TW202412631A - Gel for particle dispersion, particle dispersion gel, method for producing gel for particle dispersion and method for producing particle dispersion gel - Google Patents

Gel for particle dispersion, particle dispersion gel, method for producing gel for particle dispersion and method for producing particle dispersion gel Download PDF

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TW202412631A
TW202412631A TW112129726A TW112129726A TW202412631A TW 202412631 A TW202412631 A TW 202412631A TW 112129726 A TW112129726 A TW 112129726A TW 112129726 A TW112129726 A TW 112129726A TW 202412631 A TW202412631 A TW 202412631A
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gel
particle dispersion
dispersion gel
particles
particle
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TW112129726A
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鈴木千里
石田怜司
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日商古河機械金屬股份有限公司
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Abstract

本發明之粒子分散用凝膠係包含聚合物(A)及溶劑(B),且可使粒子分散於內部者,上述粒子分散用凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B),上述溶劑(B)包含多元醇化合物(B1)。The particle dispersion gel of the present invention comprises a polymer (A) and a solvent (B) and can disperse particles inside. The particle dispersion gel forms a three-dimensional network structure by the polymer (A), and the network structure contains the solvent (B), and the solvent (B) comprises a polyol compound (B1).

Description

粒子分散用凝膠、粒子分散凝膠、粒子分散用凝膠之製造方法及粒子分散凝膠之製造方法Gel for particle dispersion, particle dispersion gel, method for producing particle dispersion gel, and method for producing particle dispersion gel

本發明係關於一種粒子分散用凝膠、粒子分散凝膠、粒子分散用凝膠之製造方法及粒子分散凝膠之製造方法。The present invention relates to a particle dispersion gel, a particle dispersion gel, a method for producing the particle dispersion gel, and a method for producing the particle dispersion gel.

具有立體網狀結構之凝膠可於內部內包各種粒子。 作為與此種粒子分散用凝膠相關之技術,例如可例舉專利文獻1(日本專利特開2018-115140號)中記載者。 A gel having a three-dimensional network structure can contain various particles inside. As a technology related to such a gel for dispersing particles, for example, the one described in Patent Document 1 (Japanese Patent Laid-Open No. 2018-115140) can be cited.

於專利文獻1中記載有一種抗菌、除臭用水凝膠,其特徵在於:其係包含以氫氧化鈣為主成分之鈣化合物之細粉末的水凝膠,關於上述水凝膠,構成凝膠之分散質藉由物理交聯而構建成立體網狀結構狀,且上述以氫氧化鈣為主成分之鈣化合物之細粉末含有於該立體網狀結構內所內包之凝膠之分散介質中,相對於構成上述水凝膠之親水性高分子樹脂100重量份,上述以氫氧化鈣為主成分之鈣化合物之細粉末的含量為5至300重量份。 先前技術文獻  專利文獻 Patent document 1 describes an antibacterial and deodorizing hydrogel, which is characterized in that: it is a hydrogel containing fine powder of a calcium compound with calcium hydroxide as the main component, and the dispersed substance constituting the hydrogel is constructed into a three-dimensional network structure by physical crosslinking, and the fine powder of the calcium compound with calcium hydroxide as the main component is contained in the dispersion medium of the gel enclosed in the three-dimensional network structure, and the content of the fine powder of the calcium compound with calcium hydroxide as the main component is 5 to 300 parts by weight relative to 100 parts by weight of the hydrophilic polymer resin constituting the hydrogel. Prior art document   Patent document

專利文獻1:日本專利特開2018-115140號公報Patent document 1: Japanese Patent Publication No. 2018-115140

[發明所欲解決之問題][The problem the invention is trying to solve]

為了提昇所內包之粒子之分散性及保持性之平衡,追求一種可根據內包之粒子之尺寸來控制網格尺寸之粒子分散用凝膠。 本發明係鑒於上述情況而完成者,提供一種容易控制網格尺寸之粒子分散用凝膠、使用其之粒子分散凝膠、及容易控制網格尺寸之粒子分散用凝膠之製造方法、以及可提昇粒子之分散性之粒子分散凝膠之製造方法。 [解決問題之技術手段] In order to improve the balance between the dispersibility and retention of the contained particles, a particle dispersing gel that can control the mesh size according to the size of the contained particles is sought. The present invention is completed in view of the above situation, and provides a particle dispersing gel that can easily control the mesh size, a particle dispersing gel using the same, and a method for manufacturing a particle dispersing gel that can easily control the mesh size, and a method for manufacturing a particle dispersing gel that can improve the dispersibility of particles. [Technical means for solving the problem]

本發明人等為了實現上述問題而反覆進行了銳意研究。結果發現,於包含聚合物(A)及溶劑(B)之粒子分散用凝膠中,藉由包含多元醇化合物(B1)作為溶劑(B),而容易控制網格尺寸,從而完成了本發明。The inventors of the present invention have conducted intensive research to achieve the above-mentioned problem. As a result, they have found that the mesh size can be easily controlled by including a polyol compound (B1) as the solvent (B) in a particle dispersion gel containing a polymer (A) and a solvent (B), thereby completing the present invention.

根據本發明,提供一種以下所示之粒子分散用凝膠、粒子分散凝膠、粒子分散用凝膠之製造方法及粒子分散凝膠之製造方法。According to the present invention, there are provided a particle dispersion gel, a particle dispersion gel, a method for producing a particle dispersion gel, and a method for producing a particle dispersion gel as shown below.

[1] 一種粒子分散用凝膠,其係包含聚合物(A)及溶劑(B),且可使粒子分散於內部者, 上述粒子分散用凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 上述溶劑(B)包含多元醇化合物(B1)。 [2] 如上述[1]所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)之分子量為50以上300以下。 [3] 如上述[1]或[2]所記載之粒子分散用凝膠,其中利用B型黏度計於25℃、轉速30 rpm之條件下測得之上述溶劑(B)之黏度為1 mPa・s以上200 mPa・s以下。 [4] 如上述[1]至[3]中任一項所記載之粒子分散用凝膠,其中上述溶劑(B)之沸點為180℃以上300℃以下。 [5] 如上述[1]至[4]中任一項所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)包含碳數2以上6以下之二醇化合物(B2)。 [6] 如上述[1]至[5]中任一項所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。 [7] 如上述[1]至[6]中任一項所記載之粒子分散用凝膠,其中利用錐板黏度計於25℃、錐2°/20 mm、剪切速度15 s -1之條件下測得之上述粒子分散用凝膠之黏度為10 mPa・s以上60000 mPa・s以下。 [8] 如上述[1]至[7]中任一項所記載之粒子分散用凝膠,其中將藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之最頻粒徑設為X 1(nm),將藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之中值粒徑設為(X 2)(nm)時,X 1/X 2為0.20以上2.0以下。 [9] 如上述[1]至[8]中任一項所記載之粒子分散用凝膠,其中藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之最頻粒徑(X 1)為10 nm以上。 [10] 如上述[1]至[9]中任一項所記載之粒子分散用凝膠,其中藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之中值粒徑(X 2)為50 nm以上。 [11] 如上述[1]至[10]中任一項所記載之粒子分散用凝膠,其中上述聚合物(A)包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物及聚乙烯吡咯啶酮所組成之群中之一種或兩種以上。 [12] 如上述[1]至[11]中任一項所記載之粒子分散用凝膠,其中上述粒子分散用凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。 [13] 一種粒子分散凝膠,其包含如上述[1]至[12]中任一項所記載之粒子分散用凝膠、及分散於上述粒子分散用凝膠中之粒子(C)。 [14] 如上述[13]所記載之粒子分散凝膠,其中上述粒子(C)包含選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑所組成之群中之一種或兩種以上。 [15] 如上述[13]或[14]所記載之粒子分散凝膠,其中藉由雷射繞射散射法測得之上述粒子(C)之中值粒徑D 50為0.01 μm以上10 μm以下。 [16] 一種粒子分散用凝膠之製造方法,其係用以製造如上述[1]至[12]中任一項所記載之粒子分散用凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)及上述溶劑(B)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散用凝膠。 [17] 如上述[16]所記載之粒子分散用凝膠之製造方法,其中於對上述凝膠狀物進行混練之步驟中,使用輥磨機對上述凝膠狀物進行混練。 [18] 一種粒子分散凝膠之製造方法,其係用以製造如上述[13]至[15]中任一項所記載之粒子分散凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)、上述溶劑(B)及上述粒子(C)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散凝膠。 [19] 如上述[18]所記載之粒子分散凝膠之製造方法,其中上述粒子分散凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 上述粒子(C)內包於上述網狀結構內。 [20] 如上述[18]或[19]所記載之粒子分散凝膠之製造方法,其中於對上述凝膠狀物進行混練之步驟中,使用輥磨機對上述凝膠狀物進行混練。 [21] 如上述[18]至[20]中任一項所記載之粒子分散凝膠之製造方法,其中上述粒子分散凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。 [發明之效果] [1] A particle dispersing gel comprising a polymer (A) and a solvent (B) and capable of dispersing particles therein, wherein the particle dispersing gel forms a three-dimensional network structure with the polymer (A), and the network structure contains the solvent (B), and the solvent (B) comprises a polyol compound (B1). [2] The particle dispersing gel as described in [1] above, wherein the molecular weight of the polyol compound (B1) is 50 to 300. [3] The particle dispersing gel as described in [1] or [2] above, wherein the viscosity of the solvent (B) measured at 25°C and 30 rpm using a B-type viscometer is 1 to 200 mPa·s. [4] The particle dispersion gel as described in any one of [1] to [3] above, wherein the boiling point of the solvent (B) is 180°C to 300°C. [5] The particle dispersion gel as described in any one of [1] to [4] above, wherein the polyol compound (B1) comprises a diol compound (B2) having a carbon number of 2 to 6. [6] The particle dispersion gel as described in any one of [1] to [5] above, wherein the polyol compound (B1) comprises one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol. [7] The particle dispersion gel as described in any one of the above [1] to [6], wherein the viscosity of the particle dispersion gel measured by a cone viscometer at 25°C, cone 2°/20 mm, and shear rate 15 s -1 is 10 mPa・s or more and 60000 mPa・s or less. [8] The particle dispersion gel as described in any one of the above [1] to [7], wherein the mode particle size of the stereo network structure measured by the photon correlation method in accordance with JIS Z 8826:2019 is X 1 (nm), and the median particle size of the stereo network structure measured by the photon correlation method in accordance with JIS Z 8826:2019 is (X 2 ) (nm), and X 1 /X 2 is 0.20 or more and 2.0 or less. [9] The particle dispersion gel as described in any one of [1] to [8] above, wherein the mode particle size (X 1 ) of the stereo network structure measured by the photon correlation method according to JIS Z 8826:2019 is 10 nm or more. [10] The particle dispersion gel as described in any one of [1] to [9] above, wherein the median particle size (X 2 ) of the stereo network structure measured by the photon correlation method according to JIS Z 8826:2019 is 50 nm or more. [11] The particle dispersion gel as described in any one of [1] to [10] above, wherein the polymer (A) comprises one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic acid polymers, polyvinyl alcohol polymers and polyvinyl pyrrolidone. [12] A particle dispersion gel as described in any one of [1] to [11] above, wherein the content of the polymer (A) in the particle dispersion gel is 0.01 mass % to 20.0 mass %. [13] A particle dispersion gel comprising the particle dispersion gel as described in any one of [1] to [12] above, and particles (C) dispersed in the particle dispersion gel. [14] A particle dispersion gel as described in [13] above, wherein the particles (C) comprise one or more selected from the group consisting of drugs, fragrances, antibacterial agents, fungicides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents. [15] The particle dispersion gel as described in [13] or [14] above, wherein the median particle size D50 of the particles (C) measured by laser diffraction scattering is 0.01 μm or more and 10 μm or less. [16] A method for producing a particle dispersion gel, which is used to produce the particle dispersion gel as described in any one of [1] to [12] above, and comprises the following steps: obtaining a gel by mixing the polymer (A) and the solvent (B); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel. [17] A method for producing a particle dispersion gel as described in [16] above, wherein in the step of kneading the gel, the gel is kneaded using a roller mill. [18] A method for producing a particle dispersion gel, which is used to produce the particle dispersion gel as described in any one of [13] to [15] above, and comprises the following steps: obtaining a gel by mixing the polymer (A), the solvent (B) and the particles (C); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel. [19] A method for producing a particle dispersion gel as described in [18] above, wherein the particle dispersion gel forms a three-dimensional network structure by the polymer (A), and the solvent (B) is contained in the network structure, and the particles (C) are enclosed in the network structure. [20] A method for producing a particle dispersion gel as described in [18] or [19] above, wherein in the step of kneading the gel-like material, a roller mill is used to knead the gel-like material. [21] A method for producing a particle dispersion gel as described in any one of [18] to [20] above, wherein the content of the polymer (A) in the particle dispersion gel is not less than 0.01 mass % and not more than 20.0 mass %. [Effect of the Invention]

根據本發明,可提供一種容易控制網格尺寸之粒子分散用凝膠、使用其之粒子分散凝膠、及容易控制網格尺寸之粒子分散用凝膠之製造方法、以及可提昇粒子之分散性之粒子分散凝膠之製造方法。According to the present invention, a particle dispersion gel with easily controllable mesh size, a particle dispersion gel using the same, a method for producing a particle dispersion gel with easily controllable mesh size, and a method for producing a particle dispersion gel capable of improving the dispersibility of particles can be provided.

