WO2022114076A1 - 気泡含有組成物製造用添加剤 - Google Patents
気泡含有組成物製造用添加剤 Download PDFInfo
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- WO2022114076A1 WO2022114076A1 PCT/JP2021/043260 JP2021043260W WO2022114076A1 WO 2022114076 A1 WO2022114076 A1 WO 2022114076A1 JP 2021043260 W JP2021043260 W JP 2021043260W WO 2022114076 A1 WO2022114076 A1 WO 2022114076A1
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- C08J2471/02—Polyalkylene oxides
Definitions
- the present invention is for producing a bubble-containing composition, which promotes foaming and improves the stability of the generated bubbles by adding it at the time of producing the bubble-containing composition or by adding it to the bubble-containing composition. It is about additives.
- a cellulose-based material such as carbosikimethylcellulose is used as an additive that forms fine and creamy foam, maintains a good foam dispersion state, and improves foam stability.
- Patent Document 1 describes carboxymethyl cellulose having a degree of etherification of 0.8 to 2.0 and a viscosity of a 2% aqueous solution of 1 to 30 mPa ⁇ s as a stabilizer for ice cream having a low air content. -It is disclosed that a sodium salt is used.
- Patent Document 2 describes a dry cellulose composition containing crystalline fibrous cellulose and / or 30 to 95% by mass of the fibrous cellulose and 5 to 70% by mass of a water-soluble polymer and / or a hydrophilic substance. It is described that the bubble stability of processed egg foods is improved by blending the substance with liquid eggs.
- Patent Document 3 describes that chemically modified cellulose nanofibers are used as an additive for a bubble-containing composition.
- Patent Document 1 using water-soluble carboxymethyl cellulose and Patent Document 2 using non-chemically modified fibrous cellulose do not have sufficient bubble sustainability (bubble stability).
- the method using chemically modified cellulose nanofibers described in Patent Document 3 can obtain a bubble stabilizing effect.
- the foaming property the ability to form bubbles first
- An object of the present invention is to further improve the method described in Patent Document 3 to provide an additive for producing a bubble-containing composition having high foaming property (force to form bubbles) while maintaining bubble stability. And.
- carboxymethylated cellulose nanofibers having a specific degree of carboxymethyl substitution and crystallinity of cellulose type I have been obtained as a nonionic water-soluble polymer and / or surface activity. It has been found that the foaming property can be enhanced while maintaining the bubble stability of the composition by using it together with the agent as an additive for producing a bubble-containing composition.
- the present invention includes, but is not limited to, the following.
- the nonionic water-soluble polymer is at least one selected from hydroxyethyl cellulose, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, or hydroxyethyl methyl cellulose, which comprises at least a nonionic water-soluble polymer [1].
- the nonionic water-soluble polymer contains at least a nonionic water-soluble polymer, and the nonionic water-soluble polymer is polyethylene glycol, polyvinylpyrrolidone, a copolymer of vinylpyrrolidone and vinyl acetate, lactan, purulan, mannan, sclerothium gum, or guar gum.
- [4] It contains at least a surfactant, and the surfactants are sodium lauryl sulfate, lauramidopropyl hydroxysultaine, decyldimethylamine oxide, lauramine oxide, sodium oleate, sodium laureth sulfate, sodium cocoylmethyl taurine, cocoyl glutamate. Any one of [1] to [3], which is at least one selected from sodium, potassium laurate, cocamidopropyl betaine, cocamidodiethanolamide, lauramidopropyl betaine, hydrogenated lecithin, or sodium cocoamphoacetate.
- the additive for producing a bubble-containing composition according to the above section.
- [5] Amount of nonionic water-soluble polymer and / or surfactant with respect to 100 parts by mass of carboxymethylated cellulose nanofiber (when both nonionic water-soluble polymer and surfactant are contained, both)
- the additive for producing a bubble-containing composition according to any one of [1] to [5] is mixed with the material for the bubble-containing composition and stirred to foam the material.
- a method for producing a bubble-containing composition A method for stabilizing bubbles in a bubble-containing composition, which comprises adding the additive for producing a bubble-containing composition according to any one of [1] to [5] to the bubble-containing composition. ..
- the foaming property of the composition can be enhanced and the sustainability (bubble stability) of the formed bubbles can also be enhanced. Further, by adding to the bubble-containing composition, further foaming can be promoted and bubble stability can be imparted. That is, the additive of the present invention can impart both foaming property and bubble stability to the composition containing bubbles.
- the additive for producing a foaming-containing composition of the present invention contains a specific carboxymethylated cellulose nanofiber and a nonionic water-soluble polymer and / or a surfactant, but instead of, for example, a nonionic water-soluble polymer. When an anionic water-soluble polymer is used, the above effects cannot be obtained as shown in Comparative Examples 1 to 3.
- the additive for producing a bubble-containing composition of the present invention is, for example, a food or drink containing bubbles or intended to be foamed at the time of use (doughs such as ice cream, cakes and hot cakes, bread, whipped cream, etc.). , Cosmetics (washing pigment, shaving cream, etc.), cleaning agents (solid soap, kitchen detergent, body soap, shampoo, toothpaste, etc.), resins, pesticides, civil engineering, boring (air bubble shield, etc.) and the like.
- Example 1 It is a photograph which shows the result of Example 1.
- Example 7. It is a photograph which shows the result of Example 8.
- carboxymethylated cellulose nanofibers (hereinafter, “carboxymethylated” may be abbreviated as “CM” and cellulose nanofibers may be abbreviated as “CNF”) are carboxymethylated cellulose (CM-modified cellulose). Is obtained by refining to a fiber width of nanometer level, and is usually a fine fiber having a fiber width of about 3 to several hundred nm, for example, about 4 to 500 nm. The aspect ratio is not limited, but is, for example, 50 or more, preferably 100 or more.
- the average fiber diameter and average fiber length of the CM-ized CNF were randomly selected using an atomic force microscope (AFM), a transmission electron microscope (TEM), or a field emission scanning electron microscope (FE-SEM). It can be obtained by calculating the average value of the fiber diameter and the fiber length obtained from the result of observing the fiber of the book. Further, the aspect ratio can be calculated by dividing the average fiber length by the average fiber diameter.
- the CM-ized CNF can be obtained by applying a mechanical force to the CM-ized cellulose to make it finer (defibrated).
- CM-formed cellulose has a structure in which some of the hydroxyl groups in the glucose residues constituting the cellulose are ether-bonded to the carboxymethyl group.
- the CM-modified cellulose may be in the form of a salt, and when the CM-modified cellulose is referred to in the present specification, the CM-modified cellulose salt is also included.
- the salt of CM-formed cellulose include metal salts such as sodium salt of CM-formed cellulose.
- CM-ized cellulose which is the raw material of the CM-made CNF
- vegetable materials for example, wood, bamboo, hemp, jute, kenaf, farmland waste, cloth, pulp (coniferous unbleached craft).
- the CM-modified cellulose as a raw material for the CM-modified CNF may be obtained by carboxymethylating the above-mentioned cellulose raw material by a known method, or a commercially available product may be used. In either case, the degree of carboxymethyl group substitution per anhydrous glucose unit of cellulose is preferably 0.01 to 0.50. The following method can be mentioned as an example of the method for producing such CM-formed cellulose.
