JP2002105101A - Method for producing water-soluble polymer - Google Patents
Method for producing water-soluble polymerInfo
- Publication number
- JP2002105101A JP2002105101A JP2000304013A JP2000304013A JP2002105101A JP 2002105101 A JP2002105101 A JP 2002105101A JP 2000304013 A JP2000304013 A JP 2000304013A JP 2000304013 A JP2000304013 A JP 2000304013A JP 2002105101 A JP2002105101 A JP 2002105101A
- Authority
- JP
- Japan
- Prior art keywords
- water
- polymer
- pressure
- temperature
- molecular weight
- 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.)
- Pending
Links
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Beans For Foods Or Fodder (AREA)
- Cereal-Derived Products (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、水不溶性天然高分
子物質を部分分解処理して水溶性高分子物質を得るため
の方法に関する。特に、本発明は、利用価値の乏しい水
不溶性の天然高分子物質を、食品、医薬・健康栄養素
材、微生物培地等の幅広い分野において利用できる水溶
性高分子物質に転化する方法に関する。TECHNICAL FIELD The present invention relates to a method for obtaining a water-soluble polymer by partially decomposing a water-insoluble natural polymer. In particular, the present invention relates to a method of converting a water-insoluble natural polymer substance having a low utility value into a water-soluble polymer substance that can be used in a wide range of fields such as foods, medicines / health nutrition materials, and microbial media.
【０００２】[0002]
【従来の技術】天然の水溶性高分子物質は、食品用素
材、医薬用・健康栄養剤用の素材、微生物培地等の幅広
い分野において多量に利用されている。このような水溶
性天然高分子物質と同等の特性を備えた水溶性高分子物
質を水不溶性天然高分子物質から得る試みも従来からな
されてきており、たとえば、水不溶性の天然高分子物質
を酸触媒や酵素等を利用して加水分解するというような
方法も行われている。2. Description of the Related Art Natural water-soluble polymer substances are widely used in a wide range of fields such as food materials, materials for medicines and health and nutritional supplements, and microorganism culture media. Attempts have been made to obtain a water-soluble polymer having characteristics equivalent to those of the water-soluble natural polymer from a water-insoluble natural polymer. A method of performing hydrolysis using a catalyst, an enzyme, or the like is also performed.
【０００３】しかし、酸触媒を用いた場合、製造工程か
ら得られる水溶性高分子物質を利用する際に使用酸触媒
を水溶性高分子物質中より完全に除く操作が必要である
し、また、酸による製造設備の腐食防止手段を講じなけ
ればならない等、解決しなければならない問題が多い。
また、酵素を利用する場合、一般に使用する酵素は高価
であり、しかもその反応速度が遅いため、分解率を向上
させるために多量の酵素を使用する必要があってコスト
高となることが避けられない。However, when an acid catalyst is used, it is necessary to completely remove the used acid catalyst from the water-soluble polymer when using the water-soluble polymer obtained from the production process. There are many problems that need to be solved, such as the need to take measures to prevent corrosion of manufacturing equipment by acids.
In addition, when enzymes are used, generally used enzymes are expensive and the reaction rate is slow, so that it is necessary to use a large amount of enzymes in order to improve the decomposition rate, thereby avoiding high costs. Absent.
【０００４】ところで、特許３０４２０７６号公報に
は、天然又は合成高分子化合物の選択的加水分解方法と
して、超臨界状態あるいは亜臨界状態の水を溶媒として
用いて天然又は合成高分子化合物の加水分解を行うこと
によって、原料である天然又は合成高分子の構成単位程
度の低分子まで加水分解された反応生成物が得られるこ
とが記載されている。また、特開平９−２６８１６６号
公報には、超臨界水によって蛋白質が構成アミノ酸にま
で加水分解されること、その生成した遊離アミノ酸が再
結合によってペプチドとなることが記載されている。Japanese Patent No. 3042076 discloses a method for selectively hydrolyzing a natural or synthetic polymer compound using water in a supercritical or subcritical state as a solvent. It is described that by performing the reaction, a reaction product hydrolyzed to a low molecular weight of about the structural unit of a natural or synthetic polymer as a raw material is obtained. Japanese Patent Application Laid-Open No. 9-268166 describes that proteins are hydrolyzed to constituent amino acids by supercritical water, and that the free amino acids formed into peptides by recombination.