以下,對本發明之實施方式進行說明。The following describes the implementation of the present invention.

[粒子分散用凝膠] 本實施方式之粒子分散用凝膠係包含聚合物(A)及溶劑(B),且可使粒子分散於內部者,上述粒子分散用凝膠藉由聚合物(A)形成立體網狀結構,且於上述網狀結構內含有溶劑(B),溶劑(B)包含多元醇化合物(B1)。 [Gel for particle dispersion] The gel for particle dispersion of the present embodiment comprises a polymer (A) and a solvent (B), and can disperse particles inside. The gel for particle dispersion forms a three-dimensional network structure by the polymer (A), and the network structure contains a solvent (B), and the solvent (B) contains a polyol compound (B1).

如上所述,為了提昇所內包之粒子之分散性及保持性之平衡,追求一種可根據內包之粒子之尺寸來控制網格尺寸之粒子分散用凝膠。 本發明人等為了達成上述課題而反覆進行了銳意研究。結果發現,於包含聚合物(A)及溶劑(B)之粒子分散用凝膠中,藉由包含多元醇化合物(B1)作為溶劑(B),而容易控制網格尺寸。具體而言,本實施方式之粒子分散用凝膠藉由使聚合物(A)之濃度或多元醇化合物(B1)之種類發生變化,可容易地控制粒子分散用凝膠之立體網狀結構之網格尺寸。 As described above, in order to improve the balance between the dispersibility and retention of the enclosed particles, a particle dispersion gel that can control the mesh size according to the size of the enclosed particles is sought. The inventors of the present invention have repeatedly conducted intensive research to achieve the above-mentioned topic. As a result, it was found that in a particle dispersion gel comprising a polymer (A) and a solvent (B), the mesh size can be easily controlled by including a polyol compound (B1) as a solvent (B). Specifically, the particle dispersion gel of the present embodiment can easily control the mesh size of the three-dimensional network structure of the particle dispersion gel by changing the concentration of the polymer (A) or the type of the polyol compound (B1).

以下,對構成本實施方式之粒子分散用凝膠之各成分詳細地進行說明。Hereinafter, each component constituting the particle dispersion gel of the present embodiment will be described in detail.

(聚合物(A)) 本實施方式之粒子分散用凝膠包含聚合物(A)。聚合物(A)係形成本實施方式之粒子分散用凝膠中之立體網狀結構者。 聚合物(A)並無特別限定,只要為藉由包含溶劑(B)可凝膠化並形成立體網狀結構者即可,較佳為包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物、及聚乙烯吡咯啶酮等所組成之群中之一種或兩種以上,更佳為包含選自由多糖類、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物、及聚乙烯吡咯啶酮等所組成之群中之一種或兩種以上,進而較佳為包含選自由多糖類、聚乙烯醇系聚合物、及聚乙烯吡咯啶酮等所組成之群中之一種或兩種以上,進而較佳為包含多糖類,進而較佳為包含水溶性多糖類,進而較佳為包含選自由銀耳多糖體、玻尿酸、三仙膠、海藻酸、瓜爾膠、陽離子化瓜爾膠、角叉菜膠、結冷膠、瓊脂糖、羧甲基纖維素、羥乙基纖維素、羥丙基纖維素、及纖維素奈米纖維等所組成之群中之一種或兩種以上之水溶性多糖類,進而較佳為包含選自由羧甲基纖維素、羥丙基纖維素、及羥乙基纖維素等所組成之群中之一種或兩種以上之水溶性纖維素類,進而較佳為包含羥丙基纖維素。羥丙基纖維素係水溶性纖維素衍生物,通常藉由氫氧化鈉等鹼對纖維素進行處理後,與環氧丙烷等醚化劑反應而獲得。羥丙基纖維素例如可自富士膠片和光純藥公司購買。 (Polymer (A)) The particle dispersion gel of the present embodiment includes a polymer (A). The polymer (A) is a polymer that forms a three-dimensional network structure in the particle dispersion gel of the present embodiment. The polymer (A) is not particularly limited, as long as it can be gelled and form a three-dimensional network structure by containing a solvent (B). It is preferably one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic polymers, polyvinyl alcohol polymers, and polyvinyl pyrrolidone, etc., and more preferably one or more selected from the group consisting of polysaccharides, (meth)acrylic polymers, polyvinyl alcohol polymers, and polyvinyl pyrrolidone, etc., and further preferably one or more selected from the group consisting of polysaccharides, polyvinyl alcohol polymers, and polyvinyl pyrrolidone, etc. More than two kinds, more preferably polysaccharides, more preferably water-soluble polysaccharides, more preferably tremella polysaccharides, hyaluronic acid, safflower gum, alginic acid, guar gum, cationized guar gum, carrageenan, gellan gum, agarose, carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, and cellulose nanofibers, etc. One or more water-soluble celluloses selected from the group consisting of carboxymethyl cellulose, hydroxypropyl cellulose, and hydroxyethyl cellulose, etc., and more preferably hydroxypropyl cellulose. Hydroxypropyl cellulose is a water-soluble cellulose derivative, which is usually obtained by treating cellulose with a base such as sodium hydroxide and then reacting it with an etherifying agent such as propylene oxide. Hydroxypropyl cellulose can be purchased from Fuji Film Co., Ltd. and Koh Pure Chemical Industries, Ltd., for example.

就進一步提昇內包於凝膠中之粒子之移動性之觀點而言,聚合物(A)包含較佳為30質量%以上、更佳為40質量%以上、進而較佳為50質量%以上、進而較佳為60質量%以上、進而較佳為80質量%以上之羥丙基纖維素,並且,較佳為可包含100質量%以下。From the viewpoint of further improving the mobility of the particles contained in the gel, the polymer (A) preferably contains 30% by mass or more, more preferably 40% by mass or more, further preferably 50% by mass or more, further preferably 60% by mass or more, further preferably 80% by mass or more of hydroxypropyl cellulose, and preferably contains 100% by mass or less.

就提昇凝膠黏度且進一步減小網格尺寸之觀點而言,本實施方式之粒子分散用凝膠中之聚合物(A)之含量較佳為0.01質量%以上,更佳為0.05質量%以上,進而較佳為0.1質量%以上,進而較佳為0.2質量%以上,進而較佳為0.3質量%以上,就進一步增大網格尺寸之觀點而言,較佳為20.0質量%以下,更佳為15.0質量%以下,進而較佳為10.0質量%以下,進而較佳為5.0質量%以下,進而較佳為2.5質量%以下,進而較佳為1.5質量%以下,進而較佳為1.0質量%以下,進而較佳為0.8質量%以下。From the viewpoint of increasing the gel viscosity and further reducing the mesh size, the content of the polymer (A) in the particle dispersion gel of the present embodiment is preferably 0.01 mass % or more, more preferably 0.05 mass % or more, further preferably 0.1 mass % or more, further preferably 0.2 mass % or more, further preferably 0.3 mass % or more, and from the viewpoint of further increasing the mesh size, it is preferably 20.0 mass % or less, more preferably 15.0 mass % or less, further preferably 10.0 mass % or less, further preferably 5.0 mass % or less, further preferably 2.5 mass % or less, further preferably 1.5 mass % or less, further preferably 1.0 mass % or less, further preferably 0.8 mass % or less.

(溶劑(B)) 本實施方式之粒子分散用凝膠包含多元醇化合物(B1)作為溶劑(B)。 多元醇化合物(B1)並無特別限定,只要為可與聚合物(A)一起凝膠化而形成立體網狀結構者即可,就進一步提昇粒子分散用凝膠之網格尺寸之控制性之觀點而言,較佳為包含碳數2以上6以下之二醇化合物(B2),更佳為包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上,更佳為包含選自由1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。 (Solvent (B)) The particle dispersion gel of the present embodiment contains a polyol compound (B1) as a solvent (B). The polyol compound (B1) is not particularly limited as long as it can be gelled together with the polymer (A) to form a three-dimensional network structure. From the viewpoint of further improving the controllability of the mesh size of the particle dispersion gel, it is preferably a diol compound (B2) containing 2 to 6 carbon atoms, more preferably one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol, and more preferably one or more selected from the group consisting of 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol.

本實施方式之粒子分散用凝膠亦可包含除多元醇化合物(B1)以外之溶劑作為溶劑(B)。 作為除多元醇化合物(B1)以外之溶劑,並無特別限定,例如可例舉:甲醇、乙醇、異丙醇(IPA)、N,N-二甲基甲醯胺(DMF)、二甲基亞碸(DMSO)、N,N-二甲基乙醯胺、四氫呋喃(THF)、丙酮、甲基乙基酮(MEK)、環己酮、乙酸乙酯、乙腈、二氯甲烷、氯仿、甲苯、乙酸、1-甲氧基-2-丙醇(PGME)、水等,其等可單獨使用一種或組合兩種以上而使用。 The particle dispersion gel of the present embodiment may also contain a solvent other than the polyol compound (B1) as the solvent (B). The solvent other than the polyol compound (B1) is not particularly limited, and examples thereof include methanol, ethanol, isopropyl alcohol (IPA), N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide, tetrahydrofuran (THF), acetone, methyl ethyl ketone (MEK), cyclohexanone, ethyl acetate, acetonitrile, dichloromethane, chloroform, toluene, acetic acid, 1-methoxy-2-propanol (PGME), water, etc., and they may be used alone or in combination of two or more.

就進一步提昇粒子分散用凝膠之網格尺寸之控制性之觀點而言,溶劑(B)包含較佳為30質量%以上、更佳為40質量%以上、進而較佳為50質量%以上、進而較佳為60質量%以上、進而較佳為80質量%以上之多元醇化合物(B1),並且,較佳為可包含100質量%以下。From the viewpoint of further improving the controllability of the mesh size of the particle dispersion gel, the solvent (B) preferably contains 30 mass % or more, more preferably 40 mass % or more, further preferably 50 mass % or more, further preferably 60 mass % or more, further preferably 80 mass % or more of the polyol compound (B1), and preferably contains 100 mass % or less.

就進一步增大網格尺寸之觀點或進一步提昇凝膠強度之觀點、進一步提昇內包於凝膠中之粒子之移動性之觀點而言,溶劑(B)之沸點較佳為180℃以上,更佳為190℃以上,進而較佳為195℃以上,進而較佳為200℃以上,進而較佳為210℃以上,進而較佳為220℃以上,進而較佳為230℃以上,進而較佳為235℃以上,就進一步縮小網格尺寸之觀點或進一步提昇內包於凝膠中之粒子之分散性、保持性之觀點而言,較佳為300℃以下,更佳為280℃以下,進而較佳為260℃以下,進而較佳為255℃以下,進而較佳為245℃以下。From the viewpoint of further increasing the mesh size, further improving the gel strength, and further improving the mobility of the particles contained in the gel, the boiling point of the solvent (B) is preferably 180°C or higher, more preferably 190°C or higher, further preferably 195°C or higher, further preferably 200°C or higher, further preferably 210°C or higher, further preferably 220°C or higher. From the viewpoint of further reducing the mesh size or further improving the dispersibility and retention of the particles contained in the gel, the temperature is preferably below 300°C, more preferably below 280°C, further preferably below 260°C, further preferably below 255°C, further preferably below 245°C.

就進一步增大網格尺寸之觀點或進一步提昇凝膠強度之觀點、進一步提昇內包於凝膠中之粒子之移動性之觀點而言,利用B型黏度計於25℃、轉速30 rpm之條件下測得之溶劑(B)之黏度較佳為1 mPa・s以上,更佳為5 mPa・s以上,進而較佳為10 mPa・s以上,進而較佳為15 mPa・s以上,進而較佳為20 mPa・s以上,就進一步縮小網格尺寸之觀點或進一步提昇內包於凝膠中之粒子之分散性、保持性之觀點而言,較佳為200 mPa・s以下,更佳為150 mPa・s以下,進而較佳為100 mPa・s以下,進而較佳為80 mPa・s以下。From the viewpoint of further increasing the mesh size or further improving the gel strength, and from the viewpoint of further improving the mobility of the particles contained in the gel, the viscosity of the solvent (B) measured by a B-type viscometer at 25°C and a rotation speed of 30 rpm is preferably 1 mPa・s or more, more preferably 5 mPa・s or more, further preferably 10 mPa・s or more, further preferably 15 mPa・s or more, further preferably 20 mPa・s or more. From the viewpoint of further reducing the mesh size or further improving the dispersibility and retention of the particles contained in the gel, it is preferably 200 mPa・s or less, more preferably 150 mPa・s or less, further preferably 100 mPa・s or less, further preferably 80 mPa・s or less. mPa・s or less.