- Cellulose raw material and 3 to 20 times by mass of water and / or lower alcohol as solvent specifically water, methanol, ethanol, n-propyl alcohol, isopropyl alcohol, n-butanol, isobutanol, tertiary butanol, etc. Use alone or a mixed medium of two or more.
- As the mercerizing agent 0.5 to 20 times mol of alkali metal hydroxide per anhydrous glucose residue of the cellulose raw material, specifically sodium hydroxide and potassium hydroxide is used.
- the cellulose raw material, the solvent, and the mercerizing agent are mixed, and the reaction temperature is 0 to 70 ° C., preferably 10 to 60 ° C., and the reaction time is 15 minutes to 8 hours, preferably 30 minutes to 7 hours.
- a CM agent is added in an amount of 0.05 to 10.0 times per glucose residue, the reaction temperature is 30 to 90 ° C., preferably 40 to 80 ° C., and the reaction time is 30 minutes to 10 hours, preferably 1 hour to 1 hour.
- the etherification reaction is carried out for 4 hours.
- CM-modified cellulose which is a raw material for CM-modified CNF, maintains at least a part of its fibrous shape even when dispersed in water, and is distinguished from carboxymethyl cellulose, which is a kind of water-soluble polymer described later. Will be done.
- carboxymethyl cellulose which is a kind of water-soluble polymer described later.
- a fibrous substance can be observed.
- carboxymethyl cellulose which is a kind of water-soluble polymer
- the peak of cellulose type I crystal can be observed when "carboxymethylated cellulose” is measured by X-ray diffraction, but cellulose type I crystal is not observed in the water-soluble polymer carboxymethyl cellulose.
- CM-ized CNF By defibrating CM-ized cellulose, CM-ized CNF can be produced.
- the apparatus used for defibration is not particularly limited, but an apparatus such as a high-speed rotary type, a colloid mill type, a high pressure type, a roll mill type, and an ultrasonic type can be used.
- a strong shearing force At the time of defibration, it is preferable to apply a strong shearing force to the dispersion of CM-formed cellulose.
- a wet high-pressure or ultra-high pressure homogenizer capable of applying a pressure of 50 MPa or more to the dispersion and applying a strong shearing force.
- the pressure is more preferably 100 MPa or more, still more preferably 140 MPa or more.
- the dispersion may be pretreated, if necessary, using a known mixing, stirring, emulsifying, and dispersing device such as a high-speed shear mixer. ..
- the solid content concentration of the CM-formed cellulose dispersion to be defibrated is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, and particularly preferably 0. 3% by mass or more. Further, from the viewpoint of fluidity, it is preferably 10% by mass or less, and more preferably 6% by mass or less.
- the CM-ized CNF has a degree of carboxymethyl substitution per anhydrous glucose unit of cellulose of 0.01 to 0.50. If the degree of carboxymethyl substitution is less than 0.01, sufficient bubble stability and foaming property cannot be obtained. Further, when the degree of carboxymethyl substitution exceeds 0.50, dissolution in an aqueous medium is likely to occur, the fiber morphology cannot be maintained, and the bubble stability is lowered.
- the lower limit of the degree of carboxymethyl substitution is more preferably 0.10 or more, still more preferably 0.20 or more.
- the upper limit of the degree of carboxymethyl substitution is more preferably 0.40 or less.
- the degree of carboxymethyl substitution of CM-modified CNF is adjusted by controlling the amount of carboxymethylating agent to be reacted during the production of CM-modified cellulose as a raw material, the amount of mercerizing agent, the composition ratio of water and an organic solvent, and the like. be able to.
- the degree of carboxymethyl substitution of CM-modified cellulose and the degree of carboxymethyl substitution of CM-modified CNF obtained by defibrating it are usually the same.
- the anhydrous glucose unit means individual anhydrous glucose (glucose residue) constituting cellulose.
- the degree of carboxymethyl substitution (also referred to as the degree of etherification) is the ratio of hydroxyl groups in the glucose residues constituting cellulose that are substituted with carboxymethyl ether groups (carboxymethyl per glucose residue). The number of ether groups) is shown.
- the degree of carboxymethyl substitution may be abbreviated as DS.
- the method for measuring the degree of carboxymethyl substitution is as follows: Weigh about 2.0 g of the sample and place it in a 300 mL Erlenmeyer flask with a stopper. 100 mL of methanol nitrate (a solution of 1000 mL of methanol plus 100 mL of special grade concentrated nitric acid) is added and shaken for 3 hours to convert the salt of CM-formed cellulose (CMC) into H-CMC (hydrogen-type CM-formed cellulose). Weigh 1.5 to 2.0 g of the absolutely dry H-CMC and place it in a 300 mL Erlenmeyer flask with a stopper.
- the crystallinity of cellulose type I in the CM-ized CNF is 40% or more, preferably 50% or more, and more preferably 60% or more from the viewpoint of improving foaming property and bubble stability.
- the crystallinity of cellulose type I in the CM-formed CNF can be controlled by the concentration of the mercerizing agent at the time of producing the CM-formed cellulose as a raw material, the temperature at the time of treatment, and the degree of CM-forming. Since a high concentration of alkali is used in mercerization and CM formation, type I crystals of cellulose are easily converted to type II. For example, the degree of denaturation is adjusted by adjusting the amount of alkali (mercerizing agent) used.
- the upper limit of the crystallinity of cellulose type I is not particularly limited. In reality, about 90% is considered to be the upper limit.
- the crystallinity of cellulose type I of CM-formed cellulose and the crystallinity of cellulose type I of CM-formed CNF obtained by defibrating it are usually the same.
- the additive for producing a bubble-containing composition of the present invention is produced by mixing a nonionic water-soluble polymer and / or a surfactant with the above-mentioned CM-formed CNF.
- Both the nonionic water-soluble polymer and the surfactant may be contained in the additive of the present invention, or either one may be contained.
- examples of the nonionic water-soluble polymer include, but are not limited to, nonionic water-soluble polymers derived from cellulose such as hydroxyethyl cellulose, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl methyl cellulose.
- a nonionic water-soluble polymer such as polyethylene glycol, polyvinylpyrrolidone, a copolymer of vinylpyrrolidone and vinyl acetate, galactan, pullulan, mannan, sclerothium gum, and guar gum may be used.
- a nonionic water-soluble polymer for example, a plurality of types of the above may be mixed and used, or may be used alone. Of these, hydroxyethyl cellulose, methyl cellulose, or polyethylene glycol is preferred.
- the surfactant includes, for example, but not limited to, sodium lauryl sulfate, lauramidopropyl hydroxysultaine, decyldimethylamine oxide, lauramine oxide, sodium oleate, sodium laureth sulfate, sodium cocoylmethyltaurine, and cocoyl.
- Examples include sodium glutamate, potassium laurate, cocamidopropylbetaine, cocamidodiethanolamide, lauramidopropylbetaine, hydrogenated lecithin, and sodium cocoamphoacetate, among which sodium lauryl sulfate, lauramidopropyl hydroxysultaine, decyl.
- Dimethylamine oxide, lauramine oxide, and sodium oleate are preferred, with sodium lauryl sulfate, lauramidopropyl hydroxysultaine, and decyldimethylamine oxide being even more preferred.
- the surfactant for example, a plurality of types of the above may be mixed and used, or they may be used alone. The specific types of the nonionic water-soluble polymer and the surfactant may be appropriately selected depending on the bubble-containing composition to be produced.