【０００５】しかしながら、特許３０４２０７６号や特
開平９−２６８１６６号の方法では、原料である天然の
水不溶性高分子物質の多くを占めるセルロースや蛋白質
が超臨界水又は亜臨界水によって分解反応に付される
と、構成単量体又はオリゴマー程度まで低分子化され数
百程度の質量（分子量）となってしまうものであり、天
然物由来の高分子物質として幅広い用途を有する、平均
質量が１０ｋＤａ（キロダルトン）〜１００００ｋＤａ
である水溶性高分子を得る方法についての開示はない。However, in the methods disclosed in Japanese Patent No. 3042076 and Japanese Patent Application Laid-Open No. 9-268166, cellulose or protein, which is a raw material of the majority of natural water-insoluble polymer, is subjected to a decomposition reaction by supercritical water or subcritical water. Then, the molecular weight is reduced to the order of the constituent monomers or oligomers, resulting in a mass (molecular weight) of about several hundreds. The polymer has a wide range of uses as a polymer derived from natural products, and has an average mass of 10 kDa (kg). Dalton) to 10000 kDa
There is no disclosure of a method for obtaining a water-soluble polymer.
【０００６】また、蛋白質の低分子化方法としては、特
開昭６３−３２４６７号公報には、温度５０℃〜３５０
℃、圧力２５０〜５０００ｋｇ／ｃｍ2 の条件下に、５
〜６０分間、蛋白質を保持すると分子量１００００以下
の低分子化物が製造できることが記載されている。しか
し、この方法の場合、圧力が２５０ｋｇ／ｃｍ2 以上と
いう高圧条件が必須であり、より低圧条件下での低分子
化方法及びその結果についてはなんら触れられていな
い。As a method for reducing the molecular weight of a protein, Japanese Patent Application Laid-Open No. 63-32467 discloses a method for reducing the temperature from 50 ° C. to 350 ° C.
5 ° C. and a pressure of 250 to 5000 kg / cm 2.
It is described that a low molecular weight product having a molecular weight of 10,000 or less can be produced by holding the protein for 、 60 minutes. However, in the case of this method, a high pressure condition of a pressure of 250 kg / cm 2 or more is essential, and there is no mention of a method for depolymerizing under a lower pressure condition and the result thereof.
【０００７】[0007]
【発明が解決しようとする課題】本発明は、水不溶性の
天然高分子物質から、精製手段にコストがかからない水
のみを使用することにより、幅広い用途にそのまま適用
することができる安全性を備えた天然物由来の水溶性高
分子物質を安価に製造することができる方法を提供する
ことを目的とするものである。DISCLOSURE OF THE INVENTION The present invention has a safety that can be directly applied to a wide range of applications by using only inexpensive water as a purification means from a water-insoluble natural polymer substance. It is an object of the present invention to provide a method for inexpensively producing a water-soluble polymer derived from a natural product.
【０００８】[0008]
【課題を解決するための手段】本発明者らは前項記載の
目的を達成すべく鋭意研究を重ねた結果、天然の水不溶
性高分子物質を高温高圧水と接触処理せしめることによ
り幅広い用途を有する質量１０ｋＤａ〜１００００ｋＤ
ａの天然物由来の水溶性高分子を得ることができること
を見出し、これらの知見に基づいて本発明を完成するに
至った。本発明は、以下の各発明を包含する。Means for Solving the Problems The inventors of the present invention have conducted intensive studies to achieve the above-mentioned object, and as a result, have a wide range of applications by subjecting a natural water-insoluble polymer substance to contact treatment with high-temperature and high-pressure water. Mass 10kDa-10000kD
The present inventors have found that a water-soluble polymer derived from the natural product a can be obtained, and have completed the present invention based on these findings. The present invention includes the following inventions.
【０００９】(１) 水不溶性天然高分子物質からなる原
料物質と、１００℃を超える３００℃までの範囲の温度
でかつ圧力がその温度における水の蒸気圧よりも高い圧
力状態にある高温高圧水とを、該原料物質がより低分子
量の高分子物質に部分分解される時間接触せしめること
を特徴とする、水溶性高分子物質の製造方法。(1) A raw material composed of a water-insoluble natural polymer substance, and high-temperature high-pressure water at a temperature in the range of more than 100 ° C. to 300 ° C. and a pressure higher than the vapor pressure of water at that temperature. Wherein the raw material is contacted for a period of time when the raw material is partially decomposed into a polymer having a lower molecular weight.
【００１０】(２) 前記のより低分子量の高分子物質
が、質量１０ｋＤａ〜１００００ｋＤａに相当する分子
量を有する高分子物質であることを特徴とする(1)項記
載の水溶性高分子物質の製造方法。(2) The production of a water-soluble polymer according to (1), wherein the lower molecular weight polymer is a polymer having a molecular weight corresponding to a mass of 10 kDa to 10,000 kDa. Method.