就進一步增大網格尺寸之觀點或進一步提昇凝膠強度之觀點、進一步提昇內包於凝膠中之粒子之移動性之觀點而言,多元醇化合物(B1)之分子量較佳為50以上,更佳為60以上,進而較佳為70以上,進而較佳為75以上,進而較佳為80以上,進而較佳為85以上,就進一步縮小網格尺寸之觀點或進一步提昇內包於凝膠中之粒子之分散性、保持性之觀點而言,較佳為300以下,更佳為250以下,進而較佳為200以下,進而較佳為150以下,進而較佳為130以下,進而較佳為110以下。From the viewpoint of further increasing the mesh size or further improving the gel strength or further improving the mobility of the particles contained in the gel, the molecular weight of the polyol compound (B1) is preferably 50 or more, more preferably 60 or more, further preferably 70 or more, further preferably 75 or more, further preferably 80 or more, further preferably 85 or more. From the viewpoint of further reducing the mesh size or further improving the dispersibility and retention of the particles contained in the gel, it is preferably 300 or less, more preferably 250 or less, further preferably 200 or less, further preferably 150 or less, further preferably 130 or less, further preferably 110 or less.

就進一步提昇內包於凝膠中之粒子之移動性之觀點或進一步提昇凝膠之穩定性之觀點而言,利用錐板黏度計於25℃、錐2°/20 mm、剪切速度15 s -1之條件下測得之本實施方式之粒子分散用凝膠的黏度較佳為10 mPa・s以上,更佳為50 mPa・s以上,進而較佳為100 mPa・s以上,進而較佳為200 mPa・s以上,進而較佳為300 mPa・s以上,進而較佳為400 mPa・s以上,並且,較佳為60000 mPa・s以下,更佳為30000 mPa・s以下,進而較佳為5000 mPa・s以下,進而較佳為2000 mPa・s以下,進而較佳為1500 mPa・s以下,進而較佳為1000 mPa・s以下,進而較佳為800 mPa・s以下。 From the viewpoint of further improving the mobility of the particles contained in the gel or the viewpoint of further improving the stability of the gel, the viscosity of the particle dispersion gel of the present embodiment measured by a cone plate viscometer at 25°C, cone 2°/20 mm, and shear rate 15 s -1 is preferably 10 mPa・s or more, more preferably 50 mPa・s or more, further preferably 100 mPa・s or more, further preferably 200 mPa・s or more, further preferably 300 mPa・s or more, further preferably 400 mPa・s or more, and preferably 60000 mPa・s or less, more preferably 30000 mPa・s or less, further preferably 5000 mPa・s or less, further preferably 2000 mPa・s or less, more preferably 1500 mPa・s or less, further preferably 1000 mPa・s or less, further preferably 800 mPa・s or less.

將藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之最頻粒徑設為X 1(nm),將藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之中值粒徑設為(X 2)(nm)時,X 1/X 2較佳為0.20以上2.0以下。 對於粒子分散用凝膠,要求提昇所內包之粒子之分散性。 本發明人等為了提昇粒子分散用凝膠中所內包之粒子之分散性,而反覆進行了銳意研究。結果發現,於具有立體網狀結構之粒子分散用凝膠中,藉由將立體網狀結構之最頻粒徑與中值粒徑之比率設為特定範圍,可進一步提昇內包之粒子之分散性。具體而言,本實施方式之粒子分散用凝膠藉由將上述X 1/X 2調整為0.20以上2.0以下之範圍,可進一步提昇內包之粒子之分散性。 When the mode particle size of the above-mentioned three-dimensional network structure measured by the photon correlation method according to JIS Z 8826:2019 is set to X 1 (nm), and the median particle size of the above-mentioned three-dimensional network structure measured by the photon correlation method according to JIS Z 8826:2019 is set to (X 2 ) (nm), X 1 /X 2 is preferably 0.20 or more and 2.0 or less. For the particle dispersion gel, it is required to improve the dispersibility of the particles contained therein. The inventors of the present invention have repeatedly conducted intensive studies to improve the dispersibility of the particles contained in the particle dispersion gel. As a result, it was found that in a particle dispersing gel having a three-dimensional network structure, by setting the ratio of the modal particle size to the median particle size of the three-dimensional network structure to a specific range, the dispersibility of the particles contained therein can be further improved. Specifically, the particle dispersing gel of the present embodiment can further improve the dispersibility of the particles contained therein by adjusting the above X1 / X2 to a range of 0.20 or more and 2.0 or less.

於本實施方式之粒子分散用凝膠中,就進一步提昇所內包之粒子之分散性之觀點而言,上述X 1/X 2為0.20以上,較佳為0.30以上,更佳為0.40以上,進而較佳為0.50以上,進而較佳為0.60以上,並且,為2.0以下,較佳為1.8以下,更佳為1.7以下,進而較佳為1.6以下。 In the particle dispersing gel of the present embodiment, from the viewpoint of further improving the dispersibility of the particles contained therein, the above X1 / X2 is 0.20 or more, preferably 0.30 or more, more preferably 0.40 or more, further preferably 0.50 or more, further preferably 0.60 or more, and is 2.0 or less, preferably 1.8 or less, further preferably 1.7 or less, further preferably 1.6 or less.

就進一步提昇內包於凝膠中之粒子之移動性及分散性之觀點而言,藉由依據JIS Z 8826:2019之光子相關法所測得之本實施方式之粒子分散用凝膠中之立體網狀結構的最頻粒徑(X 1)較佳為10 nm以上,更佳為20 nm以上,進而較佳為50 nm以上,進而較佳為70 nm以上,進而較佳為100 nm以上,進而較佳為200 nm以上,進而較佳為300 nm以上,進而較佳為400 nm以上,就進一步提昇內包於凝膠中之粒子之保持性及凝膠強度之觀點而言,較佳為10000 nm以下,更佳為5000 nm以下,進而較佳為2000 nm以下,進而較佳為1500 nm以下,進而較佳為1000 nm以下。 From the viewpoint of further improving the mobility and dispersibility of the particles contained in the gel, the maximum frequency particle size (X1) of the three-dimensional network structure in the particle dispersion gel of the present embodiment measured by the photon correlation method according to JIS Z 8826: 2019 is preferably 10 nm or more, more preferably 20 nm or more, further preferably 50 nm or more, further preferably 70 nm or more, further preferably 100 nm or more, further preferably 200 nm or more, further preferably 300 nm or more, further preferably 400 nm or more. From the viewpoint of further improving the retention of the particles contained in the gel and the gel strength, it is preferably 10000 nm or less, more preferably 5000 nm or less, further preferably 2000 nm or less. nm or less, more preferably 1500 nm or less, and further preferably 1000 nm or less.

就進一步提昇內包於凝膠中之粒子之移動性及分散性之觀點而言,藉由依據JIS Z 8826:2019之光子相關法所測得之本實施方式之粒子分散用凝膠中之立體網狀結構的中值粒徑(X 2)較佳為50 nm以上,更佳為70 nm以上,進而較佳為80 nm以上,進而較佳為100 nm以上,進而較佳為200 nm以上,進而較佳為300 nm以上,進而較佳為400 nm以上,進而較佳為500 nm以上,就進一步提昇內包於凝膠中之粒子之保持性及凝膠強度之觀點而言,較佳為10000 nm以下,更佳為5000 nm以下,進而較佳為2000 nm以下,進而較佳為1500 nm以下,進而較佳為1000 nm以下,進而較佳為800 nm以下。 From the viewpoint of further improving the mobility and dispersibility of the particles contained in the gel, the median particle size (X 2 ) of the three-dimensional network structure in the particle dispersion gel of the present embodiment measured by the photon correlation method according to JIS Z 8826:2019 is preferably 50 nm or more, more preferably 70 nm or more, further preferably 80 nm or more, further preferably 100 nm or more, further preferably 200 nm or more, further preferably 300 nm or more, further preferably 400 nm or more, further preferably 500 nm or more. From the viewpoint of further improving the retention of the particles contained in the gel and the gel strength, it is preferably 10000 nm or less, more preferably 5000 nm or less, further preferably 2000 nm or less. nm or less, further preferably 1500 nm or less, further preferably 1000 nm or less, further preferably 800 nm or less.

作為本實施方式之粒子分散用凝膠之用途,例如可例舉選自由配線修復材、人工組織用材料、再生支架用材料、密封材、抗黏連材、藥物遞送用材料、隱形眼鏡用材料、感測器材料、表面塗佈材、分離材料、抗菌材、除臭材、創傷被覆材、觸媒、抗病毒劑及防黴劑等所組成之群中之一種或兩種以上中使用之凝膠。 其等中,本實施方式之粒子分散用凝膠較佳為用作構成配線修復材之凝膠。 As the use of the particle dispersion gel of the present embodiment, for example, it can be selected from one or more of the group consisting of wiring repair materials, artificial tissue materials, regenerative stent materials, sealing materials, anti-adhesion materials, drug delivery materials, contact lens materials, sensor materials, surface coating materials, separation materials, antibacterial materials, deodorizing materials, wound covering materials, catalysts, antiviral agents and antifungal agents. Among them, the particle dispersion gel of the present embodiment is preferably used as a gel constituting a wiring repair material.

作為內包於本實施方式之粒子分散用凝膠中之粒子,可根據粒子分散用凝膠之用途適當選擇,故無特別限定,例如可例舉選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑等所組成之群中之一種或兩種以上。 其等中,作為內包於本實施方式之粒子分散用凝膠中之粒子,較佳為金屬粒子,更佳為導電性金屬微粒子,進而較佳為包含選自由銅、金、銀及鋁所組成之群中之一種或兩種以上之導電性金屬微粒子,進而較佳為銅微粒子。又,上述金屬粒子亦可僅其表面包含上述金屬。 The particles contained in the particle dispersion gel of the present embodiment can be appropriately selected according to the purpose of the particle dispersion gel, so there is no particular limitation. For example, one or more of the group consisting of drugs, fragrances, antibacterial agents, bactericides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents can be cited. Among them, the particles contained in the particle dispersion gel of the present embodiment are preferably metal particles, more preferably conductive metal microparticles, and more preferably conductive metal microparticles containing one or more of the group consisting of copper, gold, silver and aluminum, and more preferably copper microparticles. In addition, the above-mentioned metal particles may also contain the above-mentioned metal only on their surfaces.

上述配線修復材例如為於電氣配線產生斷線部之情形時,可進行自修復之自修復型配線中使用者,例如包含粒子分散用凝膠及導電性金屬微粒子。導電性金屬微粒子分散於粒子分散用凝膠中。關於自修復型配線,於配線產生斷線部之情形時,藉由配線修復材將其修復。於用配線修復材覆蓋斷線部之情形時,一部分導電性金屬微粒子使斷線部短路,藉此斷線部通電。The wiring repair material is used in self-repairing wiring that can self-repair when a disconnection occurs in the electrical wiring, for example, and includes a particle dispersion gel and conductive metal particles. The conductive metal particles are dispersed in the particle dispersion gel. With respect to the self-repairing wiring, when a disconnection occurs in the wiring, the wiring repair material is used to repair it. When the disconnection is covered with the wiring repair material, a portion of the conductive metal particles short-circuits the disconnection, thereby energizing the disconnection.

[粒子分散用凝膠之製造方法] 本實施方式之粒子分散用凝膠例如可藉由包括如下步驟之製造方法獲得:藉由將聚合物(A)及溶劑(B)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散用凝膠。 [Method for producing a particle dispersion gel] The particle dispersion gel of the present embodiment can be obtained, for example, by a production method comprising the following steps: obtaining a gel by mixing a polymer (A) and a solvent (B); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel.

對於具有立體網狀結構之凝膠,例如就提昇內包於內部之粒子之分散性之觀點而言,要求提昇網格尺寸之均勻性。 本發明人等為了達成上述課題,而反覆進行了銳意研究。結果發現,藉由對將聚合物(A)及溶劑(B)加以混合而獲得之凝膠狀物進一步進行混練,可提昇凝膠之網格尺寸之均勻性。具體而言,藉由對將聚合物(A)及溶劑(B)加以混合而獲得之凝膠狀物進行混練,可提昇凝膠之網格尺寸之均勻性。 For a gel having a three-dimensional network structure, for example, from the viewpoint of improving the dispersibility of particles contained therein, it is required to improve the uniformity of the mesh size. The inventors of the present invention have repeatedly conducted intensive research to achieve the above-mentioned subject. As a result, it was found that the uniformity of the mesh size of the gel can be improved by further kneading the gel-like material obtained by mixing the polymer (A) and the solvent (B). Specifically, the uniformity of the mesh size of the gel can be improved by kneading the gel-like material obtained by mixing the polymer (A) and the solvent (B).

