JP3742608B2 - Low viscosity method of low viscosity sodium carboxymethyl cellulose aqueous solution - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、カルボキシメチルセルロースナトリウム（以下、ＣＭＣ−Ｎａという）水溶液を低粘度化する方法に関する。
【０００２】
【従来の技術】
ＣＭＣ−Ｎａ水溶液は、粘稠性のある水溶液であり、そのために有用な水溶液である。しかし、たとえば、Ｘ線造影剤の硫酸バリウム分散剤、石膏ボード加工時における炭酸カルシウム分散剤などの用途において低粘度のＣＭＣ−Ｎａ水溶液が好まれるように、低粘度のＣＭＣ−Ｎａ水溶液が必要とされる場合もある。
【０００３】
市販されているＣＭＣ−Ｎａには、１０重量％水溶液としたときの粘度が１０００ｍＰａ・ｓ以下の製品もあるが、目的とする低粘度の水溶液を得るためには、市販品を用いるだけでは充分ではない状況である。
【０００４】
また、水溶液中のＣＭＣ−Ｎａ濃度を下げることによって目的とする低粘度水溶液を得ることができるが、この場合には水溶液中のＣＭＣ−Ｎａ固形分が減少するために、実際に使用する場合に組成の変動が生じるなどの問題がある。
【０００５】
【発明が解決しようとする課題】
本発明では、ＣＭＣ−Ｎａ水溶液を低粘度化する方法において、ＣＭＣ−Ｎａ濃度を下げることなく、ＣＭＣ−Ｎａ水溶液の粘度を低下させる方法を提供することを目的とする。
【０００６】
【課題を解決するための手段】
本発明は、１０重量％水溶液粘度が１００００ｍＰａ・ｓ以下の低粘度であるＣＭＣ−Ｎａの水溶液にポリビニルピロリドン（以下、ＰＶＰという）を配合することを特徴とするＣＭＣ−Ｎａ水溶液の低粘度化法、
ＣＭＣ−Ｎａの１０重量％水溶液粘度が１０００ｍＰａ・ｓ以下である前記の低粘度化法、および
ＰＶＰの配合量がＣＭＣ−Ｎａに対して０．１〜２０重量％である前記の低粘度化法
に関する。
【０００７】
本発明においては、低粘度ＣＭＣ−Ｎａ水溶液の粘度を、ＣＭＣ−Ｎａの固形分量を下げることなく、さらに低下させることができる。
【０００８】
【発明の実施の形態】
本発明のＣＭＣ−Ｎａ水溶液の低粘度化は、ＣＭＣ−Ｎａ水溶液にＰＶＰを配合することにより行なわれる。
【０００９】
本発明で使用されるＣＭＣ−Ｎａは、通常、２５℃における１０重量％水溶液の粘度が２０〜１００００ｍＰａ・ｓのものである。２０ｍＰａ・ｓ未満では本発明の低粘度化法を使用する必要がなく、１００００ｍＰａ・ｓをこえると低粘度で使用する際にＣＭＣ−Ｎａ濃度を下げて使用しなければならない。低粘度品をより低粘度化させた低粘度品を得ることを目的とする本発明においては、１０００ｍＰａ・ｓ以下のものを使用することが好ましい。
【００１０】
本発明で使用されるＣＭＣ−Ｎａのエーテル化度は、好ましくは０．５〜２．０、より好ましくは０．７〜１．５である。０．５未満ではＣＭＣ−Ｎａ水溶液の透明性が低下し、２．０をこえると、とくに支障はないが、ＣＭＣ−Ｎａの価格が高いなどの問題が生じる。
【００１１】
本発明で使用されるＣＭＣ−Ｎａとしては市販品を用いることができ、たとえば、第一工業製薬（株）製のセロゲンＦ−７Ａ、Ｆ−５Ａなどを用いることができる。
【００１２】
