りのない限り重
量基準である。Next, the present invention will be explained in more detail with reference to Examples. In addition, parts and percentages in the text are based on weight unless otherwise specified.
実施例１
１％の酢酸水溶液中に脱アセチル化６３％のキトサン（
分子量約２３万）を０．１％の濃度に溶解してキトサン
の水溶液を調製し、これを入口温度５０℃、噴霧空気圧
１ｋｇ／ｃｒｎ’、送液量１〜２ｍｕ／ｍｉｎ、および
１１０００ＰＰのアンモニア濃度の条件で噴霧乾燥した
。得られたキトサン粒体をエタノール中に分散させ、遠
心分離器により分離し、乾燥して、本発明のキトサン粒
体を得た。Example 1 Deacetylated 63% chitosan (
An aqueous solution of chitosan was prepared by dissolving chitosan (molecular weight approximately 230,000) to a concentration of 0.1%, and this was mixed with ammonia of 11,000 PP at an inlet temperature of 50°C, an atomizing air pressure of 1 kg/crn', a liquid feed rate of 1 to 2 mu/min, and ammonia of 11,000 PP. It was spray-dried under the condition of concentration. The obtained chitosan granules were dispersed in ethanol, separated using a centrifuge, and dried to obtain chitosan granules of the present invention.
このキトサン粒体の１００個を任意に取り出し、顕微鏡
下で観察したところ殆どが真球状であり、平均粒径は２
μｍであった。このキトサン粒体は各種吸着材や静脈注
射剤の材料として有用である。When 100 of these chitosan particles were taken out and observed under a microscope, most of them were perfectly spherical, with an average particle size of 2.
It was μm. These chitosan particles are useful as materials for various adsorbents and intravenous injections.
実施例２〜６
実施例１におけるキトサン、酸および噴霧乾燥条件を下
記第１表の如く変えたことを除いて、他は実施例１と同
様にして本発明のキトサン粒体を得た。これらのキトサ
ン粒体はいずれも各種吸着材や静脈注射剤の材料として
有用である。Examples 2 to 6 Chitosan granules of the present invention were obtained in the same manner as in Example 1, except that the chitosan, acid, and spray drying conditions in Example 1 were changed as shown in Table 1 below. All of these chitosan particles are useful as materials for various adsorbents and intravenous injections.
第１表 ｕμ キトサン：脱アセチル化度８５％ 分子量３万 溶液濃度１０％ 酸： ８％酢酸 噴霧乾燥：入口温度８０℃ 噴霧空気圧１にｇｆ／ｃｎｆ 送液速度１〜２ｍｆｌ／ｍｉｎ。Table 1 uμ Chitosan: degree of deacetylation 85% Molecular weight 30,000 Solution concentration 10% Acid: 8% acetic acid Spray drying: Inlet temperature 80℃ Atomizing air pressure 1 to gf/cnf Liquid feeding rate 1-2 mfl/min.
アンモニア濃度； １１００００ｐｐ キトサン微小粒体の平均粒径：１００μｍ丈族例１ キトサン：脱アセチル化度７２％ 分子量５万 溶液濃度５％ 酸： ２％塩酸 噴霧乾燥：入口温度９０℃ 噴霧空気圧Ｉ Ｋｇｆ／ｃ ｒｎ２ 送液速度１〜２ｍｌ／ｍｉｎ。Ammonia concentration: 110000pp Average particle size of chitosan microparticles: 100 μm Example 1 Chitosan: degree of deacetylation 72% Molecular weight 50,000 Solution concentration 5% Acid: 2% hydrochloric acid Spray drying: Inlet temperature 90℃ Spray air pressure I Kgf/c rn2 Liquid feeding rate 1-2 ml/min.
アンモニア濃度；１１００ｐｐ キトサン微小粒体の平均粒径：５０μｍ丈施珂Ａ キトサン：脱アセチル化度９９％ 分子量２３万 溶液濃度１％ 酸： １％酢酸 噴霧乾燥：入口温度７０℃ 噴霧空気圧Ｉ Ｋｇｆ／ｃ ｒｎ’ 送液速度１〜２ｍｕ／ｍｉｎ。Ammonia concentration: 1100pp Average particle size of chitosan microparticles: 50 μm length A Chitosan: degree of deacetylation 99% Molecular weight 230,000 Solution concentration 1% Acid: 1% acetic acid Spray drying: Inlet temperature 70℃ Spray air pressure I Kgf/c rn’ Liquid feeding rate 1-2 mu/min.