(獲得凝膠狀物之步驟) 本實施方式之粒子分散用凝膠中,於獲得凝膠狀物之步驟中,藉由將聚合物(A)及溶劑(B)加以混合而獲得凝膠狀物。例如,可藉由以下程序獲得凝膠狀物。 首先,將聚合物(A)與溶劑(B)加以混合。作為聚合物(A)及溶劑(B),可使用上述者。繼而,一面攪拌所獲得之混合物,一面加熱至40~100℃左右。加熱時間並無特別限定,只要使混合物適度地凝膠化即可,例如為1~60分鐘左右。再者,即使無加熱(室溫),若花費充分之時間,則混合物亦凝膠化。繼而,停止加熱及攪拌並靜置,藉此可獲得凝膠狀物。 (Step of obtaining a gel-like substance) In the step of obtaining a gel-like substance in the particle dispersion gel of the present embodiment, a gel-like substance is obtained by mixing a polymer (A) and a solvent (B). For example, a gel-like substance can be obtained by the following procedure. First, a polymer (A) and a solvent (B) are mixed. As polymer (A) and solvent (B), the above-mentioned ones can be used. Then, the obtained mixture is heated to about 40 to 100°C while stirring. The heating time is not particularly limited, as long as the mixture is appropriately gelled, for example, about 1 to 60 minutes. Furthermore, even without heating (room temperature), the mixture will gel if sufficient time is spent. Then, stop heating and stirring and let stand to obtain a gel-like substance.

(獲得粒子分散用凝膠之步驟) 繼而,藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散用凝膠。 作為上述凝膠狀物之混練方法,就進一步提昇本實施方式之粒子分散用凝膠中之立體網狀結構之均勻性的觀點而言,較佳為使用選自由輥磨機及球磨機所組成之群中之至少一種之混練,更佳為使用輥磨機之混練。 (Step of obtaining a particle dispersion gel) Then, the above-mentioned gel-like material is kneaded to obtain a particle dispersion gel having a three-dimensional network structure. As a method for kneading the above-mentioned gel-like material, from the viewpoint of further improving the uniformity of the three-dimensional network structure in the particle dispersion gel of this embodiment, it is preferred to use at least one selected from the group consisting of a roll mill and a ball mill for kneading, and it is more preferred to use a roll mill for kneading.

本實施方式之輥磨機較佳為包含3個以上之輥,更佳為三輥輥磨機。藉此可連續地進行上述凝膠狀物之混練,故可進一步提昇所獲得之粒子分散用凝膠之生產性。The roller mill of this embodiment preferably comprises three or more rollers, and more preferably a three-roller mill. This allows the gel-like material to be mixed continuously, thereby further improving the productivity of the obtained particle dispersion gel.

[粒子分散凝膠] 本實施方式之粒子分散凝膠包含本實施方式之粒子分散用凝膠、及分散於上述粒子分散用凝膠中之粒子(C)。 就提昇凝膠黏度且進一步縮小網格尺寸之觀點而言,本實施方式之粒子分散凝膠中之聚合物(A)之含量較佳為0.01質量%以上,更佳為0.05質量%以上,進而較佳為0.1質量%以上,進而較佳為0.2質量%以上,進而較佳為0.3質量%以上,就進一步增大網格尺寸之觀點而言,較佳為20.0質量%以下,更佳為15.0質量%以下,進而較佳為10.0質量%以下,進而較佳為5.0質量%以下,進而較佳為2.5質量%以下,進而較佳為1.5質量%以下,進而較佳為1.0質量%以下,進而較佳為0.8質量%以下。 本實施方式之粒子分散凝膠中之上述粒子(C)之含量可根據粒子分散凝膠之用途或內包之粒子(C)之種類適當選擇,故無特別限定,於將粒子分散凝膠之整體設為100質量%時,例如為0.01質量%以上,較佳為0.02質量%以上,更佳為0.05質量%以上,進而較佳為0.3質量%以上,並且,例如為30質量%以下,較佳為10質量%以下,更佳為5質量%以下,進而較佳為1質量%以下,進而較佳為0.5質量%以下。 [Particle dispersion gel] The particle dispersion gel of this embodiment includes the particle dispersion gel of this embodiment and particles (C) dispersed in the particle dispersion gel. From the viewpoint of increasing gel viscosity and further reducing mesh size, the content of polymer (A) in the particle dispersion gel of the present embodiment is preferably 0.01 mass % or more, more preferably 0.05 mass % or more, further preferably 0.1 mass % or more, further preferably 0.2 mass % or more, further preferably 0.3 mass % or more, and from the viewpoint of further increasing mesh size, it is preferably 20.0 mass % or less, more preferably 15.0 mass % or less, further preferably 10.0 mass % or less, further preferably 5.0 mass % or less, further preferably 2.5 mass % or less, further preferably 1.5 mass % or less, further preferably 1.0 mass % or less, further preferably 0.8 mass % or less. The content of the above particles (C) in the particle dispersion gel of the present embodiment can be appropriately selected according to the purpose of the particle dispersion gel or the type of particles (C) contained therein, and is therefore not particularly limited. When the entire particle dispersion gel is set to 100 mass%, it is, for example, 0.01 mass% or more, preferably 0.02 mass% or more, more preferably 0.05 mass% or more, and further preferably 0.3 mass% or more, and, for example, 30 mass% or less, preferably 10 mass% or less, more preferably 5 mass% or less, further preferably 1 mass% or less, and further preferably 0.5 mass% or less.

作為本實施方式之粒子分散凝膠之用途,例如可例舉選自由配線修復材、人工組織用材料、再生支架用材料、密封材、抗黏連材、藥物遞送用材料、隱形眼鏡用材料、感測器材料、表面塗佈材、分離材料、抗菌材、除臭材、創傷被覆材、觸媒、抗病毒劑及防黴劑等所組成之群中之一種或兩種以上。 其等中,本實施方式之粒子分散凝膠較佳為用作配線修復材。 As the use of the particle dispersion gel of the present embodiment, for example, one or more of the group consisting of wiring repair materials, artificial tissue materials, regenerative stent materials, sealing materials, anti-adhesion materials, drug delivery materials, contact lens materials, sensor materials, surface coating materials, separation materials, antibacterial materials, deodorizing materials, wound covering materials, catalysts, antiviral agents and antifungal agents can be cited. Among them, the particle dispersion gel of the present embodiment is preferably used as a wiring repair material.

作為本實施方式之粒子分散凝膠中使用之粒子(C),可根據粒子分散凝膠之用途適當選擇,故無特別限定,例如可例舉選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑等所組成之群中之一種或兩種以上。 其等中,本實施方式之粒子分散凝膠中使用之粒子(C)較佳為金屬粒子,更佳為導電性金屬微粒子,進而較佳為包含選自由銅、金、銀及鋁所組成之群中之一種或兩種以上之導電性金屬微粒子,進而較佳為銅微粒子。又,上述金屬粒子亦可僅其表面包含上述金屬。 The particles (C) used in the particle dispersion gel of the present embodiment can be appropriately selected according to the purpose of the particle dispersion gel, so there is no particular limitation. For example, one or two or more selected from the group consisting of drugs, fragrances, antibacterial agents, bactericides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents can be cited. Among them, the particles (C) used in the particle dispersion gel of the present embodiment are preferably metal particles, more preferably conductive metal microparticles, and more preferably conductive metal microparticles containing one or two or more selected from the group consisting of copper, gold, silver and aluminum, and more preferably copper microparticles. In addition, the above-mentioned metal particles may also contain the above-mentioned metal only on their surfaces.

就進一步提昇粒子(C)之移動性及分散性之觀點而言,藉由雷射繞射散射法測得之上述粒子(C)之中值粒徑D 50較佳為0.01 μm以上,更佳為0.05 μm以上,進而較佳為0.1 μm以上,進而較佳為0.3 μm以上,就進一步提昇粒子(C)之保持性之觀點而言,較佳為10 μm以下,更佳為5 μm以下,進而較佳為3 μm以下,進而較佳為1 μm以下。 From the viewpoint of further improving the mobility and dispersibility of the particles (C), the median particle size D50 of the particles (C) measured by the laser diffraction scattering method is preferably 0.01 μm or more, more preferably 0.05 μm or more, further preferably 0.1 μm or more, further preferably 0.3 μm or more. From the viewpoint of further improving the retention of the particles (C), it is preferably 10 μm or less, more preferably 5 μm or less, further preferably 3 μm or less, further preferably 1 μm or less.

[粒子分散凝膠之製造方法] 本實施方式之粒子分散凝膠例如可藉由對本實施方式之粒子分散用凝膠、及上述粒子(C)進行混練而獲得。 作為對本實施方式之粒子分散用凝膠、及上述粒子(C)進行混練之方法,就進一步提昇本實施方式之粒子分散凝膠中之粒子(C)之分散性之觀點而言,較佳為使用選自由輥磨機及球磨機所組成之群中之至少一種之混練,更佳為使用輥磨機之混練。 [Method for producing particle-dispersed gel] The particle-dispersed gel of the present embodiment can be obtained, for example, by kneading the particle-dispersed gel of the present embodiment and the above-mentioned particles (C). As a method for kneading the particle-dispersed gel of the present embodiment and the above-mentioned particles (C), from the viewpoint of further improving the dispersibility of the particles (C) in the particle-dispersed gel of the present embodiment, kneading using at least one selected from the group consisting of a roll mill and a ball mill is preferred, and kneading using a roll mill is more preferred.

本實施方式之輥磨機較佳為包含3個以上之輥,更佳為三輥輥磨機。藉此可連續地進行本實施方式之粒子分散用凝膠與上述粒子之混練,故可進一步提昇所獲得之粒子分散凝膠之生產性。The roller mill of this embodiment preferably comprises three or more rollers, and more preferably a three-roller mill. In this way, the particle dispersion gel of this embodiment and the above particles can be continuously mixed, thereby further improving the productivity of the obtained particle dispersion gel.

又,本實施方式之粒子分散凝膠例如亦可藉由包括如下步驟之製造方法獲得:藉由將聚合物(A)、溶劑(B)及粒子(C)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散凝膠。Furthermore, the particle-dispersed gel of the present embodiment can also be obtained, for example, by a manufacturing method comprising the following steps: obtaining a gel-like substance by mixing a polymer (A), a solvent (B) and particles (C); and obtaining a particle-dispersed gel having a three-dimensional network structure by kneading the above-mentioned gel-like substance.

根據本實施方式之粒子分散凝膠之製造方法,藉由對將聚合物(A)、溶劑(B)及粒子(C)加以混合而獲得之凝膠狀物進一步進行混練,可提昇粒子(C)之分散性。具體而言,藉由對將聚合物(A)、溶劑(B)及粒子(C)加以混合而獲得之凝膠狀物進一步進行混練,可提昇凝膠之網格尺寸之均勻性。According to the method for producing a particle dispersion gel of the present embodiment, the dispersibility of the particles (C) can be improved by further kneading the gel-like material obtained by mixing the polymer (A), the solvent (B) and the particles (C). Specifically, the uniformity of the mesh size of the gel can be improved by further kneading the gel-like material obtained by mixing the polymer (A), the solvent (B) and the particles (C).

藉由本實施方式之粒子分散凝膠之製造方法獲得之粒子分散凝膠例如藉由聚合物(A)形成立體網狀結構,且於網狀結構內含有溶劑(B),粒子(C)內包於網狀結構內。The particle dispersion gel obtained by the method for producing the particle dispersion gel of the present embodiment, for example, forms a three-dimensional network structure with the polymer (A), and the network structure contains the solvent (B), and the particles (C) are enclosed in the network structure.