本発明で使用されるＰＶＰとしては、Ｋ値がおよそ１５〜１０３のものが市販されており、これらを使用することができる。市販品の具体例としては、たとえば、ＢＡＳＦ社製のＬｕｖｉｓｋｏｌ Ｋ−１７（パウダー、Ｋ値１５〜１９、１０重量％水溶液のｐＨ３．０〜７．０）、Ｌｕｖｉｓｋｏｌ Ｋ−３０（パウダー、Ｋ値２７〜３３、１０重量％水溶液のｐＨ３．０〜７．０）、Ｌｕｖｉｓｋｏｌ Ｋ−８０（パウダー、Ｋ値７４〜８２、１０重量％水溶液のｐＨ５．０〜８．０）、Ｌｕｖｉｓｋｏｌ Ｋ−９０（パウダー、Ｋ値８８〜９６、１０重量％水溶液のｐＨ５．０〜９．０）、Ｌｕｖｉｓｋｏｌ Ｋ−３０（約３０重量％水溶液、Ｋ値２７〜３３、１０重量％水溶液のｐＨ７．０〜９．０）、Ｌｕｖｉｓｋｏｌ Ｋ−６０（約４５重量％水溶液、Ｋ値５２〜６２、１０重量％水溶液のｐＨ７．０〜９．０）、Ｌｕｖｉｓｋｏｌ Ｋ−８５（約２０重量％水溶液、Ｋ値８３〜８８、１０重量％水溶液のｐＨ７．０〜９．０）、Ｌｕｖｉｓｋｏｌ Ｋ−９０（約２０重量％水溶液、Ｋ値９０〜１０３、１０重量％水溶液のｐＨ７．０〜９．０）などがあげられる。これらは１種で用いてもよく、２種以上を組み合わせて用いてもよい。
【００１３】
前記Ｋ値は、ドイツの化学者フィケンチャー（Fikentscher）により提案された重合度を表わす定数であり、次式より得られる。次式は、とくに天然高分子の溶液について広い範囲でよく成立するものである。
【００１４】
【数１】
上記式中、Ｃは試料（ＰＶＰ）の濃度（％：ｇ／１００ｍｌ）を示す。相対粘度ηrelは次式より得られる。各流動時間は、ウベローデ型粘度計により、２５℃で測定される値である。
ηrel＝１％ＰＶＰ水溶液の流動時間／水の流動時間
【００１６】
ＰＶＰは、ＣＭＣ−Ｎａ１００重量％に対して、０．１〜２０重量％、好ましくは０．２〜１０重量％、より好ましくは０．２〜５重量％配合される。０．１重量％未満ではＰＶＰを使用する効果を得ることができず、２０重量％をこえると水溶液中のＣＭＣ−Ｎａ自体の濃度が低下してしまうため好ましくない。
【００１７】
ＰＶＰを含有するＣＭＣ−Ｎａ水溶液の調製方法としては、たとえば、ＣＭＣ−ＮａとＰＶＰとの混合物を水に溶解させる方法、ＣＭＣ−Ｎａ水溶液にＰＶＰを溶解させる方法およびＣＭＣ−Ｎａ水溶液にＰＶＰ水溶液を配合させる方法などがあり、いずれの方法を用いてもよい。また、ＣＭＣ−ＮａおよびＰＶＰを水に溶解させる際には、たとえば、攪拌機を用いて溶解させる方法、自然放置により溶解させる方法および加熱により溶解させる方法などがあり、いずれの方法を用いてもとくに問題はない。
【００１８】
本発明により調製されたＰＶＰを含有するＣＭＣ−Ｎａ水溶液の粘度は、ＰＶＰを含有しないときに比べて低くなる。ＣＭＣ−Ｎａ水溶液中のＣＭＣ−Ｎａ分子間の摩擦がＰＶＰによって減少するために、水溶液の粘度が低下するものと考えられる。
【００１９】
本発明で得られる低粘度のＣＭＣ−Ｎａ水溶液は、一般工事用、医薬用、化粧品用などとして有用に使用されることができる。たとえば、本発明の低粘度ＣＭＣ−Ｎａ水溶液をＸ線造影用硫酸バリウム分散剤として用いた場合には、低粘度であるために服用が容易であるとともに、消化管の微細な胃・腸壁内部にまで造影剤粒子が均一に付着し、正確な造影を可能にすることができる。
【００２０】
【実施例】
実施例１〜９、比較例１〜６
使用するＣＭＣ−Ｎａ（第一工業製薬（株）製、１０重量％水溶液粘度が１０００ｍＰａ・ｓ以下のものを使用）のエーテル化度および２５℃における１０重量％水溶液粘度を下記のようにして測定した。また、所定量のＣＭＣ−ＮａおよびＰＶＰ（ＢＡＳＦ社製「Ｌｕｖｉｓｋｏｌ Ｋ−３０」、数平均分子量≒１万、Ｋ値＝２７．０〜３３．０）の混合物を水に溶解させることにより、表１に示す量のＰＶＰを含むＣＭＣ−Ｎａ水溶液を調製した。ＣＭＣ−Ｎａのエーテル化度、ＰＶＰ添加前後の１０重量％水溶液粘度を測定した結果を表１に示す。
