JPH0790121A - Production of gel of sodium salt of carboxymethylcellulose - Google Patents
Production of gel of sodium salt of carboxymethylcelluloseInfo
- Publication number
- JPH0790121A JPH0790121A JP5259024A JP25902493A JPH0790121A JP H0790121 A JPH0790121 A JP H0790121A JP 5259024 A JP5259024 A JP 5259024A JP 25902493 A JP25902493 A JP 25902493A JP H0790121 A JPH0790121 A JP H0790121A
- Authority
- JP
- Japan
- Prior art keywords
- cmc
- gel
- etherification
- degree
- sodium 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.)
- Pending
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 4
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 title abstract 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 36
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 36
- 238000006266 etherification reaction Methods 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 229920006184 cellulose methylcellulose Polymers 0.000 description 28
- 238000012710 chemistry, manufacturing and control Methods 0.000 description 28
- 238000001879 gelation Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 2
- 235000011126 aluminium potassium sulphate Nutrition 0.000 description 2
- 229940009827 aluminum acetate Drugs 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229940050271 potassium alum Drugs 0.000 description 2
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 229940095643 calcium hydroxide Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- -1 lead acetate Chemical compound 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、カルボキシメチルセル
ロースナトリウム塩（以下ＣＭＣと言う）を用いたゲル
状物の製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a gel-like product using carboxymethyl cellulose sodium salt (hereinafter referred to as CMC).
【０００２】[0002]
【従来の技術】従来のＣＭＣのゲル状物は１種のＣＭＣ
に２価又は３価の金属塩を反応させて製造されており、
製造されたゲル状物は蓄熱剤，蓄冷剤，やゲル状芳香物
質の基材等として使用されている。2. Description of the Related Art A conventional CMC gel is one type of CMC.
Is produced by reacting a divalent or trivalent metal salt with
The produced gel-like material is used as a heat storage agent, a cold storage agent, a base material for a gel-like aromatic substance, and the like.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、このよ
うな従来のＣＭＣのゲル状物にあっては、ＣＭＣの品質
が定められていないため、ゲル化が弱く、くずれたり場
合によってはゲル化しなかったり、又ゲル化がおきても
ゲル状物からの離水が生じたりして品質上問題があっ
た。However, in such a conventional CMC gel-like material, since the quality of CMC is not defined, the gelation is weak, and the gelling may occur or the gelation may not occur in some cases. Further, even if gelation occurs, water is released from the gelled material, which is a quality problem.
【０００４】[0004]
【課題を解決するための手段】この発明は、このような
従来の問題点に着目してなされたもので、特定の異なる
２種のエーテル化度をもったＣＭＣを併用し、これに２
価又は３価の金属塩を反応させることにより、前記問題
点のないＣＭＣのゲル状物が得られることを見出した。
すなわち、ＣＭＣに２価又は３価の金属塩を反応させて
ゲル状物を製造するにおいて、前記ＣＭＣにエーテル化
度が０．３以上０．８未満、１％水溶液粘度が１０〜４
００００ｍｐａ・ｓである１種以上のＣＭＣ８０〜９５
重量％とエーテル化度が０．８〜２．５、１％水溶液粘
度が１０〜２００００ｍｐａ・ｓである１種以上のＣＭ
Ｃ５〜２０重量％とを用いることを特徴とするＣＭＣの
ゲル状物の製造方法である。The present invention has been made by paying attention to such a conventional problem, and CMC having two specific different etherification degrees is used in combination therewith.
It was found that by reacting a monovalent or trivalent metal salt, a gelled product of CMC without the above problems can be obtained.
That is, when a gel-like material is produced by reacting CMC with a divalent or trivalent metal salt, the CMC has an etherification degree of 0.3 or more and less than 0.8, and a 1% aqueous solution viscosity of 10 to 4
One or more CMC 80-95 that is 0000 mpa · s
One or more types of CM having a weight% and an etherification degree of 0.8 to 2.5 and a 1% aqueous solution viscosity of 10 to 20,000 mpa · s.
C5 to 20% by weight is used, which is a method for producing a gelled product of CMC.
