JPH0425501A - Production of low-viscosity carboxymethylcellulose sodium salt - Google Patents
Production of low-viscosity carboxymethylcellulose sodium saltInfo
- Publication number
- JPH0425501A JPH0425501A JP13047490A JP13047490A JPH0425501A JP H0425501 A JPH0425501 A JP H0425501A JP 13047490 A JP13047490 A JP 13047490A JP 13047490 A JP13047490 A JP 13047490A JP H0425501 A JPH0425501 A JP H0425501A
- Authority
- JP
- Japan
- Prior art keywords
- viscosity
- hydrogen peroxide
- reaction
- cmc
- salt
- 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
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 8
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 5
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 claims description 3
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 12
- 229920000084 Gum arabic Polymers 0.000 abstract description 6
- 241000978776 Senegalia senegal Species 0.000 abstract description 6
- 239000000205 acacia gum Substances 0.000 abstract description 6
- 235000010489 acacia gum Nutrition 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 6
- 239000012530 fluid Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 239000003995 emulsifying agent Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 22
- 238000000034 method Methods 0.000 description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 239000008186 active pharmaceutical agent Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 229920003086 cellulose ether Polymers 0.000 description 3
- 239000012433 hydrogen halide Substances 0.000 description 3
- 229910000039 hydrogen halide Inorganic materials 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 125000002057 carboxymethyl group Chemical class [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229940105329 carboxymethylcellulose Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明は低粘度カルボキシメチルセルロースナトリウム
の製造方法に関する。詳しくはカルボキシメチルセルロ
ースナトリウム(以下CMCNaと略記する)に過酸化
水素を混合し、固相状態にて低粘度CM C−N aを
製造する方法において、効率よくニュートン流体のレオ
ロジー特性を持ち、且つ高濃度溶解可能なアラビアガム
類似の低粘度CM C−N aを製造する方法に関する
。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for producing low viscosity sodium carboxymethylcellulose. In detail, in the method of mixing hydrogen peroxide with carboxymethyl cellulose sodium (hereinafter abbreviated as CMCNa) and producing low-viscosity CMC-Na in a solid state, it efficiently has the rheological properties of a Newtonian fluid and has high The present invention relates to a method for producing low viscosity CM C-Na similar to gum arabic which can be dissolved in concentration.
(従来の技術)
従来低粘度セルロース誘導体を製造する方法は種々提案
されている。(Prior Art) Various methods for producing low-viscosity cellulose derivatives have been proposed.
例えば粉末状の水溶性セルロースエーテルにハロゲン化
水素ガス、ハロゲン化水素を脂肪族アルコールに吸収さ
せたもの、または塩化水素水溶液を接触させる方法(特
公昭4g−41037、特開昭6225101公報)が
開示されている。For example, a method is disclosed in which a powdered water-soluble cellulose ether is brought into contact with hydrogen halide gas, hydrogen halide absorbed into an aliphatic alcohol, or an aqueous hydrogen chloride solution (Japanese Patent Publication No. 4g-41037, 1983, Japanese Patent Application Laid-Open No. 6225101). has been done.
また別の方法は粉末状のCMC−Naに晒粉粉末を用い
て低粘化させる方法(特公昭5g−31081公報)か
開示されている。Another method is disclosed in which powdered CMC-Na is made to have a low viscosity by using bleaching powder (Japanese Patent Publication No. 5G-31081).
また別の方法は乾燥状、湿潤状のセルロースエーテルに
オゾンと酸素または空気の混合物を作用させて反応させ
る方法(特開昭55−145701公報)が開示されて
いる。Another method is disclosed (Japanese Unexamined Patent Publication No. 145701/1983) in which dry or wet cellulose ether is reacted with a mixture of ozone and oxygen or air.
また別の方法は固形の水溶性セルロース誘導体にγ線を
照射する方法(特公昭47−3964.41−3965
公報)が開示されている。Another method is to irradiate solid water-soluble cellulose derivatives with gamma rays (Japanese Patent Publication No. 47-3964.41-3965).
(Government) has been disclosed.