【００１１】（３）前記(1)項又は(2)項に記載の方法に
よって製造されている水不溶性天然高分子物質由来の水
溶性高分子物質、特に質量１０ｋＤａ〜１００００ｋＤ
ａである水不溶性天然高分子由来の水溶性高分子物質。(3) A water-soluble polymer derived from a water-insoluble natural polymer produced by the method described in the above item (1) or (2), particularly, a mass of 10 kDa to 10,000 kD.
a) a water-soluble polymer derived from a water-insoluble natural polymer.
【００１２】本発明において、水不溶性天然高分子物質
を高温高圧水で処理する手段は、具体的には、水不溶性
の天然高分子物質を高温高圧水と接触状態に置くことで
ある。In the present invention, the means for treating the water-insoluble natural high-molecular substance with high-temperature and high-pressure water is, specifically, to put the water-insoluble natural high-molecular substance in contact with high-temperature and high-pressure water.
【００１３】そして、本発明でいう高温高圧水とは、１
００℃を超える３００℃までの範囲の温度でかつ圧力が
その温度における水の蒸気圧よりも高い圧力状態にある
水を意味している。上記の高温高圧水は、少なくても前
記温度及び圧力の範囲に調整されていればよいが、好ま
しくは温度１００℃を超えて３００℃までの範囲、圧力
０．１ＭＰａを超えて２５ＭＰａ以内までの範囲、より
好ましくは温度１５０℃〜２００℃及び圧力０．５ＭＰ
ａ〜１０ＭＰａの範囲のものである。The high-temperature and high-pressure water referred to in the present invention is 1
Water at a temperature in the range of greater than 00 ° C. to 300 ° C. and at a pressure greater than the vapor pressure of water at that temperature is meant. The above high-temperature and high-pressure water may be adjusted to at least the temperature and pressure ranges described above, but preferably, the temperature ranges from more than 100 ° C. to 300 ° C., and the pressure exceeds 0.1 MPa to 25 MPa or less. Range, more preferably temperature 150 ° C to 200 ° C and pressure 0.5MP
a to 10 MPa.
【００１４】原料として使用する水不溶性の天然高分子
物質としては、セルロース系、でんぷん系及び蛋白質系
の高分子物質が好適な材料であるが、これらに限定され
ない。水不溶性の天然高分子物質はそれらの混合物であ
ってもよい。具体的には、各種でんぷん類、穀物類、バ
イオマス等が挙げられる。As the water-insoluble natural polymer used as a raw material, cellulose-based, starch-based and protein-based polymer substances are suitable, but not limited thereto. The water-insoluble natural macromolecular substance may be a mixture thereof. Specifically, various starches, cereals, biomass and the like can be mentioned.
【００１５】水不溶性の天然高分子物質と前記高温高圧
水との接触は、水不溶性の天然高分子物質が水に分散し
ているスラリー状態やペースト状態のように、水不溶性
の天然高分子物質と水とが均一に混合され、又は分散し
ている状態であれば特に制限はない。水不溶性の天然高
分子物質と水の混合割合は、水不溶性の天然高分子物質
乾燥物としての含有量が０．１〜５０重量％の範囲とな
る割合が好ましい。The contact between the water-insoluble natural polymer substance and the high-temperature and high-pressure water is carried out in a water-insoluble natural polymer substance such as a slurry state or a paste state in which the water-insoluble natural polymer substance is dispersed in water. There is no particular limitation as long as water and water are uniformly mixed or dispersed. The mixing ratio of the water-insoluble natural polymer substance and water is preferably such that the content of the water-insoluble dried natural polymer substance is in the range of 0.1 to 50% by weight.