【０００５】（手段を構成する要件）本発明に使用する
金属塩としては２価又は３価のものが用いられ、カリミ
ョウバン，硫酸アルミニウム，酢酸アルミニウム，水酸
化アルミニウム，硫酸第一鉄，塩化第一鉄，硫酸亜鉛，
塩化バリウム，硝酸クロム，酢酸鉛，塩化第二銅，塩化
スズ，硝酸銀等が挙げられる。各金属塩は５％〜飽和水
溶液を調製して反応に供せられる。(Requirements Constituting Means) As the metal salt used in the present invention, divalent or trivalent metal salts are used, and potassium alum, aluminum sulfate, aluminum acetate, aluminum hydroxide, ferrous sulfate, ferric chloride are used. Monoiron, zinc sulfate,
Examples thereof include barium chloride, chromium nitrate, lead acetate, cupric chloride, tin chloride, silver nitrate and the like. Each metal salt is used in the reaction by preparing a 5% to saturated aqueous solution.
【０００６】本発明に使用するＣＭＣは、エーテル化度
が０．３以上０．８未満、１％水溶液粘度が１０〜４０
０００ｍｐａ・ｓであるＣＭＣ８０〜９５重量部に対し
てエーテル化度が０．８〜２．５、１％水溶液粘度が１
０〜２００００ｍｐａ・ｓであるＣＭＣを５〜２０重量
部加えたものである。前記エーテル化度０．３以上０．
８未満、０．８〜２．５のＣＭＣ双方とも、２種以上の
ＣＭＣの混合物であってもよい。エーテル化度０．８〜
２．５のＣＭＣの配合量が５重量部未満である時はゲル
状物の離水が生じる。又２０重量部をこえる時はゲル化
が弱く、崩れたり又ゲル化しないこともある。The CMC used in the present invention has an etherification degree of 0.3 or more and less than 0.8 and a 1% aqueous solution viscosity of 10 to 40.
The degree of etherification is 0.8 to 2.5, and the viscosity of 1% aqueous solution is 1 to 80 to 95 parts by weight of CMC of 000 mpa · s.
5 to 20 parts by weight of CMC of 0 to 20000 mpa · s is added. The degree of etherification is 0.3 or more and 0.
Both CMCs less than 8 and 0.8 to 2.5 may be a mixture of two or more CMCs. Etherification degree 0.8〜
When the compounding amount of CMC of 2.5 is less than 5 parts by weight, syneresis of the gel material occurs. When it exceeds 20 parts by weight, gelation is weak, and it may collapse or may not gel.
【０００７】１％水溶液粘度は、２５℃に於てＢ型粘度
計を用いて測定されたものである。The viscosity of a 1% aqueous solution is measured at 25 ° C. using a B type viscometer.
【０００８】次に製造方法を詳述すると、前記金属塩の
５％〜２５％水溶液を調製し、これに前記ＣＭＣの配合
品をＣＭＣ濃度が１％〜１０％になるような量で添加
し、１０〜３０℃で撹拌均一溶解させ約１時間ほど撹拌
を継続し反応を行う。撹拌をやめ放置すると一定時間
後、ゲル化が始まりゲル状物が生成される。Next, the production method will be described in detail. A 5% to 25% aqueous solution of the metal salt is prepared, and the CMC compounded product is added thereto in an amount such that the CMC concentration is 1% to 10%. The solution is stirred and uniformly dissolved at 10 to 30 ° C., and the reaction is continued by continuing stirring for about 1 hour. When stirring is stopped and left to stand, gelation starts after a certain period of time and a gelled substance is produced.
【０００９】[0009]
【作用】ＣＭＣは２価又は３価の金属と反応してＣＭＣ
金属塩を作る。これは、金属イオンによる架橋が生じて
ゲル化するのである。このゲル化においてＣＭＣのエー
テル化度は０．８以下のものが一般にゲル化しやすい。
一方０．８以上のＣＭＣはＣＭＣ金属塩になっても架橋
構造が充分に形成されずゲル化は生じない。[Function] CMC reacts with a divalent or trivalent metal to give CMC
Make a metal salt. This is because gelation occurs due to crosslinking caused by metal ions. In this gelation, it is generally easy for the CMC to have a degree of etherification of 0.8 or less.