【００２１】
＜エーテル化度＞
ＣＭＣ−Ｎａ約１ｇを精秤し、濾紙に包んで磁性るつぼの中に入れ、６００℃で灰化し、生成した水酸化ナトリウムを０．１Ｎの硫酸によりフェノールフタレインを指示薬として滴定し、中和滴定に要した硫酸量Ａ（ｍｌ）と０．１Ｎの硫酸の力価ｆ3を用いてＣＭＣ−Ｎａのエーテル化度を計算する。
エーテル化度＝ １６２×Ａ×ｆ3／（１００００−８０×Ａ×ｆ3）
【００２２】
＜１０重量％水溶液粘度＞
【００２３】
▲１▼水分率の測定
試料（ＣＭＣ−Ｎａ）１〜２ｇを秤量瓶に精秤し、１０５±０．２℃の乾燥機中において２時間乾燥し、乾燥による減量から水分率を次式により求める。
水分率（％）＝ 減量（ｇ）／試料（ｇ） × １００
【００２４】
▲２▼粘度の測定
３００ｍｌトールビーカーに約２５ｇの試料（ＣＭＣ−Ｎａ）を精秤し、次式により求められる１０重量％水溶液を得るために必要な溶解水量の水を加えてガラス棒にて分散させる。
溶解水量（ｇ）＝ 試料（ｇ）×（９０−水分率（％））
得られる水溶液を一昼夜放置し、マグネチックスターラーで約５分間攪拌して均一な溶液とする。２５℃の恒温槽に３０分間入れて溶液を２５℃としたのち、ガラス棒で穏やかにかき混ぜ、ＢＭ型粘度計（（株）トキメック製）を用い、ローターおよびガードを取り付け、回転数６０ｒｐｍで回転させて３分後の目盛りを読み取る。
粘度（ｍＰａ・ｓ）＝ 読み取り目盛 × 係数
【００２５】
【表１】
実験例１〜９、比較実験例１〜６
実施例１〜９で得られる低粘度化したＣＭＣ−Ｎａ水溶液および比較例１〜６で得られるＣＭＣ−Ｎａ水溶液をＸ線造影剤用の硫酸バリウム分散剤として用いたときの効果について評価した。
【００２７】
水１４４ｍｌにＣＭＣ−Ｎａ２．４ｇおよびＣＭＣ−Ｎａに対して表１に示す配合量となるＰＶＰを溶解させたのち、硫酸バリウム（試薬１級）２４０ｇを加え、ホモミキサーを用いて８０００ｒｐｍで２分間攪拌分散させ、試験用造影剤を得た。
【００２８】
得られた試験用造影剤について、下記の（ａ）〜（ｃ）の条件における人工胃液添加時の粘度変化および安定性の評価を行なった。
【００２９】
＜人工胃液添加時の粘度変化＞
（ａ）造影剤１００ｍｌに人工胃液（塩酸（試薬１級）１５ｍｌを蒸留水で１０００ｍｌに希釈）１３ｍｌを加えてよく攪拌する。得られた懸濁液１００ｍｌをトールビーカーにとり、２５℃の恒温槽中に３０分間放置したのち、Ｂ型粘度計（東京計器工業（株）製）を用い、ローターを２号および３号、回転数を６０ｒｐｍとして回転させ、３分後の粘度を測定する。
粘度（ｍＰａ・ｓ）＝ 読み取り目盛 × 係数
（ｂ）造影剤１００ｍｌに人工胃液（塩酸２５ｍｌを蒸留水で１０００ｍｌに希釈）１３ｍｌを加えてよく攪拌する。得られる懸濁液について、（ａ）と同様の条件で測定を行なう。
（ｃ）造影剤１００ｍｌに水１３ｍｌを加えてよく攪拌する。得られる懸濁液について、（ａ）と同様の条件で測定を行なう。
【００３０】
＜安定性＞
試験用造影剤１００ｍｌを１００ｍｌメスシリンダーに入れて静置し、１０日後の上澄液の容量を測定する。
【００３１】
【表２】
表１において、ＣＭＣ−Ｎａ水溶液にＣＭＣ−Ｎａに対して０．５〜１０重量％のＰＶＰを配合した実施例１〜９の１０重量％水溶液粘度は、使用するＣＭＣ−Ｎａのエーテル化度および１０重量％水溶液の粘度にかかわらず、ＰＶＰ配合前（比較例１、３、５）の粘度より低下することがわかる。また、ＣＭＣ−Ｎａに対して２５重量％のＰＶＰを配合した比較例２、４、６の結果より、ＰＶＰの配合量が多いときには、配合後の水溶液粘度が配合前の粘度に比べて高くなることがわかる。