- the mixing ratio of the CM-formed CNF and the nonionic water-soluble polymer and / or the surfactant is the ratio of the nonionic water-soluble polymer and / or the surfactant when the amount of the CM-formed CNF is 100 parts by mass.
- the amount is preferably 1 to 5000 parts by mass. It is more preferably 5 to 5000 parts by mass, still more preferably 5 to 2000 parts by mass, still more preferably 5 to 1000 parts by mass, still more preferably 10 to 1000 parts by mass, still more preferably 20 to 1000 parts by mass. It is by mass, more preferably 20 to 500 parts by mass.
- the "amount of nonionic water-soluble polymer and / or surfactant” is the amount of the nonionic water-soluble polymer and / or the surfactant used when either one is used, and is nonionic water-soluble. If both the polymer and the surfactant are used, it is the total amount. Further, the amounts of the CM-ized CNF, the nonionic water-soluble polymer, and the surfactant are all solid contents.
- the method of mixing the CM-ized CNF and the nonionic water-soluble polymer and / or the surfactant is not particularly limited, and dispersions in which each of both is dispersed in a dispersion medium such as water may be mixed. , The powder or the solid may be added to one of the dispersions and mixed.
- bubble-containing composition As described above, for producing a bubble-containing composition by mixing a CM-formed CNF having a specific carboxymethyl substitution degree and a cellulose type I crystallinity with a nonionic water-soluble polymer and / or a surfactant. Manufacture additives.
- the "bubble-containing composition” refers to a composition containing a gas such as air in the form of bubbles.
- the bubble-containing composition is usually formed by stirring the liquid with a stirrer, a whisk, or the like.
- the bubble-containing composition is not limited to these, but foods and drinks containing bubbles or intended to be foamed at the time of use (doughs such as ice cream, cakes and hot cakes, bread, whipped cream, etc.). , Cosmetics (washing pigment, shaving cream, etc.), cleaning agents (solid soap, kitchen detergent, body soap, shampoo, toothpaste, etc.), resins, pesticides, civil engineering, boring (air bubble shield, etc.), etc.
- the "additive for producing a bubble-containing composition” is an additive for mixing with a material for a bubble-containing composition (a component of the composition before containing bubbles) at the time of producing the bubble-containing composition, and the bubble-containing composition.
- a material for a bubble-containing composition a component of the composition before containing bubbles
- the bubble-containing composition includes additives to be added to the product.
- the material for the bubble-containing composition is foamed to form the bubble-containing composition by stirring or the like after the addition of the additive.
- the additive is uniformly mixed in the composition by stirring or the like after the addition of the additive. In either case, foaming property (force to form bubbles) and bubble stability (force to maintain formed bubbles) can be imparted to the composition.
- the material for the bubble-containing composition is included in the final bubble-containing composition. It may contain all the components, or it may be a part of the components contained in the final bubble-containing composition. In the latter case, after the addition of the additive of the present invention, the material for the bubble-containing composition (a part of the components of the bubble-containing composition) is foamed or while the remaining components of the composition are foamed. May be mixed. Further, the material for a bubble-containing composition to which the additive of the present invention is added corresponds to a bubble agent for promoting the formation of bubbles in advance and preventing the formed bubbles from coalescing or disappearing.
- the bubble agent examples include surfactants such as higher alcohol sulfate ester salt, alkyl ether sulfate ester salt, N-acylglutamate salt, and phosphate ester salt, as well as proteins such as collagen and keratin, carboxymethyl cellulose, and crystalline cellulose. And the like can be exemplified.
- the form of the additive for producing the bubble-containing composition is not particularly limited.
- it may be in the form of a dispersion containing CM-ized CNF and a nonionic water-soluble polymer and / or a surfactant and using water or the like as a dispersion medium, or a dried solid obtained by drying such a dispersion.
- It may be in the form of an object or in the form of a powder obtained by crushing a dry solid substance. It may also be in the form of a wet solid, which is an intermediate state between the dispersion and the dry solid.
- the dry solid substance means a substance obtained by deliquessing and drying the dispersion so that the amount of liquid such as water is 12% by mass or less.
- the dispersion medium is preferably water or a mixed solvent of water and a hydrophilic organic solvent in consideration of the dispersibility of the CMized CNF.
- the dispersion medium at the time of producing the CMized CNF may be used as it is, a hydrophilic organic solvent may be added, or a part of the dispersion medium may be replaced with a hydrophilic organic solvent to obtain a dispersion medium containing the hydrophilic organic solvent. May be good.
- the amount of the hydrophilic organic solvent is preferably 10% by mass or more, preferably 20% by mass, based on the total amount of water and the hydrophilic organic solvent.
- the above is more preferable, and 25% by mass or more is further preferable.
- the upper limit of the amount is not limited, but is preferably 95% by mass or less, and more preferably 80% by mass or less.
- the hydrophilic organic solvent means an organic solvent that dissolves in water. Examples thereof are, but are not limited to, methanol, ethanol, 2-propanol, butanol, glycerin, butylene glycol, propanediol, acetone, methyl ethyl ketone, 1,4-dioxane, N-methyl-2-pyrrolidone, tetrahydrofuran, N. , N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, acetonitrile, and combinations thereof.
- lower alcohols having 1 to 4 carbon atoms such as methanol, ethanol and 2-propanol and polyols such as glycerin, butylene glycol and propanediol are preferable, and from the viewpoint of safety and availability, methanol, ethanol and glycerin are used. Butylene glycol and propanediol are preferable.
- the pH of the dispersion of the CM-formed CNF and the nonionic water-soluble polymer and / or the surfactant was adjusted to 9 to 11. Later, it is preferable to remove and dry the liquid.
- the pH is adjusted to 9 to 11 and then dried, the dispersibility in the material for the bubble-containing composition or the bubble-containing composition becomes good.
- an alkali such as sodium hydroxide may be used.
- a known method can be used, and examples thereof include spray drying, squeezing, air drying, hot air drying, and vacuum drying.
- the drying device is not particularly limited, but is a continuous tunnel drying device, a band drying device, a vertical drying device, a vertical turbo drying device, a multi-stage disk drying device, an aeration drying device, a rotary drying device, an air flow drying device, and a spray.
- a box-type drying device, a stirring drying device, or the like can be used alone or in combination of two or more.
- a device that forms a thin film and performs drying heat energy can be uniformly directly supplied to the object to be dried, and the drying process can be performed more efficiently and in a short time, so that energy efficiency is achieved. It is preferable from the point of view. Further, an apparatus for forming a thin film and drying it is preferable from the viewpoint that the dried product can be immediately recovered by a simple means such as scraping the thin film, and further, a material for a bubble-containing composition of the obtained dried solid material or a material for a bubble-containing composition. It is also preferable from the viewpoint of improving the dispersibility in the bubble-containing composition.
- Examples of the device for forming and drying a thin film include a drum-type drying device and a belt-type drying device for forming and drying a thin film on a drum or a belt. Of these, a drum-type drying device that facilitates continuous drying and recovery of dried products is preferable.
- the drum type drying device continuously supplies the dispersion to the drum surface while rotating the heated drum, evaporates and concentrates the dispersion medium, and at the same time adheres the dispersion to the drum surface in the form of a thin film for drying.
- This is a device for producing a dry solid by scraping the dried product formed on the surface of the drum with a knife.