アンモニア濃度；５００ｐｐｍ キトサン微小粒体の平均粒径ニアμｍ 丈施劇ｊ ゛ キトサン：脱アセチル化度５０％ 分子量２０万 溶液濃度０．１％ 酸： ０．４％酢酸 噴霧乾燥：人口温度８０℃ 噴霧空気圧Ｉ Ｋｇｆ／ｃ ｒｎ” 送液速度２〜３ｍ１ｌ／ｍｉｎ。Ammonia concentration: 500ppm Average particle size of chitosan microparticles near μm Josuke drama j ゛ Chitosan: degree of deacetylation 50% Molecular weight 200,000 Solution concentration 0.1% Acid: 0.4% acetic acid Spray drying: population temperature 80℃ Spray air pressure I Kgf/c rn” Liquid feeding rate 2-3 ml/min.
アンモニア濃度；１１０００ｐｐ キトサン微小粒体の平均粒径；２μｍ 夾嵐１− キトサン：脱アセチル化度８５％ 分子量３万 溶液濃度０．５％ 酸： ０．５％酢酸 噴霧乾燥；人口温度１００℃ 噴霧空気圧ＩＫｇｆ／ｃｒｎ’ 送液速度４〜５ ｍ Ｉｌ、 ／ ｍｉｎ。Ammonia concentration: 11000pp Average particle size of chitosan microparticles: 2 μm Kyo Arashi 1- Chitosan: degree of deacetylation 85% Molecular weight 30,000 Solution concentration 0.5% Acid: 0.5% acetic acid Spray drying; population temperature 100℃ Spray air pressure IKgf/crn’ Liquid feeding speed 4-5 mIl, /min.
Claims (4)
乾燥することを特徴とするキトサン粒体の製造方法。(1) A method for producing chitosan granules, which comprises spray-drying an acid aqueous solution of chitosan in an ammonia atmosphere.
あるである特許請求の範囲第（１）項に記載のキトサン
粒体の製造方法。(2) The method for producing chitosan granules according to claim (1), wherein the ammonia concentration is 100 to 10,000 ppm.
る特許請求の範囲第（１）項に記載のキトサン粒体の製
造方法。(3) The method for producing chitosan granules according to claim (1), wherein the aqueous solution concentration of chitosan is 0.1 to 20% by weight.
サン粒体の平均粒径を制御する特許請求の範囲第（１）
項に記載のキトサン粒体の製造方法。(4) Claim No. 1, which controls the average particle size of the chitosan particles obtained by controlling the concentration of the chitosan aqueous solution.
The method for producing chitosan granules as described in section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16093086A JPH0623201B2 (en) | 1986-07-10 | 1986-07-10 | Method for producing chitosan granules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16093086A JPH0623201B2 (en) | 1986-07-10 | 1986-07-10 | Method for producing chitosan granules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6317902A true JPS6317902A (en) | 1988-01-25 |
| JPH0623201B2 JPH0623201B2 (en) | 1994-03-30 |
Family
ID=15725326
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16093086A Expired - Fee Related JPH0623201B2 (en) | 1986-07-10 | 1986-07-10 | Method for producing chitosan granules |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0623201B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| US6252003B1 (en) | 1998-06-04 | 2001-06-26 | Kao Corporation | Polymer emulsion and process for producing the same |
| KR100661125B1 (en) | 2005-05-06 | 2006-12-22 | 주식회사 바이오폴리텍 | Chitosan particle and process therefor |
-
1986
- 1986-07-10 JP JP16093086A patent/JPH0623201B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010181A (en) * | 1988-03-28 | 1991-04-23 | Coughlin Robert W | Partially treated shellfish waste for removal of heavy metals from aqueous solution |
| US6252003B1 (en) | 1998-06-04 | 2001-06-26 | Kao Corporation | Polymer emulsion and process for producing the same |
| US6359032B1 (en) | 1998-06-04 | 2002-03-19 | Kao Corporation | Polymer emulsion and process for preparing the same |
| KR100661125B1 (en) | 2005-05-06 | 2006-12-22 | 주식회사 바이오폴리텍 | Chitosan particle and process therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0623201B2 (en) | 1994-03-30 |
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