【００３３】
表２より、ＣＭＣ−Ｎａ水溶液を含有するＸ線造影剤に人工胃液を添加した場合にも、ＰＶＰの配合によって粘度が低下しており、ＣＭＣ−Ｎａ水溶液をＸ線造影剤に添加する場合にもＰＶＰの配合が有効であることがわかる。また、Ｘ線造影剤を静置したのちに生じる上澄液の量は、ＰＶＰの有無によって大きな相違がないことから、ＰＶＰの添加がＸ線造影剤の安定性に影響を与えないことがわかる。
【００３４】
【発明の効果】
本発明の方法によれば、１０重量％水溶液粘度が１００００ｍＰａ・ｓ以下であるＣＭＣ−Ｎａの水溶液に、たとえば、ＣＭＣ−Ｎａの０．１〜２０重量％のＰＶＰを配合させることにより、ＣＭＣ−Ｎａ濃度を低下させることなく、水溶液粘度を低下させることができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for reducing the viscosity of an aqueous sodium carboxymethyl cellulose (hereinafter referred to as CMC-Na) solution.
[0002]
[Prior art]
The CMC-Na aqueous solution is a viscous aqueous solution and is a useful aqueous solution for that purpose. However, for example, a low-viscosity CMC-Na aqueous solution is required so that a low-viscosity CMC-Na aqueous solution is preferred in applications such as a barium sulfate dispersant for an X-ray contrast agent and a calcium carbonate dispersant for processing a gypsum board. Sometimes it is done.
[0003]
Commercially available CMC-Na has a product with a viscosity of 1000 mPa · s or less when a 10% by weight aqueous solution is used, but it is sufficient to use a commercially available product in order to obtain a target low-viscosity aqueous solution. Not a situation.
[0004]
Moreover, although the target low-viscosity aqueous solution can be obtained by lowering the CMC-Na concentration in the aqueous solution, in this case, since the CMC-Na solid content in the aqueous solution decreases, There are problems such as variations in composition.