(獲得凝膠狀物之步驟) 於本實施方式之粒子分散凝膠之製造方法中,於獲得凝膠狀物之步驟中,藉由將聚合物(A)、溶劑(B)及粒子(C)加以混合而獲得凝膠狀物。例如可藉由以下程序獲得凝膠狀物。 首先,將聚合物(A)、溶劑(B)及粒子(C)加以混合。作為聚合物(A)及溶劑(B),可使用上述者。繼而,一面攪拌所獲得之混合物,一面加熱至40~100℃左右。加熱時間並無特別限定,只要使混合物適度地凝膠化即可,例如為1~60分鐘左右。再者,即使無加熱(室溫),若花費充分之時間,則混合物亦凝膠化。繼而,停止加熱及攪拌並靜置,藉此可獲得凝膠狀物。 (Step of obtaining a gel-like substance) In the method for producing a particle-dispersed gel of the present embodiment, in the step of obtaining a gel-like substance, a polymer (A), a solvent (B) and particles (C) are mixed to obtain a gel-like substance. For example, a gel-like substance can be obtained by the following procedure. First, a polymer (A), a solvent (B) and particles (C) are mixed. As polymer (A) and solvent (B), the above-mentioned ones can be used. Then, the obtained mixture is heated to about 40 to 100°C while stirring. The heating time is not particularly limited, as long as the mixture is appropriately gelled, for example, about 1 to 60 minutes. Furthermore, even without heating (room temperature), the mixture will gel if sufficient time is spent. Then, stop heating and stirring and let stand to obtain a gel-like substance.

(獲得粒子分散凝膠之步驟) 繼而,藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散凝膠。 作為上述凝膠狀物之混練方法,就進一步提昇本實施方式之粒子分散凝膠中之立體網格尺寸之均勻性的觀點而言,較佳為使用選自由輥磨機及球磨機所組成之群中之至少一種之混練,更佳為使用輥磨機之混練。 (Step of obtaining a particle-dispersed gel) Then, the above-mentioned gel-like material is kneaded to obtain a particle-dispersed gel having a three-dimensional network structure. As a kneading method for the above-mentioned gel-like material, from the viewpoint of further improving the uniformity of the three-dimensional network size in the particle-dispersed gel of this embodiment, it is preferred to use at least one selected from the group consisting of a roll mill and a ball mill for kneading, and it is more preferred to use a roll mill for kneading.

本實施方式之輥磨機較佳為包含3個以上之輥,更佳為三輥輥磨機。藉此可連續地進行上述凝膠狀物之混練,故可進一步提昇所獲得之粒子分散凝膠之生產性。The roller mill of this embodiment preferably comprises three or more rollers, and more preferably a three-roller mill. This allows the gel-like material to be mixed continuously, thereby further improving the productivity of the obtained particle-dispersed gel.

以上,對本發明之實施方式進行了敍述,但其等係本發明之例示,可於不損害本發明之效果之範圍內,採用除上述以外之各種構成。The above is a description of the embodiments of the present invention, but these are merely examples of the present invention, and various configurations other than the above may be adopted within the scope of not impairing the effects of the present invention.

再者,本發明並不限定於上述實施方式,可達成本發明之目的之範圍內之變化、改良等包含於本發明中。 實施例 Furthermore, the present invention is not limited to the above-mentioned implementation methods, and changes and improvements within the scope of achieving the purpose of the present invention are included in the present invention. Example

以下,參照實施例對本發明詳細地進行說明,但本發明並不受該等實施例之記載任何限定。Hereinafter, the present invention will be described in detail with reference to embodiments, but the present invention is not limited in any way to the description of these embodiments.

[材料] 用於製造粒子分散用凝膠之材料之詳細情況如下所述。 (聚合物(A)) ・羥丙基纖維素(富士膠片和光純藥公司製造) [Materials] Details of the materials used to produce the particle dispersion gel are as follows. (Polymer (A)) ・Hydroxypropylcellulose (manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.)

(溶劑(B)) ・乙二醇(分子量:62.07,沸點:198℃,富士膠片和光純藥公司製造) ・1,3-丙二醇(分子量:76.09,沸點:214℃,富士膠片和光純藥公司製造) ・1,4-丁二醇(分子量:90.12,沸點:230℃,富士膠片和光純藥公司製造) ・1,5-戊二醇(分子量:104.15,沸點:242℃,富士膠片和光純藥公司製造) ・1,6-己二醇(分子量:118.17,沸點:250℃,富士膠片和光純藥公司製造) (Solvent (B)) ・Ethylene glycol (molecular weight: 62.07, boiling point: 198℃, manufactured by Fuji Film Wako Jun Chemical Co., Ltd.) ・1,3-Propanediol (molecular weight: 76.09, boiling point: 214℃, manufactured by Fuji Film Wako Jun Chemical Co., Ltd.) ・1,4-Butanediol (molecular weight: 90.12, boiling point: 230℃, manufactured by Fuji Film Wako Jun Chemical Co., Ltd.) ・1,5-Pentanediol (molecular weight: 104.15, boiling point: 242℃, manufactured by Fuji Film Wako Jun Chemical Co., Ltd.) ・1,6-Hexanediol (molecular weight: 118.17, boiling point: 250℃, manufactured by Fuji Film Wako Jun Chemical Co., Ltd.)

(粒子(C)) ・銅粒子:(FURUKAWA CHEMICALS公司製造之金屬銅粉,商品號:FMC-SB,藉由雷射繞射散射法測得之中值粒徑D 50:0.7 μm) (Particles (C)) ・Copper particles: (Metallic copper powder manufactured by FURUKAWA CHEMICALS, product number: FMC-SB, median particle size D 50 measured by laser diffraction scattering method: 0.7 μm)

[測定及評價] 於本實施例中,各種測定及評價係藉由以下方法進行。 [Measurement and Evaluation] In this embodiment, various measurements and evaluations are performed by the following methods.

(溶劑(B)之黏度) 使用B型黏度計(東機產業公司製造,製品名:TVB-10M,轉子No.1),於25℃、轉速30 rpm、溶劑(B)200 mL之條件下,測定溶劑(B)之黏度。此處,於使用2種以上之混合溶劑作為溶劑(B)之情形時,測定混合溶劑之黏度。 (Viscosity of solvent (B)) Use a B-type viscometer (manufactured by Toki Sangyo Co., Ltd., product name: TVB-10M, rotor No. 1) to measure the viscosity of solvent (B) at 25°C, rotation speed 30 rpm, and solvent (B) 200 mL. Here, when a mixed solvent of two or more is used as solvent (B), the viscosity of the mixed solvent is measured.

(粒子分散用凝膠之黏度) 使用錐板黏度計(Spectris公司製造,製品名:Kinexus pro+),於25℃、錐2°/20 mm、剪切速度15 s -1之條件下測定凝膠之黏度。 (Viscosity of the gel for particle dispersion) The viscosity of the gel was measured using a cone plate viscometer (manufactured by Spectris Corporation, product name: Kinexus pro+) at 25°C, cone 2°/20 mm, and shear rate 15 s -1 .

(粒子分散用凝膠之立體網狀結構之最頻粒徑(X 1)、中值粒徑(X 2)及半值寬) 粒子分散用凝膠之立體網狀結構之最頻粒徑(X 1)、中值粒徑(X 2)及半值寬係藉由依據JIS Z 8826:2019之光子相關法進行測定。作為測定裝置,使用HORIBA公司製造之奈米粒子解析裝置SZ-100V2凝膠單元。作為測定條件,將測定範圍設為0.3 nm~10 μm,將分佈形態設為多分散、寬分佈,將雷射照射位置以100 μm為步長設為10個點(0~900 μm)。於向測定槽中投入樣品時混入氣泡之情形時,進行消泡處理。 又,算出所獲得之立體網狀結構之網格尺寸分佈曲線之半值寬。上述半值寬係算出2個網格尺寸分佈曲線之頻度(%)為最大值之一半之網格尺寸(nm),將其等之差設為半值寬。 (Mode particle size (X 1 ), median particle size (X 2 ) and half-value width of the three-dimensional network structure of the particle dispersion gel) The mode particle size (X 1 ), median particle size (X 2 ) and half-value width of the three-dimensional network structure of the particle dispersion gel were measured by the photon correlation method in accordance with JIS Z 8826:2019. As a measuring device, a nanoparticle analyzer SZ-100V2 gel unit manufactured by HORIBA was used. As measurement conditions, the measurement range was set to 0.3 nm to 10 μm, the distribution form was set to polydisperse and wide distribution, and the laser irradiation position was set to 10 points (0 to 900 μm) with a step size of 100 μm. When bubbles are mixed into the sample when it is put into the measuring tank, defoaming treatment is performed. In addition, the half-value width of the grid size distribution curve of the obtained three-dimensional network structure is calculated. The above half-value width is calculated by calculating the grid size (nm) at which the frequency (%) of the two grid size distribution curves is half of the maximum value, and the difference between them is set as the half-value width.

(粒子之分散性評價) 將實施例11~16中獲得之粒子分散用凝膠50 g、及作為粒子(C)之銅粒子20 mg充分地混合而獲得混合物。 繼而,將所獲得之混合物50 g通過三輥輥磨機(AIMEX公司製造之BR-150V)1次,獲得銅粒子分散凝膠。此處,將三輥輥磨機之第一輥~第三輥之通過設為1次。各輥使用直徑為63.5 mm者,輥間之距離設為10 μm。又,設為第一輥之轉速:第二輥之轉速:第三輥之轉速=1.0:2.4:6.0,將第三輥之轉速設為80 rpm。對所獲得之銅粒子分散凝膠進行以下分散性評價。 首先,將所獲得之銅粒子分散凝膠50 g靜置24小時,藉由目視按照以下基準對銅粒子之分散性進行評價。 A(分散性良好):銅粒子於凝膠中均勻地分散,銅粒子之分散性良好(凝膠整體變成紅褐色)。 B(分散性不良):銅粒子於凝膠中偏集存在,銅粒子之分散性不良(凝膠整體變成紅褐色,但色調有深有淺)。 (Evaluation of particle dispersibility) 50 g of the particle dispersion gel obtained in Examples 11 to 16 and 20 mg of copper particles as particles (C) were fully mixed to obtain a mixture. Then, 50 g of the obtained mixture was passed through a three-roll mill (BR-150V manufactured by AIMEX) once to obtain a copper particle dispersion gel. Here, the passing of the first to third rolls of the three-roll mill was set to 1 time. Each roll had a diameter of 63.5 mm, and the distance between the rolls was set to 10 μm. In addition, the rotation speed of the first roll: the rotation speed of the second roll: the rotation speed of the third roll = 1.0:2.4:6.0, and the rotation speed of the third roll was set to 80 rpm. The obtained copper particle dispersion gel was evaluated for dispersibility as follows. First, 50 g of the obtained copper particle dispersion gel was left to stand for 24 hours, and the dispersibility of the copper particles was evaluated visually according to the following criteria. A (good dispersibility): The copper particles were uniformly dispersed in the gel, and the dispersibility of the copper particles was good (the gel turned reddish brown as a whole). B (poor dispersibility): The copper particles were concentrated in the gel, and the dispersibility of the copper particles was poor (the gel turned reddish brown as a whole, but the color tone was dark and light).

(銅粒子之分散性評價) 將實施例19及20中獲得之銅粒子分散凝膠50 g靜置24小時,藉由目視評價銅粒子之分散性。 (Evaluation of the dispersibility of copper particles) 50 g of the copper particle dispersion gel obtained in Examples 19 and 20 was left to stand for 24 hours, and the dispersibility of the copper particles was evaluated by visual inspection.

實施例1 首先,將作為聚合物(A)之羥丙基纖維素與作為溶劑(B)之乙二醇充分地混合而獲得混合物。聚合物(A)及溶劑(B)之調配量係如表1所記載。一面攪拌所獲得之混合物,一面於50℃下加熱2分鐘。藉此混合物變成凝膠。 加熱停止後,將所獲得之凝膠靜置至室溫(23℃)。然後,將處於室溫之凝膠100 g通過三輥輥磨機(AIMEX公司製造之BR-150V)4次,獲得粒子分散用凝膠。此處,將三輥輥磨機之第一輥~第三輥之通過設為1次。各輥使用直徑為63.5 mm者,將輥間之距離設為10 μm。又,設為第一輥之轉速:第二輥之轉速:第三輥之轉速=1.0:2.4:6.0,將第三輥之轉速設為80 rpm。對所獲得之粒子分散用凝膠分別進行上述測定。將結果示於表1。 Example 1 First, hydroxypropyl cellulose as a polymer (A) and ethylene glycol as a solvent (B) are fully mixed to obtain a mixture. The amounts of polymer (A) and solvent (B) are as shown in Table 1. The obtained mixture is heated at 50°C for 2 minutes while being stirred. The mixture is thereby turned into a gel. After the heating is stopped, the obtained gel is allowed to stand at room temperature (23°C). Then, 100 g of the gel at room temperature is passed through a three-roll mill (BR-150V manufactured by AIMEX) 4 times to obtain a gel for particle dispersion. Here, the number of passes of the first to third rolls of the three-roll mill is set to 1. Each roller has a diameter of 63.5 mm and the distance between the rollers is set to 10 μm. In addition, the rotation speed of the first roller: the rotation speed of the second roller: the rotation speed of the third roller is set to 1.0:2.4:6.0, and the rotation speed of the third roller is set to 80 rpm. The above measurements were performed on the obtained particle dispersion gel. The results are shown in Table 1.