また別の方法は粉体状または湿潤状のセルロースエーテ
ルに過酸化水素を反応させて低粘化させる方法(特公昭
45−678、特公昭48−19232公報)が開示さ
れている。Another method is disclosed in which powdered or wet cellulose ether is reacted with hydrogen peroxide to reduce the viscosity (Japanese Patent Publication No. 45-678, Japanese Patent Publication No. 48-19232).
(発明が解決しようとする課題)
しかし、以上の方法も低粘度CM C−N aを製造す
る場合いろいろ欠点を有している。(Problems to be Solved by the Invention) However, the above methods also have various drawbacks when producing low viscosity CMC-Na.
ハロゲン化水素を用いてCMC−Naを低粘化させる方
法は、CM C−N aの一部が水不溶性の酸型カルボ
キシメチルセルロースになりゲル状の不溶解物ができや
すい欠点がある。The method of lowering the viscosity of CMC-Na using hydrogen halide has the drawback that a portion of CMC-Na becomes water-insoluble acid type carboxymethylcellulose, resulting in the formation of gel-like insoluble matter.
晒粉粉末を用いる方法では、低粘化したCMC−Naを
食品、医薬品等に使用する場合、副生成物を除去するた
めに精製処理が必要となる。In the method using bleached powder, when the reduced viscosity CMC-Na is used for foods, medicines, etc., purification treatment is required to remove by-products.
また、オゾンを作用させる方法とγ線を照射する方法は
、特別な装置を必要とするためコスト高となり、装置の
維持管理も容易でない。Furthermore, the method of applying ozone and the method of irradiating with gamma rays require special equipment, resulting in high costs, and the maintenance of the equipment is not easy.
これらの方法に比し、CM C−N aに過酸化水素を
反応させて低粘化する方法は、不溶解性ゲルや副生物の
生成がなく、簡単な混合装置のみて製造可能な優れた方
法であるか、従来開示された方法では、大量の過酸化水
素を使用しても30%水溶液の粘度が100〜1000
0cpsの超低粘CM C−N aを工業的に製造する
のは困難であった。Compared to these methods, the method of reducing viscosity by reacting hydrogen peroxide with CMC-Na is an excellent method that does not produce insoluble gels or by-products and can be produced using only a simple mixing device. In the conventionally disclosed method, even if a large amount of hydrogen peroxide is used, the viscosity of a 30% aqueous solution is 100 to 1000.
It was difficult to industrially produce ultra-low viscosity CM C-Na of 0 cps.
本発明者らはCM C−N aに過酸化水素を反応させ
て低粘化する方法により、効率よく超低粘CMC−Na
を製造する方法について鋭意研究を重ねた結果、反応系
のPHの調整が重要であることを見出だし、この知見に
基づいて本発明をなすに至った。The present inventors efficiently produced ultra-low viscosity CMC-Na by reacting hydrogen peroxide with CMC-Na to reduce the viscosity.
As a result of extensive research on the method for producing , it was discovered that adjusting the pH of the reaction system is important, and based on this knowledge, the present invention was developed.
(課題を解決するための手段)
本発明は、カルボキシメチルセルロースナトリウムに過
酸化水素を混合して加温し、固相状態にて低粘度カルボ
キシメチルセルロースナトリウムを製造する方法におい
て、反応系のPHを6.5〜3.0に保ちながら反応さ
せることを特徴とする低粘度カルボキシメチルセルロー
スナトリウムの製造方法である。(Means for Solving the Problems) The present invention is a method for producing low-viscosity sodium carboxymethylcellulose in a solid state by mixing hydrogen peroxide with sodium carboxymethylcellulose and heating the mixture, in which the pH of the reaction system is reduced to 6. This is a method for producing low viscosity carboxymethylcellulose sodium, characterized by carrying out the reaction while maintaining the viscosity at .5 to 3.0.
本発明の原料となるC M C−N aは、特に限定さ
れるものではなく、カルボキシメチル基の平均置換度(
以下DSと略す)が0.6〜3.1%水溶液の粘度が1
0〜10000cpsの通常のCM C−N aを用い
ることができる。低粘度のCMCを原料とするほうが低
粘化に有利であることは言うまでもないが、DSは1.