On the other hand, a CMC of 0.8 or more does not form a crosslinked structure sufficiently even if it becomes a CMC metal salt and gelation does not occur.
【００１０】又エーテル化度０．８以下の単独のＣＭＣ
のゲル状物は製造は出来るが、保存中に離水が生じ保水
性が充分でない欠点がある。ＣＭＣのエーテル化度の異
なるものを一定配合で混合して用いた時、エーテル化度
０．８未満のＣＭＣで、ゲル状物が生成され、エーテル
化度０．８〜２．５のＣＭＣがゲル構造の中に組み込ま
れて、粘調性ある糊液状品が保水を助け離水が防止出来
るものと考えられる。A single CMC having an etherification degree of 0.8 or less
Although the gel-like product can be produced, it has a defect that water retention occurs during storage and water retention is not sufficient. When CMC having different etherification degree is mixed and used in a constant composition, a gelled product is produced with CMC having an etherification degree of less than 0.8, and CMC having an etherification degree of 0.8 to 2.5 is obtained. It is considered that the viscous paste liquid product is incorporated into the gel structure to help retain water and prevent water separation.
【００１１】[0011]
【実施例】実施例１〜４及び比較例１〜４ カリミョウバン，酢酸アルミニウム，水酸化カルシウム
の各々１０％及び２５％水溶液１００ｍｌをビーカーに
取る。このとき、溶解度以上の濃度になる水溶液はその
ままスラリー状態で反応を進める。前記ビーカー中に表
１の配合したＣＭＣを所定量添加し、２５℃で均一溶解
させ、１時間撹拌を続ける。そのまま一昼夜室温で放置
してゲル化するのを待つ。EXAMPLES Examples 1 to 4 and Comparative Examples 1 to 4 100 ml of 10% and 25% aqueous solutions of potassium alum, aluminum acetate and calcium hydroxide are placed in a beaker. At this time, the reaction proceeds in a slurry state as it is for the aqueous solution having a concentration of solubility or higher. A predetermined amount of the CMC blended in Table 1 was added to the beaker and uniformly dissolved at 25 ° C, and stirring was continued for 1 hour. Let stand at room temperature for 24 hours and wait for gelation.
【００１２】評価 一昼夜後、ビーカーよりゲル状物を取り出してゲル状態
を確認し、又離水状態はビーカー中に残っている離水を
注射器で吸い取りその重量を測定することによって評価
した。数値が大きいほど離水が多いことを示す。その評
価結果を表２に示した。 Evaluation After one day and night, the gel was taken out from the beaker to confirm the gel state, and the water separation state was evaluated by absorbing the water separation remaining in the beaker with a syringe and measuring the weight. The larger the value is, the more water is released. The evaluation results are shown in Table 2.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[0014]
【表２】 [Table 2]
【００１５】[0015]
【発明の効果】特定エーテル化度をもった異なったＣＭ
Ｃを配合する事により離水のない固いゲル状物を製造す
る事が出来る。EFFECT OF THE INVENTION Different CMs with a specific degree of etherification
By blending C, it is possible to produce a solid gel-like material without water separation.
Claims (1)
塩（以下ＣＭＣと言う）に２価又は３価の金属塩を反応
させてゲル状物を製造するにおいて、前記ＣＭＣにエー
テル化度が０．３以上０．８未満、１％水溶液粘度が１
０〜４００００ｍｐａ・ｓである１種以上のＣＭＣ８０
〜９５重量％とエーテル化度が０．８〜２．５、１％水
溶液粘度が１０〜２００００ｍｐａ・ｓである１種以上
のＣＭＣ５〜２０重量％とを用いることを特徴とするＣ
ＭＣのゲル状物の製造方法。1. When a carboxymethylcellulose sodium salt (hereinafter referred to as CMC) is reacted with a divalent or trivalent metal salt to produce a gel, the CMC has an etherification degree of 0.3 or more and 0.8 or more. Less than 1% viscosity of 1% aqueous solution
One or more CMC80 of 0 to 40,000 mpa · s
.About.95% by weight and a degree of etherification of 0.8 to 2.5 and 5% to 20% by weight of one or more CMC having a 1% aqueous solution viscosity of 10 to 20000 mpa.s.