- the drum type drying device includes a double drum type device using two drums, a twin drum type device, and a single drum type device using one drum, but any of them may be used. Among these, a double drum type device capable of adjusting the film thickness of the thin film by adjusting the clearance between the drums is preferable.
- the film thickness of the thin film to be dried is preferably 50 to 1000 ⁇ m, more preferably 100 to 300 ⁇ m. When it is 50 ⁇ m or more, it is easy to scrape after drying, and when it is 1000 ⁇ m or less, the effect of improving the dispersibility in the foam-containing composition material or the bubble-containing composition can be seen.
- the drying temperature is not particularly limited. For example, it can be dried using a temperature of about 200 ° C. or lower. When drying is performed using a drum-type drying device or a belt-type drying device that forms and dries a thin film, the drying temperature refers to the temperature of the drum or belt surface.
- Drying may be performed under normal pressure, vacuum or reduced pressure.
- drying under vacuum or reduced pressure has the advantages of lowering the boiling point of water, accelerating the evaporation rate, accelerating the drying of the object, and reducing the thermal effect on the sample. It is preferable because it can be used.
- vacuum drying When drying under vacuum or reduced pressure (hereinafter, also referred to as “vacuum drying”), it is preferable to perform drying in the range of 0 to 50 kPa. Since the lower pressure gives the advantage that the water can be evaporated at a lower temperature, it is preferably 50 kPa or less, more preferably 30 kPa or less, and further preferably 10 kPa or less.
- the drying temperature is preferably 40 ° C. or higher, more preferably 45 ° C. or higher, and even more preferably 50 ° C. or higher.
- the temperature is preferably 100 ° C. or lower, more preferably 90 ° C. or lower, more preferably 85 ° C. or lower, and 80 ° C. or lower. Is more preferable, and the temperature may be lower than 80 ° C.
- the vacuum dryer is not particularly limited, but a vacuum box dryer, a vacuum drum dryer, a vacuum spray dryer, a vacuum belt dryer, etc. can be used alone or in combination of two or more.
- a heated drum is placed under vacuum or reduced pressure, and the dispersion is continuously supplied to the drum surface while rotating the drum to evaporate and concentrate the dispersion medium, and at the same time, the drum.
- It is a device for producing a dry solid substance by adhering a dispersion in a thin film on the surface and drying it, and scraping the dried substance formed on the drum surface with a knife.
- the median diameter of the powder is preferably about 10.0 to 150.0 ⁇ m, more preferably 25.0 to 100.0 ⁇ m, and 35.0. It is more preferably ⁇ 70.0 ⁇ m.
- the median diameter is 10.0 ⁇ m or more, problems such as powder flying are unlikely to occur, and when the median diameter is 150.0 ⁇ m or less, the volume is appropriate, so that the powder filling work is easy and preferable.
- the median diameter of the powder can be adjusted by adjusting the conditions for pulverization and classification.
- the median diameter can be measured by the following procedure: Using methanol as the dispersion medium, prepare a sample so that the scattering intensity is 0.1 to 20%, and measure the sample with a laser diffraction type particle size distribution measuring device (Mastersizer (registered trademark) 3000 manufactured by Malvern).
- Mastersizer registered trademark 3000 manufactured by Malvern
- the bubble-containing composition is produced by mixing the bubble-containing composition-producing additive of the present invention with a bubble-containing composition material (a component of the composition before containing bubbles) and stirring and foaming. can do.
- the additive of the present invention can impart good foaming property to the material for the bubble-containing composition and can enhance the sustainability (bubble stability) of the formed bubbles.
- the material for the bubble-containing composition may contain all the components contained in the final bubble-containing composition, or may be some components contained in the final bubble-containing composition. .. In the latter case, after the addition of the additive of the present invention, the material for the bubble-containing composition (a part of the components of the bubble-containing composition) is foamed or while the remaining components of the composition are foamed. May be mixed.
- the stirring conditions at this time may be appropriately determined depending on the type of the bubble-containing composition and the desired degree of foaming, and are not particularly limited. Stir for about 30 minutes, preferably about 1 to 15 minutes.
- the content of the additive of the present invention in the final bubble-containing composition may be appropriately changed according to the type of the bubble-containing composition and the desired degree of foaming, and is not particularly limited.
- CM-ized CNF CM-ized CNF
- IPA isopropanol
- LBKP hardwood pulp
- 100 parts were charged by the dry mass when dried at 100 ° C. for 60 minutes.
- Mercerized cellulose was prepared by stirring and mixing at 30 ° C. for 90 minutes. While further stirring, 15 parts of IPA and 12 parts of monochloroacetic acid were added, and after stirring for 30 minutes, the temperature was raised to 70 ° C. and a CM conversion reaction was carried out for 90 minutes. After completion of the reaction, the mixture was neutralized with acetic acid until the pH reached 7, washed with hydrous methanol, deflated, dried and pulverized to obtain CM-formed cellulose having a carboxymethyl substitution degree of 0.18.
- the CM-modified cellulose obtained in the above step was adjusted to 1.0% by mass with water and treated three times with an ultra-high pressure homogenizer (20 ° C., 150 MPa) to obtain a CM-modified CNF dispersion.
- the obtained fibers had an average fiber diameter of 5 nm, an aspect ratio of 150, and a cellulose I-type crystallinity of 72%.
- Example 1 A 1.0% by mass aqueous dispersion of CMized CNF obtained above was prepared. Further, hydroxyethyl cellulose (manufactured by Daicel Co., Ltd., trade name SE550) was selected as the nonionic water-soluble polymer (hereinafter, “hydroxyethyl cellulose” is abbreviated as “HEC”), and a CM-formed CNF 1.0% by mass aqueous dispersion was selected. A 2.0% by mass aqueous dispersion of HEC was prepared so as to have a viscosity similar to that of HEC.
- HEC nonionic water-soluble polymer
- CM-formed CNF 1.0% by mass aqueous dispersion and HEC 2.0 mass% aqueous dispersion are shown in Table 1 in a polypropylene container with a lid (manufactured by AS ONE, trade name: Pack Clean) having a capacity of 250 ml. Was mixed so as to have a mass ratio of. Each sample was stirred with a homodisper at 3000 rpm for 10 minutes. In order to evaluate foaming property and bubble stability, the height from the bottom surface of the container to the top surface of the dispersion was measured both immediately after stirring and after standing at room temperature for 1 day. I also took a picture. The photograph is shown in FIG.
- CM-ized CNF 1.0 mass% aqueous dispersion and the HEC 2.0 mass% aqueous dispersion are in the range of 90:10 to 30:70 (that is, when the CM-formed CNF is 100 parts by mass).
- HEC was mixed at a mass ratio of 22 to 467 parts by mass), placed in a vial, and allowed to stand at room temperature, and it was confirmed that bubbles remained even after one week. From the above, it was found that by using a mixture of HEC and CM-ized CNF, a high initial foaming property and a high bubble stabilizing effect over time can be obtained.
- Example 2 A 1.0% by mass aqueous dispersion of CMized CNF obtained above was prepared. Further, as a nonionic water-soluble polymer, a 1.0 mass% aqueous dispersion of polyethylene glycol (molecular weight 4,000,000) (hereinafter, “polyethylene glycol” is abbreviated as “PEG”) was prepared. The obtained CM-ized CNF 1.0% by mass aqueous dispersion and PEG1.0 mass% aqueous dispersion were placed in a polypropylene container with a lid (manufactured by AS ONE, trade name: Pack Clean) having a capacity of 250 ml, as shown in Table 2. 100 g was added at a time so as to have the stated mass ratio.