0以上のものが好ましい。DSが1.0以下のCM C
−N aを原料とする場合は、低粘化効率が低い上に得
られた低粘CMC−Naは構造粘性を有し、アラビヤガ
ムに似たニュートン流に近いレオロジー特性を持つCM
C−N aを得るのが難しい。CMC−Naは製造工
程中のものでも製品でもよいが、実質上乾燥した粉状又
は粒状のものが望ましい。CMC-Na, which is the raw material of the present invention, is not particularly limited, and the average degree of substitution of carboxymethyl groups (
(hereinafter abbreviated as DS) has a viscosity of 0.6 to 3.1% aqueous solution of 1
A normal CM C-Na of 0-10000 cps can be used. It goes without saying that using CMC with low viscosity as a raw material is more advantageous in reducing the viscosity, but DS is 1.
It is preferably 0 or more. CM C with DS of 1.0 or less
- When Na is used as a raw material, the low viscosity reduction efficiency is low, and the obtained low viscosity CMC-Na has structural viscosity and has rheological properties close to Newtonian flow similar to gum arabic.
Difficult to obtain C-N a. CMC-Na may be used in the manufacturing process or as a product, but it is preferably in the form of a substantially dry powder or granules.
本発明において過酸化水素の反応時のPHの調整が重要
であり、反応系のPHを6.5〜3,0の範囲、好まし
くは6.0〜4.5の範囲にすることが必要がある。P
Hが6.5以上になると低粘化効率が悪くなり、3.0
以下になるとゲル状の水不溶解物が生成しやすくなる。In the present invention, it is important to adjust the pH during the reaction of hydrogen peroxide, and it is necessary to keep the pH of the reaction system in the range of 6.5 to 3.0, preferably in the range of 6.0 to 4.5. be. P
When H is 6.5 or more, the low viscosity efficiency deteriorates, and 3.0
Below that, gel-like water-insoluble substances tend to form.
先行技術の特公昭48−19232公報には、PHが約
8〜11の温和なアルカリ条件のもとて過酸化物による
酸化は、大変効果的であると記載されているが、われわ
れが検討した結果PH6,5以上では低粘化効率が反っ
て悪くなることを明らかにした。これはアルカリ条件下
では過酸化水素の分解による活性酸素の発生はよくなる
が、大気中への飛散か多くなり低粘化効率が反って悪く
なるものと考えられる。The prior art, Japanese Patent Publication No. 48-19232, states that oxidation with peroxide under mild alkaline conditions with a pH of approximately 8 to 11 is very effective; The results revealed that at pH 6.5 or higher, the viscosity-lowering efficiency deteriorates. This is thought to be because under alkaline conditions, the generation of active oxygen through the decomposition of hydrogen peroxide is better, but more is scattered into the atmosphere, which deteriorates the viscosity-lowering efficiency.
過酸化水素の反応時のPHの調整は、酸を直接反応系に
添加してもよいが、過酸化水素水溶液に酸を予め添加す
ることによって行うこともてきる。The pH during the hydrogen peroxide reaction may be adjusted by adding the acid directly to the reaction system, but it can also be done by adding the acid to the hydrogen peroxide aqueous solution in advance.
PH副調整使用する酸は、各種の無機酸、有機酸が使用
できるが、酢酸を用いるのがPHの調整が容易で好まし
い。Although various inorganic acids and organic acids can be used as the acid for sub-adjustment of PH, acetic acid is preferably used because the PH can be easily adjusted.
本発明においては、反応開始時の混合物の水分を17〜
10重量%、好ましくは15〜12重量%の範囲に保つ
ことが望ましい。反応開始時の混合物の水分が17重量
%以上の場合は、低粘化が進むにつれて反応装置内の粉
体または粒体の団粒化が起こり、直径1〜10cmの塊
状になり粉状または粒状の状態を保てなくなる。このよ
うになると塊の中が反応熱により局部的に高温になり、
反応が不均一となり、また発火したりして危険な状態と
なる。また反応装置側壁にCM C−N aが付着して
積層板状となり、混合羽根に接触して装置の運転に支障
をきたすことになる。逆に反応開始時の混合物の水分が
10重量%以下の場合は低粘化効率が悪くなるので望ま
しくない。In the present invention, the water content of the mixture at the start of the reaction is 17 to
It is desirable to keep it in the range of 10% by weight, preferably 15-12% by weight. If the water content of the mixture at the start of the reaction is 17% by weight or more, as the viscosity decreases, the powder or granules in the reactor will aggregate, forming lumps with a diameter of 1 to 10 cm, and forming powder or granules. It becomes impossible to maintain the state of When this happens, the inside of the lump becomes locally high temperature due to the heat of reaction,
The reaction may become uneven and may ignite, creating a dangerous situation. In addition, CMC-N a adheres to the side walls of the reactor and forms a laminated plate, which comes into contact with the mixing blades and interferes with the operation of the reactor. On the other hand, if the water content of the mixture at the start of the reaction is less than 10% by weight, this is undesirable because the viscosity reduction efficiency will be poor.