Method for producing MC gel-like material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5259024A JPH0790121A (en) | 1993-09-22 | 1993-09-22 | Production of gel of sodium salt of carboxymethylcellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5259024A JPH0790121A (en) | 1993-09-22 | 1993-09-22 | Production of gel of sodium salt of carboxymethylcellulose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0790121A true JPH0790121A (en) | 1995-04-04 |
Family
ID=17328293
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5259024A Pending JPH0790121A (en) | 1993-09-22 | 1993-09-22 | Production of gel of sodium salt of carboxymethylcellulose |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0790121A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11106561A (en) * | 1997-10-03 | 1999-04-20 | Daicel Chem Ind Ltd | Novel carboxymethylcellulose sodium salt containing hydrogel composition and its production |
| JPH11199678A (en) * | 1997-04-23 | 1999-07-27 | Daicel Chem Ind Ltd | Aqueous gel and its production |
| JP2002293987A (en) * | 2001-03-30 | 2002-10-09 | Kobayashi Pharmaceut Co Ltd | Water gel composition |
| US7514097B1 (en) | 1999-11-09 | 2009-04-07 | Denki Kagaku Kogyo Kabushiki Kaisha | Use of soluble cellulose derivative having been made hardly soluble in water and process for producing the same |
| WO2010122687A1 (en) | 2009-04-20 | 2010-10-28 | 独立行政法人日本原子力研究開発機構 | Method for producing gel of carboxymethyl cellulose alkali metal salt |
| US8633254B2 (en) | 2006-09-15 | 2014-01-21 | Japan Atomic Energy Agency | Preparation of gels derived from carboxymethyl cellulose alkali metal salt |
| JP2016222868A (en) * | 2015-06-03 | 2016-12-28 | 第一工業製薬株式会社 | Method for producing water-insoluble carboxy-methyl cellulose cation salt, and cosmetic containing the same |
| JPWO2017104384A1 (en) * | 2015-12-17 | 2018-10-25 | リファインホールディングス株式会社 | Algae inhibitor, method for producing the algae inhibitor, and method for inhibiting algae |
-
1993
- 1993-09-22 JP JP5259024A patent/JPH0790121A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11199678A (en) * | 1997-04-23 | 1999-07-27 | Daicel Chem Ind Ltd | Aqueous gel and its production |
| JPH11106561A (en) * | 1997-10-03 | 1999-04-20 | Daicel Chem Ind Ltd | Novel carboxymethylcellulose sodium salt containing hydrogel composition and its production |
| US7514097B1 (en) | 1999-11-09 | 2009-04-07 | Denki Kagaku Kogyo Kabushiki Kaisha | Use of soluble cellulose derivative having been made hardly soluble in water and process for producing the same |
| JP2002293987A (en) * | 2001-03-30 | 2002-10-09 | Kobayashi Pharmaceut Co Ltd | Water gel composition |
| JP4717241B2 (en) * | 2001-03-30 | 2011-07-06 | 小林製薬株式会社 | Aqueous gel composition |
| US8633254B2 (en) | 2006-09-15 | 2014-01-21 | Japan Atomic Energy Agency | Preparation of gels derived from carboxymethyl cellulose alkali metal salt |
| WO2010122687A1 (en) | 2009-04-20 | 2010-10-28 | 独立行政法人日本原子力研究開発機構 | Method for producing gel of carboxymethyl cellulose alkali metal salt |
| JP2016222868A (en) * | 2015-06-03 | 2016-12-28 | 第一工業製薬株式会社 | Method for producing water-insoluble carboxy-methyl cellulose cation salt, and cosmetic containing the same |
| JPWO2017104384A1 (en) * | 2015-12-17 | 2018-10-25 | リファインホールディングス株式会社 | Algae inhibitor, method for producing the algae inhibitor, and method for inhibiting algae |
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