- PEG polyethylene glycol
- CM-formed CNF 1.0% by mass aqueous dispersion and carbomer 0.08 mass% aqueous dispersion were placed in a polypropylene container with a lid (manufactured by AS ONE, trade name: Pack Clean) having a capacity of 250 ml, as shown in Table 3. 100 g each was added so as to have the mass ratio described in 1. Each sample was stirred with a homodisper at 3000 rpm for 10 minutes. For the sample immediately after stirring, the height from the bottom surface of the container to the top surface of the dispersion was measured in the same manner as in Examples 1 and 2. I also took a picture. The photograph is shown in FIG.
- Example 2 The PEG in Example 2 is replaced with carboxymethyl cellulose (F350HC-4 manufactured by Nippon Paper Industries, Ltd.) (hereinafter, “carboxymethyl cellulose” is abbreviated as “CMC”) which is an anionic water-soluble polymer, and is the same as in Example 2.
- CMC carboxymethyl cellulose
- the CM-ized CNF 1.0% by mass aqueous dispersion and the CMC 1.0% by mass aqueous dispersion were mixed so as to have the mass ratios shown in Table 4 and placed in a polypropylene container, and each sample was homodispered. The mixture was stirred at 3000 rpm for 10 minutes. For the sample immediately after stirring, the height from the bottom surface of the container to the top surface of the dispersion was measured in the same manner as in Examples 1 and 2. I also took a picture. The photograph is shown in FIG.
- Example 3 The PEG in Example 2 was replaced with xanthan gum (Celtrol® CG-T manufactured by Sansho Co., Ltd.), which is an anionic water-soluble polymer, and CM-formed CNF 1.0% by mass water was used in the same manner as in Example 2.
- the dispersion and the xanthan gum 1.0% by mass aqueous dispersion were mixed so as to have the mass ratios shown in Table 5 and placed in a polypropylene container, and each sample was stirred with a homodisper at 3000 rpm for 10 minutes.
- the height from the bottom surface of the container to the top surface of the dispersion was measured in the same manner as in Examples 1 and 2. I also took a picture. The photograph is shown in FIG.
- Example 3 100 g of an aqueous dispersion containing 0.2% by mass of CM-modified CNF and 0.01% by mass of sodium lauryl sulfate obtained above is placed in a polypropylene container with a lid (manufactured by AS ONE, trade name: Pack Clean) having a capacity of 600 ml. It was added and stirred with a homodisper at 3000 rpm for 5 minutes. For comparison, an aqueous dispersion containing only 0.01% by mass of sodium lauryl sulfate was also placed in a container and stirred.
- the height from the bottom surface of the container to the top surface of the dispersion was measured immediately after stirring, after standing at room temperature for 5 minutes, and after standing for 10 minutes. I also took a picture. The photograph is shown in FIG.
- CM-ized CNF 1.0% by mass aqueous dispersion and MC1.0% by mass aqueous dispersion were placed in a polypropylene container with a lid (manufactured by AS ONE, trade name: Pack Clean) having a capacity of 250 ml, as shown in Table 6. 100 g was added at a time so as to have the stated mass ratio. Each sample was stirred with a homodisper at 3000 rpm for 5 minutes. In order to evaluate foaming property and bubble stability, those left at room temperature for 10 minutes, those left at room temperature for 1 day, and those left at room temperature for 4 days were dispersed from the bottom of the container immediately after stirring. The height to the upper surface of the body was measured. I also took a picture. The photograph is shown in FIG.
- Example 5 100 g of an aqueous dispersion containing 0.2% by mass of CM-modified CNF obtained above and 0.01% by mass of lauramidopropyl hydroxysultaine (Kawaken Fine Chemical Co., Ltd., trade name: Softazoline (registered trademark) LSB-R). was placed in a polypropylene container with a lid (manufactured by AS ONE, trade name: Pack Clean) having a capacity of 600 ml, and stirred with a homodisper at 3000 rpm for 5 minutes. For comparison, an aqueous dispersion containing only 0.01% by mass of lauramidopropyl hydroxysultaine was also placed in a container and stirred.
- Example 6 Examples except that 0.01% by mass of lauramidopropyl hydroxysultaine was changed to 0.2% by mass of decyldimethylamine oxide (Lion Specialty Chemical Co., Ltd., trade name: Cadenax (registered trademark) DM10D-W). Foaming property and bubble stability were evaluated in the same manner as in 5. The photograph is shown in FIG.
- Example 7 Lauramide propyl hydroxysultaine 0.01% by mass was changed to 0.003% by mass of lauramine oxide (Lion Specialty Chemical Co., Ltd., trade name: Cadenax (registered trademark) DW12D-W (C)) 0.003% by mass. Foaming property and bubble stability were evaluated in the same manner as in Example 5. The photograph is shown in FIG.
- Example 8 Foaming property and bubble stability were evaluated in the same manner as in Example 5 except that 0.01% by mass of lauramidopropyl hydroxysultaine was changed to 0.03% by mass of sodium oleate. The photograph is shown in FIG.