【００１６】本発明の水溶性天然高分子物質の製造方法
において、水不溶性の天然高分子物質と水との接触時間
は重要であるが、該接触時間は、被処理原料の種類に応
じて設定されるべきであり、各種原料に対応する好適接
触時間は、各種原料それぞれについて、前記高温高圧水
との接触時間と生成物との関係を事前の予備実験により
測定して把握しておくことで容易に設定することができ
る。一般的には、水不溶性の天然高分子物質と水との接
触時間が長くなるほど分子量は低下し、最終的に高分子
を構成する単量体やその分解物である揮発性有機物が生
成されるまで分解が進行するので、目的とする平均質量
の分解生成物が得られる接触時間を正確に把握しておく
ことが特に重要である。In the method for producing a water-soluble natural polymer of the present invention, the contact time between the water-insoluble natural polymer and water is important, and the contact time is set according to the type of the raw material to be treated. It should be performed, the preferred contact time corresponding to the various raw materials, for each of the various raw materials, by measuring the relationship between the contact time with the high-temperature and high-pressure water and the product by preliminary preliminary experiments and grasping. It can be easily set. In general, the longer the contact time between water and a water-insoluble natural polymer substance and water, the lower the molecular weight, eventually producing the monomers that constitute the polymer and the volatile organic substances that are its decomposition products. Since the decomposition proceeds up to this point, it is particularly important to accurately understand the contact time at which the decomposition product having the desired average mass is obtained.
【００１７】[0017]
【実施例】以下、本発明を実施例によって更に詳細に説
明するが、下記実施例は本発明を限定するものではな
く、前記及び後記の趣旨に徴して設計変更することは、
いずれも、本発明の技術的範囲に含まれるものである。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples. However, the following examples do not limit the present invention.
All of them are included in the technical scope of the present invention.
【００１８】実施例１：水溶性コーン高分子の製造 １０，０００ｒｐｍで遠心粉砕し、０．５ｍｍメッシュ
スクリーンで篩分けした乾燥コーンに水を加え、コーン
スラリー３３重量％を調製した。図１の装置を使用し、
このコーンスラリーを高圧ポンプで送液し、１５０℃、
又は、２００℃に加熱した反応器に導入し、反応を開始
した。反応時間、すなわち、反応器を通過する時間は１
分とした。また、反応器出口に取り付けた二重冷却管に
導入し急冷することで反応を停止させた。反応液はライ
ン出口に設置した背圧弁から回収した。なお、系内の圧
力は背圧弁によって調節し、高圧ポンプの吐出口から背
圧弁までを５ＭＰａに保持した。Example 1 Production of Water-Soluble Cone Polymer Water was added to a dried corn which was centrifuged and ground at 10,000 rpm and sieved with a 0.5 mm mesh screen to prepare a corn slurry (33% by weight). Using the device of FIG. 1,
This corn slurry is sent by a high pressure pump,
Alternatively, it was introduced into a reactor heated to 200 ° C. to start the reaction. The reaction time, ie the time passing through the reactor, is 1
Minutes. Further, the reaction was stopped by introducing into a double cooling tube attached to the outlet of the reactor and rapidly cooling it. The reaction solution was collected from a back pressure valve installed at the line outlet. The pressure in the system was adjusted by a back pressure valve, and the pressure from the discharge port of the high pressure pump to the back pressure valve was maintained at 5 MPa.
【００１９】得られた各反応液を遠心分離（１５，００
０ｒｐｍ、１０分）し、その上澄み液を乾燥コーン重量
で０．５重量％濃度となるように水を加え、さらに０．
４５μｍのフィルターによってろ過を行い、得られた各
液をＧＰＣ（カラム：ＡｓａｈｉＰＡＣ ＧＳ−６２０
ＨＱ、カラム温度：３０℃、溶離液：水、０．５ｍＬ
／ｍｉｎ、検出：ＲＩ）によって分子量分布を調べた。Each reaction solution obtained was centrifuged (15,000).
0 rpm for 10 minutes), and water was added to the supernatant to a concentration of 0.5% by weight on a dry corn basis.
Filtration was performed with a 45 μm filter, and each obtained liquid was subjected to GPC (column: AsahiPAC GS-620).
HQ, column temperature: 30 ° C., eluent: water, 0.5 mL
/ Min, detection: RI).
【００２０】分子量分布については、分子量既知である
標準品（昭和電工製Ｐｕｌｌｕｌａｎ Ｐ−８２）を予
め測定し、その分子量とＧＰＣの保持時間との相関式を
作成し、分子量計算を行った。分子量と保持時間の関係
を図６に示す。図２にＧＰＣチャートを示すが、温度が
１５０℃と２００℃のいずれも、供給したコーンスラリ
ーと比較して質量５００ｋＤａ〜３，０００ｋＤａに相
当する水溶性コーン高分子の存在が増大していることか
ら、供給したコーンスラリー中の水不溶性物質の一部が
水溶性コーン高分子物質に転化され、溶出していること
が確認された。Regarding the molecular weight distribution, a standard product having a known molecular weight (Pululan P-82 manufactured by Showa Denko) was measured in advance, and a correlation formula between the molecular weight and the retention time of GPC was prepared to calculate the molecular weight. FIG. 6 shows the relationship between the molecular weight and the retention time. FIG. 2 shows the GPC chart. At both the temperatures of 150 ° C. and 200 ° C., the presence of the water-soluble corn polymer corresponding to the mass of 500 kDa to 3,000 kDa was increased as compared with the supplied corn slurry. From this, it was confirmed that a part of the water-insoluble substance in the supplied corn slurry was converted into a water-soluble corn polymer substance and eluted.