過酸化水素の添加、加熱処理については、従来公知の方
法を用いればよい。過酸化水素は通常30〜40重量%
水溶液として使用する。反応装置で原料の粉状又は粒状
のCMC−Naを混合攪拌しつつ、乾燥CM C−N
aに対し0.1〜0.5重量%の過酸化水素を一度に又
は何回かに分けてスプレーした後、添加した過酸化水素
が反応するのに十分な時間60〜150℃に加熱混合し
低粘CM C−N aを得る。For addition of hydrogen peroxide and heat treatment, conventionally known methods may be used. Hydrogen peroxide is usually 30-40% by weight
Use as an aqueous solution. While mixing and stirring raw material powder or granular CMC-Na in a reaction device, dry CM C-N
After spraying 0.1 to 0.5% by weight of hydrogen peroxide to a at once or in several batches, heat and mix at 60 to 150°C for a sufficient time for the added hydrogen peroxide to react. to obtain a low viscosity CM C-Na.
(発明の効果)
本発明の方法は低粘化効率が高く、従来製造困難であっ
た30重量%水溶液の粘度が100〜10000cps
でニュートン流体に近いレオロジー特性をもったアラビ
アガム類似の超低粘CM C−N aを工業的に製造す
る方法を提供するものである。アラビアガムは天然品ゆ
えに天候により生産量、品質か一定せず産業界ではその
代替品か待望されていたが本発明によりこの問題が解決
されることになる。(Effect of the invention) The method of the present invention has high viscosity reduction efficiency, and the viscosity of a 30% aqueous solution, which was difficult to produce in the past, is 100 to 10,000 cps.
The present invention provides a method for industrially producing ultra-low viscosity CMC-Na similar to gum arabic and having rheological properties close to Newtonian fluids. Since gum arabic is a natural product, its production volume and quality are not constant depending on the weather, and the industry has long been looking for a substitute for it.This problem will be solved by the present invention.
本発明の方法は低粘化効率か高く少量の過酸化水素で低
粘化できるので、製造工程における危険性が低く、また
過酸化水素の分解により生成する水が少ないのて、粉体
又は粒体の団粒化ないし塊状化が起りにくく工業生産に
適している。The method of the present invention has a high viscosity efficiency and can reduce viscosity with a small amount of hydrogen peroxide, so there is less danger in the manufacturing process, and since less water is produced by decomposing hydrogen peroxide, powder or granules can be produced. It is suitable for industrial production because it is unlikely to cause agglomeration or clumping.
(実施例)
以下本発明の実施例を示すが本発明はこれらに限定され
るものではない。(Examples) Examples of the present invention will be shown below, but the present invention is not limited thereto.