實施例2~10 除將聚合物(A)及溶劑(B)之組成變更成表1所示之組成以外,以與實施例1相同之方式分別獲得粒子分散用凝膠。對所獲得之粒子分散用凝膠分別進行上述測定。將結果示於表1。 Examples 2 to 10 Except that the composition of the polymer (A) and the solvent (B) was changed to the composition shown in Table 1, the particle dispersion gel was obtained in the same manner as in Example 1. The above-mentioned measurements were performed on the obtained particle dispersion gel. The results are shown in Table 1.

[表1] 表1 <粒子分散用凝膠之組成> 單位 實施例1 實施例2 實施例3 實施例4 實施例5 實施例6 實施例7 實施例8 實施例9 實施例10 聚合物(A) 羥丙基纖維素 質量份 0.5 0.5 0.5 0.5 0.5 0.1 2.0 3.0 5.0 7.0 溶劑(B) 乙二醇 質量份 99.5          49.75 99.9 98.0 97.0 95.0 93.0 1,3-丙二醇 質量份    99.5                         1,4-丁二醇 質量份       99.5                      1,5-戊二醇 質量份          99.5                   1,6-己二醇 質量份             49.75                溶劑(B)之黏度 mPa・s 16 36 62 93 25 16 16 16 16 16 凝膠之黏度 mPa・s 279 540 713 852 470 33 7990 20100 50300 43200 立體網狀結構之最頻粒徑(X 1) nm 54 81 480 561 851 324 47 47 36 31 立體網狀結構之中值粒徑(X 2) nm 473 99 683 654 563 491 68 56 41 36 [Table 1] Table 1 <Composition of particle dispersion gel> Unit Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7 Embodiment 8 Embodiment 9 Embodiment 10 Polymer (A) Hydroxypropyl cellulose Quality 0.5 0.5 0.5 0.5 0.5 0.1 2.0 3.0 5.0 7.0 Solvent (B) Ethylene glycol Quality 99.5 49.75 99.9 98.0 97.0 95.0 93.0 1,3-Propanediol Quality 99.5 1,4-Butanediol Quality 99.5 1,5-Pentanediol Quality 99.5 1,6-Hexanediol Quality 49.75 Viscosity of solvent (B) mPa・s 16 36 62 93 25 16 16 16 16 16 Gel viscosity mPa・s 279 540 713 852 470 33 7990 20100 50300 43200 The most frequent particle size of the three-dimensional network structure (X 1 ) nm 54 81 480 561 851 324 47 47 36 31 Median particle size in three-dimensional network structure (X 2 ) nm 473 99 683 654 563 491 68 56 41 36

根據表1,可瞭解藉由改變多元醇化合物(B1)之種類或聚合物(A)之濃度,可改變粒子分散用凝膠之網格尺寸。即,可知本實施方式之粒子分散用凝膠容易控制網格尺寸。From Table 1, it can be seen that the mesh size of the particle dispersing gel can be changed by changing the type of the polyol compound (B1) or the concentration of the polymer (A). That is, it can be seen that the mesh size of the particle dispersing gel of the present embodiment is easily controlled.

實施例11 首先,將作為聚合物(A)之羥丙基纖維素與作為溶劑(B)之乙二醇充分地混合而獲得混合物。聚合物(A)及溶劑(B)之調配量係如表2所記載。一面攪拌所獲得之混合物,一面於50℃下加熱2分鐘。藉此,混合物變成凝膠。 加熱停止後,將所獲得之凝膠靜置至室溫(23℃)。然後,將處於室溫之凝膠100 g通過三輥輥磨機(AIMEX公司製造之BR-150V)4次,獲得粒子分散用凝膠。此處,將三輥輥磨機之第一輥~第三輥之通過設為1次。各輥使用直徑為63.5 mm者,將輥間之距離設為10 μm。又,設為第一輥之轉速:第二輥之轉速:第三輥之轉速=1.0:2.4:6.0,將第三輥之轉速設為80 rpm。對所獲得之粒子分散用凝膠分別進行上述測定。將結果示於表2。 Example 11 First, hydroxypropyl cellulose as a polymer (A) and ethylene glycol as a solvent (B) are fully mixed to obtain a mixture. The amounts of polymer (A) and solvent (B) are as shown in Table 2. The obtained mixture is heated at 50°C for 2 minutes while being stirred. Thereby, the mixture becomes a gel. After the heating is stopped, the obtained gel is allowed to stand at room temperature (23°C). Then, 100 g of the gel at room temperature is passed through a three-roll mill (BR-150V manufactured by AIMEX) 4 times to obtain a gel for particle dispersion. Here, the passing of the first to third rolls of the three-roll mill is set to 1 time. Each roller has a diameter of 63.5 mm and the distance between the rollers is set to 10 μm. In addition, the rotation speed of the first roller: the rotation speed of the second roller: the rotation speed of the third roller is set to 1.0:2.4:6.0, and the rotation speed of the third roller is set to 80 rpm. The above measurements were performed on the obtained particle dispersion gel. The results are shown in Table 2.

實施例12~16 除將聚合物(A)及溶劑(B)之組成變更成表2所示之組成以外,以與實施例11相同之方式分別獲得粒子分散用凝膠。對所獲得之粒子分散用凝膠分別進行上述測定。將結果示於表2。 Examples 12 to 16 Except that the composition of the polymer (A) and the solvent (B) was changed to the composition shown in Table 2, the particle dispersion gel was obtained in the same manner as in Example 11. The above-mentioned measurements were performed on the obtained particle dispersion gel. The results are shown in Table 2.

[表2] 表2 <粒子分散用凝膠之組成> 單位 實施例11 實施例12 實施例13 實施例14 實施例15 實施例16 聚合物(A) 羥丙基纖維素 質量份 0.5 0.5 0.5 0.5 0.5 0.1 溶劑(B) 乙二醇 質量份 99.5          49.75 99.9 1,3-丙二醇 質量份    99.5             1,4-丁二醇 質量份       99.5          1,5-戊二醇 質量份          99.5       1,6-己二醇 質量份             49.75    溶劑(B)之黏度 mPa・s 16 36 62 93 25 16 凝膠之黏度 mPa・s 279 540 713 852 470 33 立體網狀結構之最頻粒徑(X 1) nm 54 81 480 561 851 324 立體網狀結構之中值粒徑(X 2) nm 473 99 683 654 563 491 X 1/X 2 - 0.11 0.83 0.70 0.86 1.51 0.66 粒子之分散性評價 - B A A A A A [Table 2] Table 2 <Composition of particle dispersion gel> Unit Embodiment 11 Embodiment 12 Embodiment 13 Embodiment 14 Embodiment 15 Embodiment 16 Polymer (A) Hydroxypropyl cellulose Quality 0.5 0.5 0.5 0.5 0.5 0.1 Solvent (B) Ethylene glycol Quality 99.5 49.75 99.9 1,3-Propanediol Quality 99.5 1,4-Butanediol Quality 99.5 1,5-Pentanediol Quality 99.5 1,6-Hexanediol Quality 49.75 Viscosity of solvent (B) mPa・s 16 36 62 93 25 16 Gel viscosity mPa・s 279 540 713 852 470 33 The most frequent particle size of the three-dimensional network structure (X 1 ) nm 54 81 480 561 851 324 Median particle size in three-dimensional network structure (X 2 ) nm 473 99 683 654 563 491 X1 / X2 - 0.11 0.83 0.70 0.86 1.51 0.66 Particle dispersion evaluation - B A A A A A

根據表2,可瞭解與X 1/X 2未達0.20之實施例11之粒子分散用凝膠相比,X 1/X 2為0.20以上2.0以下之實施例12~16之粒子分散用凝膠提昇內包之粒子之分散性。即,可知X 1/X 2為0.20以上2.0以下之粒子分散用凝膠可提昇內包之粒子之分散性。 According to Table 2, it can be seen that the particle dispersing gels of Examples 12 to 16 with X1 / X2 of 0.20 or more and 2.0 or less can improve the dispersibility of the particles contained therein, compared with the particle dispersing gel of Example 11 with X1 / X2 less than 0.20. In other words, it can be seen that the particle dispersing gels with X1 / X2 of 0.20 or more and 2.0 or less can improve the dispersibility of the particles contained therein.

實施例17 首先,將作為聚合物(A)之羥丙基纖維素與作為溶劑(B)之1,3-丙二醇充分地混合而獲得混合物。聚合物(A)及溶劑(B)之調配量係如表3所記載。一面攪拌所獲得之混合物,一面於50℃下加熱2分鐘。藉此,混合物變成凝膠。 加熱停止後,將所獲得之凝膠靜置至室溫(23℃)。然後,將處於室溫之凝膠100 g通過三輥輥磨機(AIMEX公司製造之BR-150V)4次,獲得凝膠。此處,將三輥輥磨機之第一輥~第三輥之通過設為1次。各輥使用直徑為63.5 mm者,將輥間之距離設為10 μm。又,設為第一輥之轉速:第二輥之轉速:第三輥之轉速=1.0:2.4:6.0,將第三輥之轉速設為80 rpm。對所獲得之凝膠分別進行上述測定。將結果示於表3。 Example 17 First, hydroxypropyl cellulose as a polymer (A) and 1,3-propylene glycol as a solvent (B) are fully mixed to obtain a mixture. The amounts of polymer (A) and solvent (B) are as shown in Table 3. The obtained mixture is heated at 50°C for 2 minutes while being stirred. Thereby, the mixture becomes a gel. After the heating is stopped, the obtained gel is allowed to stand at room temperature (23°C). Then, 100 g of the gel at room temperature is passed through a three-roll mill (BR-150V manufactured by AIMEX) 4 times to obtain a gel. Here, the passing of the first to third rolls of the three-roll mill is set to 1 time. Each roller has a diameter of 63.5 mm and the distance between the rollers is set to 10 μm. In addition, the rotation speed of the first roller: the rotation speed of the second roller: the rotation speed of the third roller is set to 1.0:2.4:6.0, and the rotation speed of the third roller is set to 80 rpm. The above measurements were performed on the obtained gels. The results are shown in Table 3.

實施例18 首先,將作為聚合物(A)之羥丙基纖維素與作為溶劑(B)之1,3-丙二醇充分地混合而獲得混合物。聚合物(A)及溶劑(B)之調配量係如表3所記載。一面攪拌所獲得之混合物,一面於50℃下加熱2分鐘。藉此,混合物變成凝膠。 加熱停止後,將所獲得之凝膠靜置至室溫(23℃),獲得凝膠。對所獲得之凝膠分別進行上述測定。將結果示於表3。 Example 18 First, hydroxypropyl cellulose as a polymer (A) and 1,3-propylene glycol as a solvent (B) are fully mixed to obtain a mixture. The amounts of polymer (A) and solvent (B) are as shown in Table 3. The obtained mixture is heated at 50°C for 2 minutes while being stirred. Thus, the mixture becomes a gel. After the heating is stopped, the obtained gel is left to stand at room temperature (23°C) to obtain a gel. The above-mentioned measurements are performed on the obtained gels. The results are shown in Table 3.

[表3] 表3 <凝膠之組成> 單位 實施例17 實施例18 聚合物(A) 羥丙基纖維素 質量份 0.5 0.5 溶劑(B) 1,3-丙二醇 質量份 99.5 99.5 溶劑(B)之黏度 mPa・s 36 36 立體網狀結構之最頻粒徑(X 1) nm 81 83 立體網狀結構之中值粒徑(X 2) nm 99 62 網格尺寸分佈曲線之半值寬 nm 150 171 [Table 3] Table 3 <Gel composition> Unit Embodiment 17 Embodiment 18 Polymer (A) Hydroxypropyl cellulose Quality 0.5 0.5 Solvent (B) 1,3-Propanediol Quality 99.5 99.5 Viscosity of solvent (B) mPa・s 36 36 The most frequent particle size of the three-dimensional network structure (X 1 ) nm 81 83 Median particle size in three-dimensional network structure (X 2 ) nm 99 62 Half-value width of the grid size distribution curve nm 150 171

根據表3,可瞭解藉由實施例17之製造方法獲得之凝膠的網格尺寸分佈曲線之半值寬較小,與藉由實施例18之製造方法獲得之凝膠相比,凝膠之網格尺寸之均勻性提昇。即,可知藉由對將聚合物(A)及溶劑(B)加以混合而獲得之凝膠狀物進行混練,可提昇所獲得之凝膠之網格尺寸之均勻性。According to Table 3, it can be seen that the half-value width of the mesh size distribution curve of the gel obtained by the manufacturing method of Example 17 is smaller, and the uniformity of the mesh size of the gel is improved compared with the gel obtained by the manufacturing method of Example 18. That is, it can be seen that by kneading the gel-like material obtained by mixing the polymer (A) and the solvent (B), the uniformity of the mesh size of the obtained gel can be improved.