【００２１】実施例２：水溶性おから高分子 乾燥おからに水を加え、おからスラリー６重量％を調製
した。図１の装置を使用し、このおからスラリーを高圧
ポンプで送液し、２００℃に加熱した反応器に導入し、
実施例１と同様に、反応開始、反応停止、反応液を回収
した。反応時間は４４秒とした。また、系内の圧力は５
ＭＰａに保持した。得られた反応液を実施例１と同様な
処理を行い、ＧＰＣによって、分子量分布を測定した。
図３にＧＰＣチャートを示すが、供給したおからスラリ
ーと比較して、質量５００ｋＤａ〜３，０００ｋＤａに
相当する水溶性おから高分子の存在が増大していること
から、供給したおからスラリー中の水不溶性物質の一部
が水溶性高分子物質に転化され、溶出していることが確
認された。Example 2 Water-soluble okara polymer Water was added to dried okara to prepare 6% by weight of okara slurry. Using the apparatus of FIG. 1, this okara slurry was sent by a high-pressure pump and introduced into a reactor heated to 200 ° C.
As in Example 1, the reaction was started, stopped, and the reaction solution was recovered. The reaction time was 44 seconds. The pressure in the system is 5
It was kept at MPa. The obtained reaction solution was subjected to the same treatment as in Example 1, and the molecular weight distribution was measured by GPC.
FIG. 3 shows a GPC chart. Compared with the supplied okara slurry, the presence of a water-soluble okara polymer corresponding to a mass of 500 kDa to 3,000 kDa is increased. It was confirmed that a part of the water-insoluble substance was converted to a water-soluble polymer substance and eluted.
【００２２】実施例３：水溶性でんぷん高分子 タピオカでんぷんに水を加え、タピオカでんぷんスラリ
ー２．５重量％を調製した。図１の装置を使用し、この
タピオカでんぷんスラリーを高圧ポンプで送液し、反応
器直前で予め熱していた水と接触させ反応器に導入する
ことで反応開始とし、また実施例１と同様に、反応停
止、反応液を回収した。温度は２００℃、又は、２５０
℃、反応時間はそれぞれ１３秒、１２秒とした。また、
系内の圧力は５ＭＰａに保持した。得られた反応液を実
施例１と同様な処理を行い、ＧＰＣによって、分子量分
布を測定した。図４にＧＰＣチャートを示すが、２００
℃条件では質量５００ｋＤａ〜３，０００ｋＤａ、２５
０℃条件では質量１０ｋＤａ〜１，０００ｋＤａに相当
する供給したスラリー中に存在しなかった水溶性でんぷ
ん高分子の存在が確認された。Example 3: Water-soluble starch polymer Water was added to tapioca starch to prepare 2.5% by weight of tapioca starch slurry. Using the apparatus of FIG. 1, this tapioca starch slurry is fed by a high-pressure pump, brought into contact with pre-heated water immediately before the reactor, and introduced into the reactor to start the reaction, and in the same manner as in Example 1, The reaction was stopped, and the reaction solution was recovered. Temperature is 200 ° C or 250
C. and the reaction time were 13 seconds and 12 seconds, respectively. Also,
The pressure in the system was maintained at 5 MPa. The obtained reaction solution was subjected to the same treatment as in Example 1, and the molecular weight distribution was measured by GPC. FIG. 4 shows a GPC chart.
Under the condition of ° C, the mass is 500 kDa to 3,000 kDa, 25
Under the condition of 0 ° C., the presence of a water-soluble starch polymer which was not present in the supplied slurry corresponding to a mass of 10 kDa to 1,000 kDa was confirmed.