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Abstract
Description
[1]グルコース単位当たりのカルボキシメチル置換度が0.01~0.50であり、セルロースI型の結晶化度が40%以上であるカルボキシメチル化セルロースナノファイバーと、ノニオン性水溶性高分子及び/または界面活性剤とを含む、気泡含有組成物製造用添加剤。
[2]少なくともノニオン性水溶性高分子を含み、ノニオン性水溶性高分子が、ヒドロキシエチルセルロース、メチルセルロース、ヒドロキシプロピルセルロース、ヒドロキシプロピルメチルセルロース、またはヒドロキシエチルメチルセルロースから選択される少なくとも1種である、[1]に記載の気泡含有組成物製造用添加剤。
[3]少なくともノニオン性水溶性高分子を含み、ノニオン性水溶性高分子が、ポリエチレングリコール、ポリビニルピロリドン、ビニルピロリドンと酢酸ビニルの共重合体、ラクタン、プルラン、マンナン、スクレロチウムガム、またはグァーガムから選択される少なくとも1種である、[1]に記載の気泡含有組成物製造用添加剤。
[4]少なくとも界面活性剤を含み、界面活性剤が、ラウリル硫酸ナトリウム、ラウラミドプロピルヒドロキシスルタイン、デシルジメチルアミンオキシド、ラウラミンオキシド、オレイン酸ナトリウム、ラウレス硫酸ナトリウム、ココイルメチルタウリンナトリウム、ココイルグルタミン酸ナトリウム、ラウリン酸カリウム、コカミドプロピルベタイン、コカミドジエタノールアミド、ラウラミドプロピルベタイン、水添レシチン、またはココアンホ酢酸ナトリウムから選択される少なくとも1種である、[1]~[3]のいずれか1項に記載の気泡含有組成物製造用添加剤。
[5]カルボキシメチル化セルロースナノファイバー100質量部に対して、ノニオン性水溶性高分子及び/または界面活性剤の量(ノニオン性水溶性高分子と界面活性剤の両者を含む場合には両者の合計量)が1~5000質量部である、[1]~[4]のいずれか1項に記載の気泡含有組成物製造用添加剤。
[6][1]~[5]のいずれか1項に記載の気泡含有組成物製造用添加剤を、気泡含有組成物用材料に混合し、撹拌して前記材料を起泡させることを含む、気泡含有組成物の製造方法。
[7][1]~[5]のいずれか1項に記載の気泡含有組成物製造用添加剤を、気泡含有組成物に添加することを含む、気泡含有組成物の気泡を安定化させる方法。
本発明において、カルボキシメチル化セルロースナノファイバー(以下、「カルボキシメチル化」を「CM化」、セルロースナノファイバーを「CNF」と略すことがある。)は、カルボキシメチル化したセルロース(CM化セルロース)を、ナノメートルレベルの繊維幅まで微細化することにより得られるものであり、通常は、繊維幅が約3~数百nm程度、例えば、4~500nm程度の微細繊維である。アスペクト比は、限定されないが、例えば、50以上であり、好ましくは100以上である。CM化CNFの平均繊維径および平均繊維長は、原子間力顕微鏡(AFM)、透過型電子顕微鏡(TEM)、または電界放出型走査電子顕微鏡(FE-SEM)を用いて、ランダムに選んだ200本の繊維を観察した結果から得られる繊維径および繊維長の平均値を算出することによって得ることができる。また、平均繊維長を平均繊維径で除すことによりアスペクト比を算出することができる。CM化CNFは、CM化セルロースに機械的な力を加えて微細化(解繊)することによって得ることができる。
CM化CNFの原料となるCM化セルロースを製造するためのセルロース原料としては、例えば、植物性材料(例えば、木材、竹、麻、ジュート、ケナフ、農地残廃物、布、パルプ(針葉樹未漂白クラフトパルプ(NUKP)、針葉樹漂白クラフトパルプ(NBKP)、広葉樹未漂白クラフトパルプ(LUKP)、広葉樹漂白クラフトパルプ(LBKP)、針葉樹未漂白サルファイトパルプ(NUSP)、針葉樹漂白サルファイトパルプ(NBSP)サーモメカニカルパルプ(TMP)、再生パルプ、古紙等))、動物性材料(例えばホヤ類)、藻類、微生物(例えば酢酸菌(アセトバクター))、及び微生物産生物等を起源とするものを挙げることができ、それらのいずれも使用できる。好ましくは植物又は微生物由来のセルロース繊維であり、より好ましくは植物由来のセルロース繊維である。
CM化CNFの原料となるCM化セルロースは、上記のセルロース原料を公知の方法でカルボキシメチル化することにより得てもよいし、市販品を用いてもよい。いずれの場合も、セルロースの無水グルコース単位当たりのカルボキシメチル基置換度が0.01~0.50となるものが好ましい。そのようなCM化セルロースを製造する方法の一例として次のような方法を挙げることができる。
CM化セルロースを解繊することにより、CM化CNFを製造することができる。解繊に用いる装置は特に限定されないが、高速回転式、コロイドミル式、高圧式、ロールミル式、超音波式などの装置を用いることができる。解繊の際にはCM化セルロースの分散体に強力なせん断力を印加することが好ましい。特に、効率よく解繊するには、前記分散体に50MPa以上の圧力を印加し、かつ強力なせん断力を印加できる湿式の高圧または超高圧ホモジナイザーを用いることが好ましい。前記圧力は、より好ましくは100MPa以上であり、さらに好ましくは140MPa以上である。また、高圧ホモジナイザーでの解繊及び分散処理に先立って、必要に応じて、高速せん断ミキサーなどの公知の混合、攪拌、乳化、分散装置を用いて、前記分散体に予備処理を施してもよい。
CM化CNFは、セルロースの無水グルコース単位当たりのカルボキシメチル置換度が0.01~0.50である。カルボキシメチル置換度が0.01未満であると、十分な気泡安定性や起泡性が得られない。また、カルボキシメチル置換度が0.50を超えると水系媒体への溶解が起こりやすくなり、繊維形態を維持できなくなり、気泡安定性が低下する。カルボキシメチル置換度の下限値は、より好ましくは0.10以上であり、さらに好ましくは0.20以上である。カルボキシメチル置換度の上限値は、より好ましくは0.40以下である。CM化CNFのカルボキシメチル置換度は、原料となるCM化セルロースの製造時に反応させるカルボキシメチル化剤の添加量、マーセル化剤の量、水と有機溶媒の組成比率をコントロールすること等によって調整することができる。CM化セルロースのカルボキシメチル置換度と、それを解繊して得たCM化CNFのカルボキシメチル置換度とは、通常、同じである。
試料約2.0gを精秤して、300mL共栓付き三角フラスコに入れる。硝酸メタノール(メタノール1000mLに特級濃硝酸100mLを加えた液)100mLを加え、3時間振盪して、CM化セルロースの塩(CMC)をH-CMC(水素型CM化セルロース)に変換する。その絶乾H-CMCを1.5~2.0g精秤し、300mL共栓付き三角フラスコに入れる。80%メタノール15mLでH-CMCを湿潤し、0.1N-NaOHを100mL加え、室温で3時間振盪する。指示薬として、フェノールフタレインを用いて、0.1N-H2SO4で過剰のNaOHを逆滴定し、次式によってカルボキシメチル置換度(DS値)を算出する。
A=[(100×F’-0.1N-H2SO4(mL)×F)×0.1]/(H-CMCの絶乾質量(g))
カルボキシメチル置換度=0.162×A/(1-0.058×A)
F’:0.1N-H2SO4のファクター
F:0.1N-NaOHのファクター。
CM化CNFにおけるセルロースI型の結晶化度は、起泡性と気泡安定性向上の観点から、40%以上であり、好ましくは50%以上であり、さらに好ましくは60%以上である。CM化CNFにおけるセルロースI型の結晶化度は、原料となるCM化セルロースの製造時のマーセル化剤の濃度と処理時の温度、並びにCM化の度合によって制御することができる。マーセル化及びCM化においては高濃度のアルカリが使用されるために、セルロースのI型結晶がII型に変換されやすいが、例えば、アルカリ(マーセル化剤)の使用量を調整して変性の度合いを調整することによって、所望の結晶性を維持させることができる。セルロースI型の結晶化度の上限は特に限定されない。現実的には90%程度が上限となると考えられる。CM化セルロースのセルロースI型の結晶化度と、それを解繊して得たCM化CNFのセルロースI型の結晶化度とは、通常、同じである。