実施例1,2および比較例1、参考例
DSの異なるC M C−N a 1 、 5 kgを
ブレンダーに仕込み、70〜80℃に加温し、酢酸にて
初期PHを6.5以下に調節したのち、35%濃度の過
酸化水素水溶液200 mlを3回に分けて添加し低粘
化反応をおこなった。3回に分けたのは反応開始時の水
分を17〜10重量%にするためである。その結果が表
1である。この結果からもわかるように DSが1.0
以下の比較例1では、10重量%濃度では同じ位の粘度
であっても30重量%濃度では非常に異なった粘度をし
めずことがわかる。また30重量%濃度における流動特
性をみると、回転粘度計による回転数6 Orpmにお
ける粘度と回転数6 rpmにおける粘度の比であるP
VI値か参考のアラビアガムと比較して大きな開きがあ
るが、DSが1.0以上の実施例1.2では同じ数値を
示していることがわかる。Examples 1 and 2, Comparative Example 1, and Reference Example 5 kg of CMC-N a 1 with different DS were placed in a blender, heated to 70 to 80°C, and the initial pH was adjusted to 6.5 or less with acetic acid. After adjustment, 200 ml of a 35% hydrogen peroxide aqueous solution was added in three portions to perform a viscosity reduction reaction. The reason why the reaction was divided into three times was to adjust the water content at the start of the reaction to 17 to 10% by weight. Table 1 shows the results. As you can see from this result, DS is 1.0
In Comparative Example 1 below, it can be seen that even if the viscosity is about the same at a concentration of 10% by weight, the viscosity is not very different at a concentration of 30% by weight. In addition, looking at the flow characteristics at a concentration of 30% by weight, P is the ratio of the viscosity at a rotational speed of 6 orpm and the viscosity at a rotational speed of 6 rpm measured by a rotational viscometer.
It can be seen that although there is a large difference in VI value compared to the reference gum arabic, Example 1.2 with a DS of 1.0 or more shows the same value.
以下余白
実施例3,4.5および比較例2
DSが1.55.2重量%濃度水溶液の粘度が445
cpsのCMC−Na2kgをブレンダーニ仕込み、7
0〜80℃に加温し、酢酸の添加量を変えて初期PHを
変えたのち、35%濃度の過酸化水素水溶液120 m
lを3回にわけて添加し低粘化反応をおこなった。反応
を進めていくとPHが下がってくるが、比較例2ではP
Hを7.0以上に保つために炭酸ナトリウム水溶液で調
節しながら反応を行なった。その結果が表2である。こ
の結果からもわかるように反応系のPHが7.0以上の
比較例2は、PH6,5以下の実施例3,4゜5に比べ
同量の過酸化水素を使用しても低粘度CMC−Naの粘
度が高く反応効率が悪いことがわかる。The following margins Examples 3, 4.5 and Comparative Example 2 DS is 1.55.2% by weight aqueous solution has a viscosity of 445
Add 2 kg of cps CMC-Na to blender, 7
After heating to 0 to 80°C and changing the initial pH by changing the amount of acetic acid added, 120 m of a 35% hydrogen peroxide aqueous solution was added.
A viscosity-lowering reaction was carried out by adding 1 in 3 portions. As the reaction progresses, the pH decreases, but in Comparative Example 2, the P
The reaction was carried out while controlling with an aqueous sodium carbonate solution to maintain H at 7.0 or higher. Table 2 shows the results. As can be seen from this result, Comparative Example 2, in which the pH of the reaction system was 7.0 or higher, had a lower viscosity than CMC, even when using the same amount of hydrogen peroxide, compared to Examples 3 and 4.5, in which the pH of the reaction system was 6.5 or lower. It can be seen that the viscosity of -Na is high and the reaction efficiency is low.
以下余白
実施例6および比較例3
DSが1.54.2重量%濃度水溶液の粘度が91.0
cps、水分9.9重量%のCM C−N a2.5k
gをブレンダーに仕込み、70〜80℃に加温し、酢酸
にて初期PHを7,0以下に調節したのち35%濃度の
過酸化水素水溶液120m1を添加し低粘化反応をおこ
なった。実施例6は過酸化水素水溶液を3回に分けて添
加したが、比較例3は一度に添加した。その結果反応開
始時の水分は表3のようになった。表3の結果からもわ
かるように反応開始時の水分が17重量%以上では反応
途中で塊状物が生成し、また反応装置側壁にCMC−N
aが付着し、積層板状となり最終的には混合羽根が動か
なくなった。しかし反応開始時の水分が17重量%以下
の場合はそのようなことがなく、順調に最後まで混合で
き低粘化CMC−Naを製造することが出来た。The following margins Example 6 and Comparative Example 3 DS is 1.54.2% by weight aqueous solution has a viscosity of 91.0
cps, CM C-N a2.5k with moisture 9.9% by weight
g was placed in a blender, heated to 70 to 80°C, and the initial pH was adjusted to 7.0 or less with acetic acid, and then 120 ml of a 35% hydrogen peroxide aqueous solution was added to perform a viscosity-lowering reaction. In Example 6, the aqueous hydrogen peroxide solution was added in three parts, but in Comparative Example 3, it was added all at once. As a result, the water content at the start of the reaction was as shown in Table 3. As can be seen from the results in Table 3, when the water content at the start of the reaction is 17% by weight or more, lumps are formed during the reaction, and CMC-N
a adhered to it, forming a laminated plate shape, and eventually the mixing blade stopped moving. However, when the water content at the start of the reaction was 17% by weight or less, this did not occur, and the mixture could be mixed smoothly to the end, and low-viscosity CMC-Na could be produced.