【００２３】実施例４：水溶性キャッサバ高分子 １０，０００ｒｐｍで遠心粉砕し、０．５ｍｍメッシュ
スクリーンで篩分けした乾燥キャッサバに水を加え、キ
ャッサバスラリー３３重量％を調製した。図１の装置を
使用し、このキャッサバスラリーを高圧ポンプで送液
し、２００℃に加熱した反応器に導入し、実施例１と同
様に、反応開始、反応停止、反応液を回収した。反応時
間は１２０秒とした。得られた反応液を実施例１と同様
な処理を行い、ＧＰＣによって、分子量分布を測定し
た。図５に示すように原料スラリーに存在しなかった質
量５００ｋＤａ〜３，０００ｋＤａに相当する水溶性高
分子の存在が確認された。Example 4: Water-soluble cassava polymer Water was added to a dried cassava sieved by centrifugation at 10,000 rpm and sieved with a 0.5 mm mesh screen to prepare a cassava slurry (33% by weight). Using the apparatus shown in FIG. 1, the cassava slurry was fed by a high-pressure pump, introduced into a reactor heated to 200 ° C., and the reaction was started, stopped, and the reaction solution was recovered as in Example 1. The reaction time was 120 seconds. The obtained reaction solution was subjected to the same treatment as in Example 1, and the molecular weight distribution was measured by GPC. As shown in FIG. 5, the presence of a water-soluble polymer corresponding to a mass of 500 kDa to 3,000 kDa that was not present in the raw material slurry was confirmed.
【００２４】比較例１ 実施例１で使用したコーンスラリーについて、実施例１
に記載した反応液と同様の処理を行い、ＧＰＣ分析を行
った。ＧＰＣチャートは図２に示す。Comparative Example 1 The corn slurry used in Example 1 was used in Example 1.
And the GPC analysis was performed. The GPC chart is shown in FIG.
【００２５】比較例２ 実施例２で使用したおからスラリーについて、実施例１
に記載した反応液と同様の処理を行い、ＧＰＣ分析を行
った。ＧＰＣチャートは図４に示す。Comparative Example 2 Okara slurry used in Example 2 was used in Example 1.
And the GPC analysis was performed. The GPC chart is shown in FIG.
【００２６】比較例３ 実施例３で使用したタピオカでんぷんスラリーについ
て、実施例１に記載した反応液と同様の処理を行った
が、０．４５μｍフィルターろ過を行うことができなか
った。Comparative Example 3 The tapioca starch slurry used in Example 3 was treated in the same manner as in the reaction solution described in Example 1, but could not be filtered with a 0.45 μm filter.
【００２７】比較例４ 実施例４で使用したキャッサバスラリーについて、実施
例１に記載した反応液と同様の処理を行ったが、０．４
５μｍフィルターろ過を行うことができなかった。Comparative Example 4 The cassava slurry used in Example 4 was treated in the same manner as in the reaction solution described in Example 1, except that
5 μm filter filtration could not be performed.
【００２８】[0028]
【発明の効果】以上のように、本発明の方法によれば、
水不溶性天然高分子物質から水溶性天然高分子を効率よ
く生産することが可能となり、食品、医薬・健康栄養素
材、微生物培地等の分野において多くの利用の可能性が
期待できる材料を供給することができる。As described above, according to the method of the present invention,
Supplying materials that enable efficient production of water-soluble natural polymers from water-insoluble natural polymer substances and are expected to have many potential uses in the fields of foods, pharmaceuticals / health and nutritional materials, and microbial media. Can be.
【図１】本発明を実施するために構成される装置例を示
す概略図である。FIG. 1 is a schematic diagram showing an example of an apparatus configured to carry out the present invention.
【図２】実施例１及び比較例１の生成物のＧＰＣチャー
トを示す図である。FIG. 2 is a diagram showing a GPC chart of products of Example 1 and Comparative Example 1.
【図３】実施例２及び比較例２の生成物のＧＰＣチャー
トを示す図である。FIG. 3 is a diagram showing a GPC chart of products of Example 2 and Comparative Example 2.
【図４】実施例３の生成物ＧＰＣチャートを示す図であ
る。FIG. 4 is a diagram showing a product GPC chart of Example 3.
【図５】実施例４の生成物のＧＰＣチャートを示す図で
ある。FIG. 5 is a diagram showing a GPC chart of a product of Example 4.