[0005]
[Problems to be solved by the invention]
An object of the present invention is to provide a method for reducing the viscosity of a CMC-Na aqueous solution without lowering the CMC-Na concentration in a method for reducing the viscosity of an aqueous CMC-Na solution.
[0006]
[Means for Solving the Problems]
The present invention relates to a method for reducing the viscosity of an aqueous CMC-Na solution, characterized in that polyvinyl pyrrolidone (hereinafter referred to as PVP) is blended with an aqueous solution of CMC-Na having a low viscosity of 10% by weight aqueous solution of 10,000 mPa · s or less. ,
The viscosity reducing method described above wherein the viscosity of a 10% by weight aqueous solution of CMC-Na is 1000 mPa · s or less, and the method of reducing viscosity described above, wherein the blending amount of PVP is 0.1 to 20% by weight with respect to CMC-Na. About.
[0007]
In the present invention, the viscosity of the low-viscosity CMC-Na aqueous solution can be further reduced without lowering the solid content of CMC-Na.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
The viscosity reduction of the CMC-Na aqueous solution of the present invention is performed by blending PVP with the CMC-Na aqueous solution.
[0009]
CMC-Na used in the present invention usually has a viscosity of 20 to 10,000 mPa · s in a 10 wt% aqueous solution at 25 ° C. If the viscosity is less than 20 mPa · s, it is not necessary to use the method for reducing the viscosity of the present invention. If it exceeds 10000 mPa · s, the CMC-Na concentration must be lowered when used at a low viscosity. In the present invention aiming at obtaining a low-viscosity product in which the low-viscosity product is further reduced, it is preferable to use a product having a viscosity of 1000 mPa · s or less.
[0010]
The degree of etherification of CMC-Na used in the present invention is preferably 0.5 to 2.0, more preferably 0.7 to 1.5. If it is less than 0.5, the transparency of the CMC-Na aqueous solution is lowered, and if it exceeds 2.0, there is no particular problem, but there is a problem that the price of CMC-Na is high.
[0011]
A commercial item can be used as CMC-Na used by this invention, For example, Daigen Kogyo Seiyaku Co., Ltd. cellogen F-7A, F-5A, etc. can be used.
[0012]
As PVP used in the present invention, those having a K value of about 15 to 103 are commercially available, and these can be used. Specific examples of commercially available products include, for example, Luviskol K-17 (powder, K value 15-19, pH 3.0 to 7.0 of a 10 wt% aqueous solution) manufactured by BASF, Luviskol K-30 (powder, K value). 27 to 33, pH 3.0 to 7.0 of 10% by weight aqueous solution), Luviskol K-80 (powder, K value 74 to 82, pH 5.0 to 8.0 of 10% by weight aqueous solution), Luviskol K-90 ( Powder, K value 88-96, pH 5.0-9.0 of 10 wt% aqueous solution), Luviskol K-30 (about 30 wt% aqueous solution, K value 27-33, pH 7.0 of 10 wt% aqueous solution 7.0-9. 0), Luviskol K-60 (about 45 wt% aqueous solution, K value 52-62, pH 7.0 of 10 wt% aqueous solution 7.0-9.0), Luviskol K-85 (about 20 wt% aqueous solution) Solution, K value 83-88, pH 7.0-9.0 of 10 wt% aqueous solution), Luviskol K-90 (about 20 wt% aqueous solution, K value 90-103, pH 7.0 of 10 wt% aqueous solution 7.0-9. 0). These may be used alone or in combination of two or more.
[0013]
The K value is a constant representing the degree of polymerization proposed by German chemist Fikentscher and is obtained from the following equation. The following equation is well established in a wide range especially for natural polymer solutions.
[0014]
[Expression 1]
In the above formula, C represents the concentration (%: g / 100 ml) of the sample (PVP). The relative viscosity ηrel is obtained from the following equation. Each flow time is a value measured at 25 ° C. by an Ubbelohde viscometer.