實施例19 首先,將作為聚合物(A)之羥丙基纖維素0.5 g、作為溶劑(B)之乙二醇50 g、及作為粒子(C)之銅粒子20 mg充分地混合而獲得混合物。一面攪拌所獲得之混合物,一面於50℃下加熱2分鐘。藉此,混合物變成凝膠。 加熱停止後,將所獲得之凝膠靜置至室溫(23℃)。然後,將處於室溫之凝膠50 g通過三輥輥磨機(AIMEX公司製造之BR-150V)4次,獲得銅粒子分散凝膠。此處,將三輥輥磨機之第一輥~第三輥之通過設為1次。各輥使用直徑為63.5 mm者,輥間之距離設為10 μm。又,設為第一輥之轉速:第二輥之轉速:第三輥之轉速=1.0:2.4:6.0,將第三輥之轉速設為80 rpm。對所獲得之銅粒子分散凝膠進行銅粒子之分散性評價。結果,銅粒子於凝膠中均勻地分散,銅粒子之分散性良好(凝膠整體變成紅褐色)。 Example 19 First, 0.5 g of hydroxypropyl cellulose as a polymer (A), 50 g of ethylene glycol as a solvent (B), and 20 mg of copper particles as particles (C) are fully mixed to obtain a mixture. The obtained mixture is heated at 50°C for 2 minutes while being stirred. Thereby, the mixture becomes a gel. After the heating is stopped, the obtained gel is allowed to stand at room temperature (23°C). Then, 50 g of the gel at room temperature is passed through a three-roll mill (BR-150V manufactured by AIMEX) 4 times to obtain a copper particle dispersed gel. Here, the passing of the first to third rolls of the three-roll mill is set to 1 time. Each roller used had a diameter of 63.5 mm, and the distance between the rollers was set to 10 μm. In addition, the rotation speed of the first roller: the rotation speed of the second roller: the rotation speed of the third roller was set to 1.0:2.4:6.0, and the rotation speed of the third roller was set to 80 rpm. The copper particle dispersion gel obtained was evaluated for the dispersibility of the copper particles. As a result, the copper particles were uniformly dispersed in the gel, and the dispersibility of the copper particles was good (the gel turned reddish brown as a whole).

實施例20 首先,將作為聚合物(A)之羥丙基纖維素0.5 g、作為溶劑(B)之乙二醇50 g、及作為粒子(C)之銅粒子20 mg充分地混合而獲得混合物。一面攪拌所獲得之混合物,一面於50℃下加熱2分鐘。藉此混合物變成凝膠。 加熱停止後,將所獲得之凝膠靜置至室溫(23℃),獲得銅粒子分散凝膠。對所獲得之銅粒子分散凝膠進行銅粒子之分散性評價。結果,銅粒子於凝膠中偏集存在,銅粒子之分散性不良(凝膠整體變成紅褐色,但色調有深有淺)。 Example 20 First, 0.5 g of hydroxypropyl cellulose as a polymer (A), 50 g of ethylene glycol as a solvent (B), and 20 mg of copper particles as particles (C) are fully mixed to obtain a mixture. The obtained mixture is heated at 50°C for 2 minutes while being stirred. The mixture is thereby turned into a gel. After the heating is stopped, the obtained gel is allowed to stand at room temperature (23°C) to obtain a copper particle dispersion gel. The copper particle dispersion gel obtained is evaluated for its dispersibility. As a result, the copper particles are concentrated in the gel, and the copper particles have poor dispersibility (the gel as a whole becomes reddish brown, but the color tone varies).

該申請案主張以於2022年8月8日提出申請之日本申請特願2022-126110號、日本申請特願2022-126111號、及日本申請特願2022-126112號為基礎之優先權,並將其揭示之全部內容併入本文中。This application claims priority based on Japanese Patent Application No. 2022-126110, Japanese Patent Application No. 2022-126111, and Japanese Patent Application No. 2022-126112 filed on August 8, 2022, and all the contents disclosed in them are incorporated herein.

本發明亦可採用以下態樣。The present invention can also adopt the following aspects.

[1a] 一種粒子分散用凝膠,其係包含聚合物(A)及溶劑(B),且可使粒子分散於內部者, 上述粒子分散用凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 上述溶劑(B)包含多元醇化合物(B1)。 [2a] 如上述[1a]所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)之分子量為50以上300以下。 [3a] 如上述[1a]或[2a]所記載之粒子分散用凝膠,其中利用B型黏度計於25℃、轉速30 rpm之條件下測得之上述溶劑(B)之黏度為1 mPa・s以上200 mPa・s以下。 [4a] 如上述[1a]至[3a]中任一項所記載之粒子分散用凝膠,其中上述溶劑(B)之沸點為180℃以上300℃以下。 [5a] 如上述[1a]至[4a]中任一項所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)包含碳數2以上6以下之二醇化合物(B2)。 [6a] 如上述[1a]至[5a]中任一項所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。 [7a] 如上述[1a]至[6a]中任一項所記載之粒子分散用凝膠,其中利用錐板黏度計於25℃、錐2°/20 mm、剪切速度15 s -1之條件下測得之上述粒子分散用凝膠之黏度為10 mPa・s以上60000 mPa・s以下。 [8a] 如上述[1a]至[7a]中任一項所記載之粒子分散用凝膠,其中藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之最頻粒徑(X 1)為10 nm以上。 [9a] 如上述[1a]至[8a]中任一項所記載之粒子分散用凝膠,其中藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之中值粒徑(X 2)為50 nm以上。 [10a] 如上述[1a]至[9a]中任一項所記載之粒子分散用凝膠,其中上述聚合物(A)包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物及聚乙烯吡咯啶酮所組成之群中之一種或兩種以上。 [11a] 如上述[1a]至[10a]中任一項所記載之粒子分散用凝膠,其中上述粒子分散用凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。 [12a] 一種粒子分散凝膠,其包含如上述[1a]至[11a]中任一項所記載之粒子分散用凝膠、及分散於上述粒子分散用凝膠中之粒子。 [13a] 如上述[12a]所記載之粒子分散凝膠,其中上述粒子包含選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑所組成之群中之一種或兩種以上。 [14a] 如上述[12a]或[13a]所記載之粒子分散凝膠,其中藉由雷射繞射散射法測得之上述粒子之中值粒徑D 50為0.01 μm以上10 μm以下。 [15a] 一種粒子分散用凝膠之製造方法,其係用以製造如上述[1a]至[11a]中任一項所記載之粒子分散用凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)及上述溶劑(B)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散用凝膠。 [1a] A particle dispersing gel comprising a polymer (A) and a solvent (B) and capable of dispersing particles therein, wherein the particle dispersing gel forms a three-dimensional network structure with the polymer (A), and the network structure contains the solvent (B), and the solvent (B) comprises a polyol compound (B1). [2a] The particle dispersing gel as described in [1a] above, wherein the molecular weight of the polyol compound (B1) is 50 to 300. [3a] The particle dispersing gel as described in [1a] or [2a] above, wherein the viscosity of the solvent (B) measured at 25°C and 30 rpm using a B-type viscometer is 1 to 200 mPa·s. [4a] The particle dispersion gel as described in any one of [1a] to [3a] above, wherein the boiling point of the solvent (B) is 180°C to 300°C. [5a] The particle dispersion gel as described in any one of [1a] to [4a] above, wherein the polyol compound (B1) comprises a diol compound (B2) having a carbon number of 2 to 6. [6a] The particle dispersion gel as described in any one of [1a] to [5a] above, wherein the polyol compound (B1) comprises one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol. [7a] The particle dispersion gel as described in any one of the above [1a] to [6a], wherein the viscosity of the particle dispersion gel measured by a cone viscometer at 25°C, cone 2°/20 mm, and shear rate 15 s -1 is 10 mPa・s or more and 60000 mPa・s or less. [8a] The particle dispersion gel as described in any one of the above [1a] to [7a], wherein the mode particle size (X 1 ) of the three-dimensional network structure measured by the photon correlation method in accordance with JIS Z 8826 is 10 nm or more. [9a] The particle dispersion gel as described in any one of [1a] to [8a] above, wherein the median particle size ( X2 ) of the three-dimensional network structure measured by the photon correlation method according to JIS Z 8826 is 50 nm or more. [10a] The particle dispersion gel as described in any one of [1a] to [9a] above, wherein the polymer (A) comprises one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic acid polymers, polyvinyl alcohol polymers and polyvinyl pyrrolidone. [11a] The particle dispersion gel as described in any one of [1a] to [10a] above, wherein the content of the polymer (A) in the particle dispersion gel is 0.01 mass % or more and 20.0 mass % or less. [12a] A particle dispersion gel comprising a particle dispersion gel as described in any one of [1a] to [11a] above, and particles dispersed in the particle dispersion gel. [13a] The particle dispersion gel as described in [12a] above, wherein the particles comprise one or more selected from the group consisting of drugs, fragrances, antibacterial agents, fungicides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents. [14a] The particle dispersion gel as described in [12a] or [13a] above, wherein the median particle size D50 of the particles measured by laser diffraction scattering is not less than 0.01 μm and not more than 10 μm. [15a] A method for producing a particle dispersion gel, which is used to produce the particle dispersion gel described in any one of [1a] to [11a] above, and comprises the following steps: obtaining a gel-like substance by mixing the polymer (A) and the solvent (B); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel-like substance.

本發明亦可採用以下態樣。The present invention can also adopt the following aspects.

[1b] 一種粒子分散用凝膠,其係包含聚合物(A)及溶劑(B),且可使粒子分散於內部者, 上述粒子分散用凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 將藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之最頻粒徑設為X 1(nm),將藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之中值粒徑設為(X 2)(nm)時,X 1/X 2為0.20以上2.0以下。 [2b] 如上述[1b]所記載之粒子分散用凝膠,其中上述溶劑(B)包含多元醇化合物(B1)。 [3b] 如上述[2b]所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)包含碳數2以上6以下之二醇化合物(B2)。 [4b] 如上述[2b]或[3b]所記載之粒子分散用凝膠,其中上述多元醇化合物(B1)包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。 [5b] 如上述[1b]至[4b]中任一項所記載之粒子分散用凝膠,其中藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之最頻粒徑(X 1)為10 nm以上。 [6b] 如上述[1b]至[5b]中任一項所記載之粒子分散用凝膠,其中藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之中值粒徑(X 2)為50 nm以上。 [7b] 如上述[1b]至[6b]中任一項所記載之粒子分散用凝膠,其中上述聚合物(A)包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物及聚乙烯吡咯啶酮所組成之群中之一種或兩種以上。 [8b] 如上述[1b]至[7b]中任一項所記載之粒子分散用凝膠,其中上述粒子分散用凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。 [9b] 一種粒子分散凝膠,其包含如上述[1b]至[8b]中任一項所記載之粒子分散用凝膠、及分散於上述粒子分散用凝膠中之粒子。 [10b] 如上述[9b]所記載之粒子分散凝膠,其中上述粒子包含選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑所組成之群中之一種或兩種以上。 [11b] 如上述[9b]或[10b]所記載之粒子分散凝膠,其中藉由雷射繞射散射法測得之上述粒子之中值粒徑D 50為0.01 μm以上10 μm以下。 [12b] 一種粒子分散用凝膠之製造方法,其係用以製造如上述[1b]至[8b]中任一項所記載之粒子分散用凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)及上述溶劑(B)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散用凝膠。 [1b] A particle dispersing gel comprising a polymer (A) and a solvent (B) and capable of dispersing particles therein, wherein the particle dispersing gel forms a three-dimensional network structure with the polymer (A), and the network structure contains the solvent (B), and when the mode particle size of the three-dimensional network structure measured by the photon correlation method in accordance with JIS Z 8826 is X1 (nm), and when the median particle size of the three-dimensional network structure measured by the photon correlation method in accordance with JIS Z 8826 is ( X2 ) (nm), X1 / X2 is 0.20 or more and 2.0 or less. [2b] The particle dispersing gel as described in [1b] above, wherein the solvent (B) comprises a polyol compound (B1). [3b] The particle dispersion gel as described in [2b] above, wherein the polyol compound (B1) comprises a diol compound (B2) having a carbon number of 2 or more and 6 or less. [4b] The particle dispersion gel as described in [2b] or [3b] above, wherein the polyol compound (B1) comprises one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol. [5b] The particle dispersion gel as described in any one of [1b] to [4b] above, wherein the maximum frequency particle size ( X1 ) of the stereo network structure measured by the photon correlation method in accordance with JIS Z 8826 is 10 nm or more. [6b] The particle dispersion gel as described in any one of [1b] to [5b] above, wherein the median particle size ( X2 ) of the three-dimensional network structure measured by the photon correlation method according to JIS Z 8826 is 50 nm or more. [7b] The particle dispersion gel as described in any one of [1b] to [6b] above, wherein the polymer (A) comprises one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic acid polymers, polyvinyl alcohol polymers and polyvinyl pyrrolidone. [8b] The particle dispersion gel as described in any one of [1b] to [7b] above, wherein the content of the polymer (A) in the particle dispersion gel is 0.01 mass % or more and 20.0 mass % or less. [9b] A particle dispersion gel comprising a particle dispersion gel as described in any one of [1b] to [8b] above, and particles dispersed in the particle dispersion gel. [10b] The particle dispersion gel as described in [9b] above, wherein the particles comprise one or more selected from the group consisting of drugs, fragrances, antibacterial agents, fungicides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents. [11b] The particle dispersion gel as described in [9b] or [10b] above, wherein the median particle size D50 of the particles measured by laser diffraction scattering is not less than 0.01 μm and not more than 10 μm. [12b] A method for producing a particle dispersion gel, which is used to produce the particle dispersion gel described in any one of [1b] to [8b] above, and comprises the following steps: obtaining a gel-like substance by mixing the polymer (A) and the solvent (B); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel-like substance.