【図６】図２〜図５における保持時間と分子量の関係を
示す図である。FIG. 6 is a diagram showing the relationship between retention time and molecular weight in FIGS. 2 to 5;
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ０８Ｂ 15/00 Ｃ０８Ｂ 15/00 Ｃ０８Ｈ 1/00 Ｃ０８Ｈ 1/00 Ｆターム(参考） 4B018 LB10 LE05 MD47 ME11 MF04 MF10 4B020 LB24 LG07 LP03 LP09 LS10 4B023 LC05 LE30 LG08 LG10 LK08 LP07 LQ01 4C090 AA04 BA07 BA13 BA17 BA24 BA34 BB12 BC11 BC12 BD03 BD37 CA04 CA05 CA31 DA22 DA27 DA32 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C08B 15/00 C08B 15/00 C08H 1/00 C08H 1/00 F term (Reference) 4B018 LB10 LE05 MD47 ME11 MF04 MF10 4B020 LB24 LG07 LP03 LP09 LS10 4B023 LC05 LE30 LG08 LG10 LK08 LP07 LQ01 4C090 AA04 BA07 BA13 BA17 BA24 BA34 BB12 BC11 BC12 BD03 BD37 CA04 CA05 CA31 DA22 DA27 DA32
Claims (2)
と、１００℃を超える３００℃までの範囲の温度でかつ
圧力がその温度における水の蒸気圧よりも高い圧力状態
にある高温高圧水とを、該原料物質がより低分子量の高
分子物質に部分分解される時間接触せしめることを特徴
とする水溶性高分子物質の製造方法。1. A raw material comprising a water-insoluble natural polymer, and high-temperature high-pressure water at a temperature in the range of more than 100 ° C. to 300 ° C. and a pressure higher than the vapor pressure of water at that temperature. A method for producing a water-soluble polymer substance, wherein the raw material substance is brought into contact with the polymer substance having a lower molecular weight for a partial decomposition time.
量１０ｋＤａ〜１００００ｋＤａに相当する高分子物質
であることを特徴とする請求項1記載の水溶性高分子物
質の製造方法。2. The method for producing a water-soluble polymer substance according to claim 1, wherein the lower molecular weight polymer substance is a polymer substance having a mass of 10 kDa to 10,000 kDa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000304013A JP2002105101A (en) | 2000-10-03 | 2000-10-03 | Method for producing water-soluble polymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000304013A JP2002105101A (en) | 2000-10-03 | 2000-10-03 | Method for producing water-soluble polymer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002105101A true JP2002105101A (en) | 2002-04-10 |
Family
ID=18785125
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000304013A Pending JP2002105101A (en) | 2000-10-03 | 2000-10-03 | Method for producing water-soluble polymer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2002105101A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005034808A (en) * | 2003-07-18 | 2005-02-10 | Hyogo Prefecture | Continuous treatment apparatus using subcritical or supercritical water and hydrolysate of organic material obtained using the same |
| WO2008090804A1 (en) * | 2007-01-24 | 2008-07-31 | Ajinomoto Co., Inc. | Method for production of saccharide from starch-containing plant raw material |
| WO2008155890A1 (en) * | 2007-06-21 | 2008-12-24 | J-Oil Mills, Inc. | Method for producing glycoside aglycone |
| JP2009232747A (en) * | 2008-03-27 | 2009-10-15 | National Univ Corp Shizuoka Univ | Production system of water-soluble saccharide derived from paper sludge and production method of water-soluble saccharide derived from paper sludge |
| JP2009540106A (en) * | 2006-06-15 | 2009-11-19 | バイオポリマー エンジニアリング インコーポレイテッド ディービーエイ バイオセラ インコーポレイテッド | Glucan preparation |
| WO2011013530A1 (en) * | 2009-07-31 | 2011-02-03 | 物産フードサイエンス株式会社 | Process for production of galactomannan with reduced moleculr weight and catalyst to be used therein |
| KR20140105620A (en) * | 2007-05-08 | 2014-09-01 | 바이오테라, 인크. | Particulate-soluble glucan preparation |
| US10111901B2 (en) | 2014-07-10 | 2018-10-30 | Biothera, Inc. | Beta-glucan in combination with anti-cancer agents affecting the tumor microenvironment |
| US10111900B2 (en) | 2014-11-06 | 2018-10-30 | Biothera, Inc. | β-glucan methods and compositions that affect the tumor microenvironment |
| US11815435B2 (en) | 2017-02-24 | 2023-11-14 | Hibercell, Inc. | Beta glucan immunopharmacodynamics |
-
2000
- 2000-10-03 JP JP2000304013A patent/JP2002105101A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005034808A (en) * | 2003-07-18 | 2005-02-10 | Hyogo Prefecture | Continuous treatment apparatus using subcritical or supercritical water and hydrolysate of organic material obtained using the same |
| JP4664580B2 (en) * | 2003-07-18 | 2011-04-06 | 兵庫県 | Continuous processing equipment using subcritical water or supercritical water |
| JP2014025079A (en) * | 2006-06-15 | 2014-02-06 | Biothera Inc | Glucan preparation |