ηrel = 1% PVP aqueous solution flow time / water flow time
PVP is blended in an amount of 0.1 to 20% by weight, preferably 0.2 to 10% by weight, and more preferably 0.2 to 5% by weight with respect to 100% by weight of CMC-Na. If it is less than 0.1% by weight, the effect of using PVP cannot be obtained, and if it exceeds 20% by weight, the concentration of CMC-Na itself in the aqueous solution is undesirably lowered.
[0017]
Examples of a method for preparing a CMC-Na aqueous solution containing PVP include a method of dissolving a mixture of CMC-Na and PVP in water, a method of dissolving PVP in a CMC-Na aqueous solution, and a solution of PVP in a CMC-Na aqueous solution. There are methods for blending, and any method may be used. In addition, when CMC-Na and PVP are dissolved in water, for example, there are a method of dissolving using a stirrer, a method of dissolving by natural standing, a method of dissolving by heating, etc. No problem.
[0018]
The viscosity of the CMC-Na aqueous solution containing PVP prepared according to the present invention is lower than when no PVP is contained. It is considered that the viscosity of the aqueous solution decreases because the friction between CMC-Na molecules in the CMC-Na aqueous solution is reduced by PVP.
[0019]
The low-viscosity CMC-Na aqueous solution obtained in the present invention can be usefully used for general construction, pharmaceuticals, cosmetics and the like. For example, when the low-viscosity CMC-Na aqueous solution of the present invention is used as a barium sulfate dispersant for X-ray contrast, it is easy to take because of its low viscosity, and the inside of the fine stomach / intestinal wall of the digestive tract Contrast agent particles can evenly adhere to each other, enabling accurate imaging.
[0020]
【Example】
Examples 1-9, Comparative Examples 1-6
The degree of etherification of CMC-Na used (made by Daiichi Kogyo Seiyaku Co., Ltd., using a 10 wt% aqueous solution viscosity of 1000 mPa · s or less) and the 10 wt% aqueous solution viscosity at 25 ° C were measured as follows. did. Further, by dissolving a predetermined amount of a mixture of CMC-Na and PVP (“Luviskol K-30” manufactured by BASF, number average molecular weight≈10,000, K value = 27.0 to 33.0) in water, CMC-Na aqueous solution containing the amount of PVP shown in 1 was prepared. Table 1 shows the results of measuring the degree of etherification of CMC-Na and the viscosity of a 10 wt% aqueous solution before and after the addition of PVP.
[0021]
<Degree of etherification>
About 1 g of CMC-Na is precisely weighed, wrapped in filter paper, placed in a magnetic crucible, ashed at 600 ° C., and the resulting sodium hydroxide is titrated with 0.1 N sulfuric acid using phenolphthalein as an indicator to neutralize The degree of etherification of CMC-Na is calculated using the sulfuric acid amount A (ml) required for titration and the titer f 3 of 0.1 N sulfuric acid.
Degree of etherification = 162 × A × f 3 / (10000−80 × A × f 3 )
[0022]
<10 wt% aqueous solution viscosity>
[0023]
(1) Moisture content measurement Sample (CMC-Na) 1 to 2 g is precisely weighed in a weighing bottle and dried in a dryer at 105 ± 0.2 ° C. for 2 hours. Ask.
Moisture content (%) = weight loss (g) / sample (g) × 100
[0024]
(2) Viscosity measurement Approximately 25 g of a sample (CMC-Na) is precisely weighed in a 300 ml tall beaker, and a water amount of dissolved water necessary for obtaining a 10% by weight aqueous solution obtained by the following formula is added with a glass rod. Disperse.