試料をガラスセルに乗せ、X線回折測定装置(LabX XRD-6000、島津製作所製)を用いて測定する。結晶化度の算出はSegal等の手法を用いて行い、X線回折図の2θ=10゜~30゜の回折強度をベースラインとして、2θ=22.6゜の002面の回折強度と2θ=18.5゜のアモルファス部分の回折強度から次式により算出する:
Xc=(I002c―Ia)/I002c×100
Xc=セルロースのI型の結晶化度(%)
I002c:2θ=22.6゜、002面の回折強度
Ia:2θ=18.5゜、アモルファス部分の回折強度。
上記のCM化CNFに対し、ノニオン性水溶性高分子及び/または界面活性剤を混合することにより、本発明の気泡含有組成物製造用添加剤を製造する。ノニオン性水溶性高分子と界面活性剤の両方を本発明の添加剤に含有させてもよいし、どちらか一方を含有させてもよい。例えば、ノニオン性水溶性高分子としては、これらに限定されないが、ヒドロキシエチルセルロース、メチルセルロース、ヒドロキシプロピルセルロース、ヒドロキシプロピルメチルセルロース、ヒドロキシエチルメチルセルロースのようなセルロース由来のノニオン性水溶性高分子が挙げられる。また、ポリエチレングリコール、ポリビニルピロリドン、ビニルピロリドンと酢酸ビニルの共重合体、ガラクタン、プルラン、マンナン、スクレロチウムガム、グァーガムのようなノニオン性水溶性高分子を用いてもよい。ノニオン性水溶性高分子は、例えば上記のものを複数種類混合して用いてもよいし、単独で用いてもよい。これらの中では、ヒドロキシエチルセルロース、メチルセルロース、またはポリエチレングリコールが好ましい。また、界面活性剤としては、例えば、これらに限定されないが、ラウリル硫酸ナトリウム、ラウラミドプロピルヒドロキシスルタイン、デシルジメチルアミンオキシド、ラウラミンオキシド、オレイン酸ナトリウム、ラウレス硫酸ナトリウム、ココイルメチルタウリンナトリウム、ココイルグルタミン酸ナトリウム、ラウリン酸カリウム、コカミドプロピルベタイン、コカミドジエタノールアミド、ラウラミドプロピルベタイン、水添レシチン、ココアンホ酢酸ナトリウムが挙げられ、これらの中では、ラウリル硫酸ナトリウム、ラウラミドプロピルヒドロキシスルタイン、デシルジメチルアミンオキシド、ラウラミンオキシド、及びオレイン酸ナトリウムが好ましく、ラウリル硫酸ナトリウム、ラウラミドプロピルヒドロキシスルタイン、及びデシルジメチルアミンオキシドがさらに好ましい。界面活性剤は、例えば上記のものを複数種類を混合して用いてもよいし、単独で用いてもよい。ノニオン性水溶性高分子と界面活性剤の具体的な種類は、製造しようとする気泡含有組成物に応じて適宜選択すればよい。
上記の通り、特定のカルボキシメチル置換度とセルロースI型の結晶化度を有するCM化CNFと、ノニオン性水溶性高分子及び/または界面活性剤とを混合することにより、気泡含有組成物製造用添加剤を製造する。「気泡含有組成物」とは、組成物中に空気などの気体を泡の状態で含んだものをいう。気泡含有組成物は通常、液体を攪拌機や泡立て器などにより攪拌することによって形成される。例えば、気泡含有組成物としては、これらに限定されないが、気泡を含有する又は使用時に起泡させることが意図された飲食品(アイスクリーム、ケーキ・ホットケーキ等の生地、パン、ホイップクリームなど)、化粧品(洗顔料、シェービングクリームなど)、洗浄剤(固形石鹸、台所洗剤、ボディーソープ、シャンプー、歯磨き粉など)、樹脂、農薬、土木、ボーリング(気泡シールドなど)等が挙げられる。
乾燥固形物を105℃のオーブンで12時間乾燥させ、乾燥前後の質量から乾燥固形物中の液体量を算出する。
乾燥固形物中の液体量(質量%)={1-(乾燥後の質量/乾燥前の質量)}×100。
エネルギー効率の点から好ましい。また、薄膜を形成させて乾燥を行う装置は、薄膜を掻き取る等の簡便な手段で直ちに乾燥物を回収できる点からも好ましく、さらに、得られた乾燥固形物の気泡含有組成物用材料または気泡含有組成物への分散性が向上する点からも好ましい。薄膜を形成させて乾燥を行う装置としては、例えば、ドラムやベルト上に薄膜を形成させて乾燥させるドラム型乾燥装置やベルト型乾燥装置が挙げられる。中でも連続乾燥と乾燥物の回収が容易なドラム型乾燥装置が好ましい。
分散媒としてメタノールを用い、散乱強度0.1~20%となるようにサンプルを調製し、レーザー回折式粒度分布測定装置(マルバーン社製、マスターサイザー(登録商標)3000)にて測定する。
本発明の気泡含有組成物製造用添加剤を、気泡含有組成物用材料(気泡を含有させる前の組成物の成分)に混合し、撹拌して起泡させることにより、気泡含有組成物を製造することができる。本発明の添加剤は、気泡含有組成物用材料に良好な起泡性を付与し、また、形成した気泡の持続性(気泡安定性)を高めることができる。気泡含有組成物用材料は、最終的な気泡含有組成物に含まれるすべての成分を含んでいてもよいし、また、最終的な気泡含有組成物に含まれる一部の成分であってもよい。後者の場合には、本発明の添加剤の添加後に、気泡含有組成物用材料(気泡含有組成物の一部の成分)を起泡させてからあるいは起泡させながら、組成物の残りの成分を混合してもよい。
回転数を100rpmに調節した二軸ニーダーに、イソプロパノール(IPA)620部と、水酸化ナトリウム10部を水30部に溶解したものとを加え、広葉樹パルプ(日本製紙(株)製、LBKP)を100℃で60分間乾燥した際の乾燥質量で100部仕込んだ。30℃で90分間撹拌、混合しマーセル化セルロースを調製した。更に撹拌しつつIPA15部と、モノクロロ酢酸12部を添加し、30分間撹拌した後、70℃に昇温して90分間CM化反応をさせた。反応終了後、pH7になるまで酢酸で中和し、含水メタノールで洗浄、脱液、乾燥、粉砕して、カルボキシメチル置換度0.18のCM化セルロースを得た。
上記で得られたCM化CNFの1.0質量%水分散体を用意した。また、ノニオン性水溶性高分子として、ヒドロキシエチルセルロース(ダイセル社製、商品名SE550)を選択し(以下、「ヒドロキシエチルセルロース」を「HEC」と略す。)、CM化CNF1.0質量%水分散体と同程度の粘度となるように、HECの2.0質量%水分散体を用意した。得られたCM化CNF1.0質量%水分散体と、HEC2.0質量%水分散体とを、容量250mlの蓋つきポリプロピレン製容器(アズワン社製、商品名:パッククリーン)に表1に記載の質量比となるように混合した。各サンプルをホモディスパーで3000rpmで10分間撹拌した。起泡性及び気泡安定性を評価するために、撹拌直後と、室温で1日間静置した後の両方について、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図1に示す。
上記で得られたCM化CNFの1.0質量%水分散体を用意した。また、ノニオン性水溶性高分子として、ポリエチレングリコール(分子量4,000,000)(以下、「ポリエチレングリコール」を「PEG」と略す。)の1.0質量%水分散体を用意した。得られたCM化CNF1.0質量%水分散体と、PEG1.0質量%水分散体とを、容量250mlの蓋つきポリプロピレン製容器(アズワン社製、商品名:パッククリーン)に、表2に記載の質量比となるように、100gずつ加えた。各サンプルをホモディスパーで3000rpmで10分間撹拌した。起泡性及び気泡安定性を評価するために、撹拌直後と、室温で10分間静置したもの、及び1時間静置したものについて、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図2に示す。