| US10272101B2 (en) | 2006-06-15 | 2019-04-30 | Biothera Inc. | Glucan preparations |
| US9610303B2 (en) | 2006-06-15 | 2017-04-04 | Biothera, Inc. | Glucan preparations |
| JP2009540106A (en) * | 2006-06-15 | 2009-11-19 | バイオポリマー エンジニアリング インコーポレイテッド ディービーエイ バイオセラ インコーポレイテッド | Glucan preparation |
| WO2008090804A1 (en) * | 2007-01-24 | 2008-07-31 | Ajinomoto Co., Inc. | Method for production of saccharide from starch-containing plant raw material |
| KR101665216B1 (en) * | 2007-05-08 | 2016-10-11 | 바이오테라, 인크. | Particulate-soluble glucan preparation |
| KR20140105620A (en) * | 2007-05-08 | 2014-09-01 | 바이오테라, 인크. | Particulate-soluble glucan preparation |
| WO2008155890A1 (en) * | 2007-06-21 | 2008-12-24 | J-Oil Mills, Inc. | Method for producing glycoside aglycone |
| JP2009232747A (en) * | 2008-03-27 | 2009-10-15 | National Univ Corp Shizuoka Univ | Production system of water-soluble saccharide derived from paper sludge and production method of water-soluble saccharide derived from paper sludge |
| WO2011013530A1 (en) * | 2009-07-31 | 2011-02-03 | 物産フードサイエンス株式会社 | Process for production of galactomannan with reduced moleculr weight and catalyst to be used therein |
| US10111901B2 (en) | 2014-07-10 | 2018-10-30 | Biothera, Inc. | Beta-glucan in combination with anti-cancer agents affecting the tumor microenvironment |
| US10111900B2 (en) | 2014-11-06 | 2018-10-30 | Biothera, Inc. | β-glucan methods and compositions that affect the tumor microenvironment |
| US11815435B2 (en) | 2017-02-24 | 2023-11-14 | Hibercell, Inc. | Beta glucan immunopharmacodynamics |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sedaghat et al. | Bioconversion of shrimp waste Penaeus merguiensis using lactic acid fermentation: An alternative procedure for chemical extraction of chitin and chitosan | |
| Wang et al. | Ultrasound assisted enzymatic hydrolysis of starch catalyzed by glucoamylase: Investigation on starch properties and degradation kinetics | |
| Jeon et al. | Continuous production of chitooligosaccharides using a dual reactor system | |
| Zhang et al. | Enzymatic hydrolysis of chitin pretreated by bacterial fermentation to obtain pure N-acetyl-d-glucosamine | |
| EP4137207A1 (en) | Dextran-poly alpha-1,3-glucan graft copolymers and synthesis methods thereof | |
| Mohammed et al. | Extraction of chitin from prawn shells and conversion to low molecular mass chitosan | |
| Zhang et al. | Efficient hydrolysis of chitosan in ionic liquids | |
| US20070267008A1 (en) | Method of Hydrolyzing an Organic Compound | |
| JP2002105101A (en) | Method for producing water-soluble polymer | |
| CN108264574B (en) | Ozone degradation method of polysaccharide | |
| US20180230239A1 (en) | A starch-based food thickener with low molecular weight and a preparation method thereof | |
| JP2006204207A (en) | Method for producing starch decomposition product and white dextrin | |
| CN109232770A (en) | A kind of preparation method of high substituted degree acetylation Sodium Hyaluronate | |
| CN110862461B (en) | Preparation method of resistant dextrin | |
| US5376537A (en) | Process for production of cyclodextrins | |
| HU220079B (en) | Method of producing starch decomposition products and the use of this method | |
| WO2002030219A1 (en) | Dietary fibers and oligosaccharides from ginseng and process for preparation thereof | |
| JPH04261401A (en) | Water-soluble celurose acetate and preparation thereof | |
| JP5777634B2 (en) | Coffee processing method | |
| CN111234040A (en) | Preparation method and application of urea modified starch | |
| Bai et al. | Synthesis of octenylsuccinic‐anhydride‐modified cassava starch in supercritical carbon dioxide | |
| JPH08140585A (en) | Production of low-molecular potato protein | |
| JP2010106068A (en) | New chemical modification method for polysaccharide | |
| JPWO2008004530A1 (en) | Hyaluronic acid or its salt powder and method for producing the same | |
| CN108157582A (en) | It is a kind of that the method for improving sesame protein gelation is modified using immobilised enzymes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20060223 |
|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20060223 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20090908 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20100216 |