Dissolved water amount (g) = sample (g) × (90−water content (%))
The resulting aqueous solution is allowed to stand overnight and stirred with a magnetic stirrer for about 5 minutes to make a uniform solution. After putting the solution in a thermostatic bath at 25 ° C for 30 minutes to make the solution 25 ° C, gently stir with a glass rod, attach a rotor and guard using a BM type viscometer (manufactured by Tokimec Co., Ltd.), and rotate at a rotation speed of 60 rpm. Read the scale after 3 minutes.
Viscosity (mPa · s) = Reading scale × Coefficient [0025]
[Table 1]
Experimental Examples 1-9, Comparative Experimental Examples 1-6
The effects of using the CMC-Na aqueous solution with reduced viscosity obtained in Examples 1 to 9 and the CMC-Na aqueous solution obtained in Comparative Examples 1 to 6 as barium sulfate dispersants for X-ray contrast media were evaluated.
[0027]
After dissolving 2.4 g of CMC-Na in 144 ml of water and PVP having the blending amounts shown in Table 1 with respect to CMC-Na, 240 g of barium sulfate (reagent grade 1) is added, and using a homomixer at 8000 rpm for 2 minutes. The test contrast medium was obtained by stirring and dispersing.
[0028]
About the obtained contrast agent for a test, the viscosity change at the time of artificial gastric fluid addition on the conditions of the following (a)-(c) and evaluation of stability were performed.
[0029]
<Viscosity change when artificial gastric juice is added>
(A) 13 ml of artificial gastric juice (15 ml of hydrochloric acid (reagent grade 1) diluted to 1000 ml with distilled water) is added to 100 ml of the contrast medium and stirred well. 100 ml of the obtained suspension was placed in a tall beaker and allowed to stand in a thermostatic bath at 25 ° C. for 30 minutes, and then a B type viscometer (manufactured by Tokyo Keiki Kogyo Co., Ltd.) was used to rotate the rotors Nos. 2 and 3. The number is rotated at 60 rpm and the viscosity after 3 minutes is measured.
Viscosity (mPa · s) = reading scale × coefficient (b) 13 ml of artificial gastric juice (25 ml of hydrochloric acid diluted to 1000 ml with distilled water) is added to 100 ml of the contrast agent and stirred well. The obtained suspension is measured under the same conditions as in (a).
(C) Add 13 ml of water to 100 ml of contrast medium and stir well. The obtained suspension is measured under the same conditions as in (a).
[0030]
<Stability>
100 ml of the contrast medium for test is placed in a 100 ml graduated cylinder and allowed to stand, and the volume of the supernatant after 10 days is measured.
[0031]
[Table 2]
In Table 1, the 10 wt% aqueous solution viscosity of Examples 1 to 9 in which 0.5 to 10 wt% PVP was blended with CMC-Na in CMC-Na aqueous solution is the degree of etherification of CMC-Na used and It can be seen that, regardless of the viscosity of the 10 wt% aqueous solution, the viscosity is lower than that before the PVP blending (Comparative Examples 1, 3, 5). Moreover, from the results of Comparative Examples 2, 4, and 6 in which 25 wt% PVP was blended with respect to CMC-Na, when the blending amount of PVP is large, the aqueous solution viscosity after blending is higher than the viscosity before blending. I understand that.
[0033]
From Table 2, when the artificial gastric juice is added to the X-ray contrast medium containing the CMC-Na aqueous solution, the viscosity decreases due to the blending of PVP, and the CMC-Na aqueous solution is added to the X-ray contrast medium. It can be seen that the blending of PVP is also effective. In addition, the amount of the supernatant produced after the X-ray contrast medium is allowed to stand does not differ greatly depending on the presence or absence of PVP, so it can be seen that the addition of PVP does not affect the stability of the X-ray contrast medium. .
[0034]
【The invention's effect】
According to the method of the present invention, for example, by adding 0.1 to 20% by weight of PVP of CMC-Na to an aqueous solution of CMC-Na having a 10% by weight aqueous solution viscosity of 10,000 mPa · s or less, CMC- The aqueous solution viscosity can be reduced without reducing the Na concentration.
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