上記で得られたCM化CNFの1.0質量%水分散体を用意した。また、アニオン性水溶性高分子としてカルボキシビニルポリマー(岩瀬コスファ社製、商品名Carbopol(登録商標)940Polymer)を用い(以下、「カルボキシビニルポリマー」を「カルボマー」と略す。)、CM化CNF1.0質量%水分散体と同程度の粘度となるように、カルボマーの0.08質量%水分散体を用意した。得られたCM化CNF1.0質量%水分散体と、カルボマー0.08質量%水分散体とを、容量250mlの蓋つきポリプロピレン製容器(アズワン社製、商品名:パッククリーン)に、表3に記載の質量比となるように、100gずつ加えた。各サンプルをホモディスパーで3000rpmで10分間撹拌した。撹拌直後のサンプルについて、実施例1、2と同様に、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図3に示す。
実施例2におけるPEGを、アニオン性水溶性高分子であるカルボキシメチルセルロース(日本製紙社製F350HC-4)(以下、「カルボキシメチルセルロース」を「CMC」と略す。)に代えて、実施例2と同様に、CM化CNF1.0質量%水分散体と、CMC1.0質量%水分散体とを、表4に記載の質量比となるように混合してポリプロピレン製容器に入れ、各サンプルをホモディスパーで3000rpmで10分間撹拌した。撹拌直後のサンプルについて、実施例1、2と同様に、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図4に示す。
実施例2におけるPEGを、アニオン性水溶性高分子であるキサンタンガム(三晶社製ケルトロール(登録商標)CG-T)に代えて、実施例2と同様に、CM化CNF1.0質量%水分散体と、キサンタンガム1.0質量%水分散体とを、表5に記載の質量比となるように混合してポリプロピレン製容器に入れ、各サンプルをホモディスパーで3000rpmで10分間撹拌した。撹拌直後と1日後のサンプルについて、実施例1、2と同様に、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図5に示す。
上記で得られたCM化CNF0.2質量%とラウリル硫酸ナトリウム0.01質量%とを含む水分散体100gを、容量600mlの蓋つきポリプロピレン製容器(アズワン社製、商品名:パッククリーン)に入れ、ホモディスパーで3000rpmで5分間撹拌した。比較として、ラウリル硫酸ナトリウムのみを0.01質量%含む水分散体についても同様に容器に入れ撹拌した。起泡性及び気泡安定性を評価するために、撹拌直後、室温で5分静置後、及び10分静置後のものについて、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図6に示す。
上記で得られたCM化CNFの1.0質量%水分散体を用意した。また、ノニオン性水溶性高分子として、メチルセルロース(Methyl Cellulose (7000-10000mPa・s, 2% in Water at 20°C)、東京化成工業株式会社)(以下、「メチルセルロース」を「MC」と略す。)の1.0質量%水分散体を用意した。得られたCM化CNF1.0質量%水分散体と、MC1.0質量%水分散体とを、容量250mlの蓋つきポリプロピレン製容器(アズワン社製、商品名:パッククリーン)に、表6に記載の質量比となるように、100gずつ加えた。各サンプルをホモディスパーで3000rpmで5分間撹拌した。起泡性及び気泡安定性を評価するために、撹拌直後、室温で10分間静置したもの、室温で1日間静置きしたもの、及び室温で4日間静置したものについて、容器の底面から分散体の上面までの高さを測定した。また、写真を撮影した。写真を図7に示す。
上記で得られたCM化CNF0.2質量%とラウラミドプロピルヒドロキシスルタイン(川研ファインケミカル株式会社、商品名:ソフタゾリン(登録商標)LSB-R)0.01質量%とを含む水分散体100gを、容量600mlの蓋つきポリプロピレン製容器(アズワン社製、商品名:パッククリーン)に入れ、ホモディスパーで3000rpmで5分間撹拌した。比較として、ラウラミドプロピルヒドロキシスルタインのみを0.01質量%含む水分散体についても同様に容器に入れ撹拌した。起泡性及び気泡安定性を評価するために、撹拌直後、室温で5分静置後、及び10分静置後のものについて、容器の底面から分散体の上面までの高さと、容器の底面から気泡の下面までの高さを測定した。また、写真を撮影した。写真を図8に示す。
ラウラミドプロピルヒドロキシスルタイン0.01質量%を、デシルジメチルアミンオキシド(ライオン・スペシャリティ・ケミカル株式会社、商品名:カデナックス(登録商標)DM10D-W)0.2質量%に変更した以外は実施例5と同様にして、起泡性及び気泡安定性を評価した。写真を図9に示す。
ラウラミドプロピルヒドロキシスルタイン0.01質量%を、ラウラミンオキシド(ライオン・スペシャリティ・ケミカル株式会社、商品名:カデナックス(登録商標)DW12D-W(C))0.003質量%に変更した以外は実施例5と同様にして、起泡性及び気泡安定性を評価した。写真を図10に示す。
ラウラミドプロピルヒドロキシスルタイン0.01質量%を、オレイン酸ナトリウム0.03質量%に変更した以外は実施例5と同様にして、起泡性及び気泡安定性を評価した。写真を図11に示す。
Claims (7)
- グルコース単位当たりのカルボキシメチル置換度が0.01~0.50であり、セルロースI型の結晶化度が40%以上であるカルボキシメチル化セルロースナノファイバーと、ノニオン性水溶性高分子及び/または界面活性剤とを含む、気泡含有組成物製造用添加剤。
- 少なくともノニオン性水溶性高分子を含み、ノニオン性水溶性高分子が、ヒドロキシエチルセルロース、メチルセルロース、ヒドロキシプロピルセルロース、ヒドロキシプロピルメチルセルロース、またはヒドロキシエチルメチルセルロースから選択される少なくとも1種である、請求項1に記載の気泡含有組成物製造用添加剤。
- 少なくともノニオン性水溶性高分子を含み、ノニオン性水溶性高分子が、ポリエチレングリコール、ポリビニルピロリドン、ビニルピロリドンと酢酸ビニルの共重合体、ガラクタン、プルラン、マンナン、スクレロチウムガム、またはグァーガムから選択される少なくとも1種である、請求項1に記載の気泡含有組成物製造用添加剤。
- 少なくとも界面活性剤を含み、界面活性剤が、ラウリル硫酸ナトリウム、ラウラミドプロピルヒドロキシスルタイン、デシルジメチルアミンオキシド、ラウラミンオキシド、オレイン酸ナトリウム、ラウレス硫酸ナトリウム、ココイルメチルタウリンナトリウム、ココイルグルタミン酸ナトリウム、ラウリン酸カリウム、コカミドプロピルベタイン、コカミドジエタノールアミド、ラウラミドプロピルベタイン、水添レシチン、またはココアンホ酢酸ナトリウムから選択される少なくとも1種である、請求項1~3のいずれか1項に記載の気泡含有組成物製造用添加剤。
- カルボキシメチル化セルロースナノファイバー100質量部に対して、ノニオン性水溶性高分子及び/または界面活性剤の量(ノニオン性水溶性高分子と界面活性剤の両者を含む場合には両者の合計量)が1~5000質量部である、請求項1~4のいずれか1項に記載の気泡含有組成物製造用添加剤。
- 請求項1~5のいずれか1項に記載の気泡含有組成物製造用添加剤を、気泡含有組成物用材料に混合し、撹拌して前記材料を起泡させることを含む、気泡含有組成物の製造方法。
- 請求項1~5のいずれか1項に記載の気泡含有組成物製造用添加剤を、気泡含有組成物に添加することを含む、気泡含有組成物の気泡を安定化させる方法。
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