以下余白 = =Margin below = =
Claims (1)
混合して加温し、固相状態にて低粘度カルボキシメチル
セルロースナトリウムを製造する方法において、反応系
のPHを6.5〜3.0に保ちながら反応させることを
特徴とする低粘度カルボキシメチルセルロースナトリウ
ムの製造方法。In a method for producing low-viscosity sodium carboxymethylcellulose in a solid state by mixing hydrogen peroxide with sodium carboxymethylcellulose and heating the mixture, the reaction is carried out while maintaining the pH of the reaction system between 6.5 and 3.0. Characteristic method for producing low viscosity carboxymethyl cellulose sodium.
Priority Applications (1)
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---|---|---|---|
JP13047490A JP2800061B2 (en) | 1990-05-21 | 1990-05-21 | Method for producing low viscosity sodium carboxymethyl cellulose |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13047490A JP2800061B2 (en) | 1990-05-21 | 1990-05-21 | Method for producing low viscosity sodium carboxymethyl cellulose |
Publications (2)
Publication Number | Publication Date |
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JPH0425501A true JPH0425501A (en) | 1992-01-29 |
JP2800061B2 JP2800061B2 (en) | 1998-09-21 |
Family
ID=15035113
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JP13047490A Expired - Fee Related JP2800061B2 (en) | 1990-05-21 | 1990-05-21 | Method for producing low viscosity sodium carboxymethyl cellulose |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04306245A (en) * | 1990-07-02 | 1992-10-29 | Aqualon Co | High-solid, low-viscosity polysaccharide composition |
JP2002531593A (en) * | 1998-11-27 | 2002-09-24 | ヴオルフ・ヴアルスロデ・アクチエンゲゼルシヤフト | Method for producing low viscosity water-soluble cellulose ether |
JP2006241374A (en) * | 2005-03-04 | 2006-09-14 | Dai Ichi Kogyo Seiyaku Co Ltd | Process for producing carboxymethyl cellulose salt |
CN102367279A (en) * | 2011-10-18 | 2012-03-07 | 杭州弘博化工有限公司 | Preparation method of ultralow-viscosity sodium carboxymethyl cellulose |
CN114773489A (en) * | 2022-05-19 | 2022-07-22 | 浙江三和食品科技有限公司 | Preparation method of low-viscosity sodium carboxymethylcellulose |
-
1990
- 1990-05-21 JP JP13047490A patent/JP2800061B2/en not_active Expired - Fee Related
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04306245A (en) * | 1990-07-02 | 1992-10-29 | Aqualon Co | High-solid, low-viscosity polysaccharide composition |
JP2002531593A (en) * | 1998-11-27 | 2002-09-24 | ヴオルフ・ヴアルスロデ・アクチエンゲゼルシヤフト | Method for producing low viscosity water-soluble cellulose ether |
JP2006241374A (en) * | 2005-03-04 | 2006-09-14 | Dai Ichi Kogyo Seiyaku Co Ltd | Process for producing carboxymethyl cellulose salt |
CN102367279A (en) * | 2011-10-18 | 2012-03-07 | 杭州弘博化工有限公司 | Preparation method of ultralow-viscosity sodium carboxymethyl cellulose |
CN114773489A (en) * | 2022-05-19 | 2022-07-22 | 浙江三和食品科技有限公司 | Preparation method of low-viscosity sodium carboxymethylcellulose |
CN114773489B (en) * | 2022-05-19 | 2023-02-24 | 浙江三和食品科技有限公司 | Preparation method of low-viscosity sodium carboxymethylcellulose |
Also Published As
Publication number | Publication date |
---|---|
JP2800061B2 (en) | 1998-09-21 |
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