本發明亦可採用以下態樣。The present invention can also adopt the following aspects.

[1c] 一種凝膠之製造方法,其係用以製造包含聚合物(A)及溶劑(B)且具有立體網狀結構之凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)及上述溶劑(B)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之凝膠。 [2c] 如上述[1c]所記載之凝膠之製造方法,其中上述凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B)。 [3c] 如上述[1c]或[2c]所記載之凝膠之製造方法,其中於對上述凝膠狀物進行混練之步驟中,使用輥磨機對上述凝膠狀物進行混練。 [4c] 如上述[1c]至[3c]中任一項所記載之凝膠之製造方法,其中上述溶劑(B)包含多元醇化合物(B1)。 [5c] 如上述[4c]所記載之凝膠之製造方法,其中上述多元醇化合物(B1)包含碳數2以上6以下之二醇化合物(B2)。 [6c] 如上述[4c]或[5c]所記載之凝膠之製造方法,其中上述多元醇化合物(B1)包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。 [7c] 如上述[1c]至[6c]中任一項所記載之凝膠之製造方法,其中藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之最頻粒徑(X 1)為10 nm以上。 [8c] 如上述[1c]至[7c]中任一項所記載之凝膠之製造方法,其中藉由依據JIS Z 8826之光子相關法所測得之上述立體網狀結構之中值粒徑(X 2)為50 nm以上。 [9c] 如上述[1c]至[8c]中任一項所記載之凝膠之製造方法,其中上述聚合物(A)包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物及聚乙烯吡咯啶酮所組成之群中之一種或兩種以上。 [10c] 如上述[1c]至[9c]中任一項所記載之凝膠之製造方法,其中上述凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。 [11c] 一種粒子分散凝膠之製造方法,其係用以製造包含聚合物(A)、溶劑(B)及粒子(C)且具有立體網狀結構之粒子分散凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)、上述溶劑(B)及上述粒子(C)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散凝膠。 [12c] 如上述[11c]所記載之粒子分散凝膠之製造方法,其中上述粒子分散凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 上述粒子(C)內包於上述網狀結構內。 [13c] 如上述[11c]或[12c]所記載之粒子分散凝膠之製造方法,其中於對上述凝膠狀物進行混練之步驟中,使用輥磨機對上述凝膠狀物進行混練。 [14c] 如上述[11c]至[13c]中任一項所記載之粒子分散凝膠之製造方法,其中上述溶劑(B)包含多元醇化合物(B1)。 [15c] 如上述[14c]所記載之粒子分散凝膠之製造方法,其中上述多元醇化合物(B1)包含碳數2以上6以下之二醇化合物(B2)。 [16c] 如上述[14c]或[15c]所記載之粒子分散凝膠之製造方法,其中上述多元醇化合物(B1)包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。 [17c] 如上述[11c]至[16c]中任一項所記載之粒子分散凝膠之製造方法,其中上述聚合物(A)包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物及聚乙烯吡咯啶酮所組成之群中之一種或兩種以上。 [18c] 如上述[11c]至[17c]中任一項所記載之粒子分散凝膠之製造方法,其中上述粒子分散凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。 [19c] 如上述[11c]至[18c]中任一項所記載之粒子分散凝膠之製造方法,其中上述粒子(C)包含選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑所組成之群中之一種或兩種以上。 [20c] 如上述[11c]至[19c]中任一項所記載之粒子分散凝膠之製造方法,其中藉由雷射繞射散射法測得之上述粒子(C)之中值粒徑D 50為0.01 μm以上10 μm以下。 [1c] A method for producing a gel, which is a method for producing a gel having a three-dimensional network structure and comprising the following steps: obtaining a gel-like substance by mixing the polymer (A) and the solvent (B); and obtaining a gel having a three-dimensional network structure by kneading the gel-like substance. [2c] A method for producing a gel as described in [1c] above, wherein the gel forms a three-dimensional network structure by the polymer (A), and the solvent (B) is contained in the network structure. [3c] The method for producing a gel as described in [1c] or [2c] above, wherein in the step of kneading the gel-like material, the gel-like material is kneaded using a roll mill. [4c] The method for producing a gel as described in any one of [1c] to [3c] above, wherein the solvent (B) contains a polyol compound (B1). [5c] The method for producing a gel as described in [4c] above, wherein the polyol compound (B1) contains a diol compound (B2) having a carbon number of 2 or more and 6 or less. [6c] The method for producing a gel as described in [4c] or [5c] above, wherein the polyol compound (B1) contains one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol. [7c] The method for producing a gel as described in any one of [1c] to [6c] above, wherein the mode particle size (X 1 ) of the stereo network structure measured by the photon correlation method according to JIS Z 8826 is 10 nm or more. [8c] The method for producing a gel as described in any one of [1c] to [7c] above, wherein the median particle size (X 2 ) of the stereo network structure measured by the photon correlation method according to JIS Z 8826 is 50 nm or more. [9c] The method for producing a gel as described in any one of [1c] to [8c] above, wherein the polymer (A) comprises one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic acid polymers, polyvinyl alcohol polymers and polyvinyl pyrrolidone. [10c] A method for producing a gel as described in any one of [1c] to [9c] above, wherein the content of the polymer (A) in the gel is not less than 0.01 mass % and not more than 20.0 mass %. [11c] A method for producing a particle-dispersed gel, which is a method for producing a particle-dispersed gel having a three-dimensional network structure and comprises the following steps: obtaining a gel-like substance by mixing the polymer (A), the solvent (B) and the particles (C); and obtaining a particle-dispersed gel having a three-dimensional network structure by kneading the gel-like substance. [12c] A method for producing a particle-dispersed gel as described in [11c] above, wherein the particle-dispersed gel forms a three-dimensional network structure by the polymer (A), and the solvent (B) is contained in the network structure, and the particles (C) are enclosed in the network structure. [13c] A method for producing a particle-dispersed gel as described in [11c] or [12c] above, wherein in the step of kneading the gel-like substance, a roller mill is used to knead the gel-like substance. [14c] A method for producing a particle-dispersed gel as described in any one of [11c] to [13c] above, wherein the solvent (B) contains a polyol compound (B1). [15c] The method for producing a particle dispersion gel as described in [14c] above, wherein the polyol compound (B1) comprises a diol compound (B2) having a carbon number of 2 or more and 6 or less. [16c] The method for producing a particle dispersion gel as described in [14c] or [15c] above, wherein the polyol compound (B1) comprises one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butylene glycol, 1,5-pentanediol and 1,6-hexanediol. [17c] The method for producing a particle dispersion gel as described in any one of [11c] to [16c] above, wherein the polymer (A) comprises one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic acid polymers, polyvinyl alcohol polymers and polyvinyl pyrrolidone. [18c] A method for producing a particle dispersion gel as described in any one of [11c] to [17c] above, wherein the content of the polymer (A) in the particle dispersion gel is 0.01 mass % to 20.0 mass %. [19c] A method for producing a particle dispersion gel as described in any one of [11c] to [18c] above, wherein the particles (C) comprise one or more selected from the group consisting of drugs, fragrances, antibacterial agents, fungicides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents. [20c] A method for producing a particle dispersion gel as described in any one of [11c] to [19c] above, wherein the median particle size D50 of the above particles (C) measured by laser diffraction scattering method is not less than 0.01 μm and not more than 10 μm.

Claims (21)

一種粒子分散用凝膠,其係包含聚合物(A)及溶劑(B),且可使粒子分散於內部者, 上述粒子分散用凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 上述溶劑(B)包含多元醇化合物(B1)。 A particle dispersing gel, which comprises a polymer (A) and a solvent (B) and can disperse particles inside. The particle dispersing gel forms a three-dimensional network structure by the polymer (A), and the network structure contains the solvent (B). The solvent (B) comprises a polyol compound (B1). 如請求項1之粒子分散用凝膠,其中上述多元醇化合物(B1)之分子量為50以上300以下。The particle dispersion gel of claim 1, wherein the molecular weight of the polyol compound (B1) is 50 to 300. 如請求項1或2之粒子分散用凝膠,其中利用B型黏度計於25℃、轉速30 rpm之條件下測得之上述溶劑(B)之黏度為1 mPa・s以上200 mPa・s以下。The particle dispersion gel of claim 1 or 2, wherein the viscosity of the solvent (B) measured by a B-type viscometer at 25°C and a rotation speed of 30 rpm is 1 mPa・s or more and 200 mPa・s or less. 如請求項1或2之粒子分散用凝膠,其中上述溶劑(B)之沸點為180℃以上300℃以下。The particle dispersion gel of claim 1 or 2, wherein the boiling point of the solvent (B) is not less than 180°C and not more than 300°C. 如請求項1或2之粒子分散用凝膠,其中上述多元醇化合物(B1)包含碳數2以上6以下之二醇化合物(B2)。The particle dispersion gel of claim 1 or 2, wherein the polyol compound (B1) comprises a diol compound (B2) having a carbon number of 2 to 6. 如請求項1或2之粒子分散用凝膠,其中上述多元醇化合物(B1)包含選自由乙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇及1,6-己二醇所組成之群中之一種或兩種以上。The particle dispersion gel of claim 1 or 2, wherein the polyol compound (B1) comprises one or more selected from the group consisting of ethylene glycol, 1,3-propylene glycol, 1,4-butanediol, 1,5-pentanediol and 1,6-hexanediol. 如請求項1或2之粒子分散用凝膠,其中利用錐板黏度計於25℃、錐2°/20 mm、剪切速度15 s -1之條件下測得之上述粒子分散用凝膠之黏度為10 mPa・s以上60000 mPa・s以下。 The particle dispersion gel of claim 1 or 2, wherein the viscosity of the particle dispersion gel measured by a cone plate viscometer at 25°C, cone 2°/20 mm, and shear rate 15 s -1 is not less than 10 mPa・s and not more than 60000 mPa・s. 如請求項1或2之粒子分散用凝膠,其中將藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之最頻粒徑設為X 1(nm),將藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之中值粒徑設為(X 2)(nm)時,X 1/X 2為0.20以上2.0以下。 In the particle dispersion gel of claim 1 or 2, when the mode particle size of the stereo-network structure measured by the photon correlation method in accordance with JIS Z 8826:2019 is X 1 (nm), and the median particle size of the stereo-network structure measured by the photon correlation method in accordance with JIS Z 8826:2019 is (X 2 ) (nm), X 1 /X 2 is 0.20 or more and 2.0 or less. 如請求項1或2之粒子分散用凝膠,其中藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之最頻粒徑(X 1)為10 nm以上。 The particle dispersion gel of claim 1 or 2, wherein the mode particle size (X 1 ) of the three-dimensional network structure measured by a photon correlation method according to JIS Z 8826:2019 is 10 nm or more. 如請求項1或2之粒子分散用凝膠,其中藉由依據JIS Z 8826:2019之光子相關法所測得之上述立體網狀結構之中值粒徑(X 2)為50 nm以上。 The particle dispersion gel of claim 1 or 2, wherein the median particle size (X 2 ) of the three-dimensional network structure measured by a photon correlation method according to JIS Z 8826:2019 is 50 nm or more. 如請求項1或2之粒子分散用凝膠,其中上述聚合物(A)包含選自由多糖類、蛋白質、肽、(甲基)丙烯酸系聚合物、聚乙烯醇系聚合物及聚乙烯吡咯啶酮所組成之群中之一種或兩種以上。The particle dispersion gel of claim 1 or 2, wherein the polymer (A) comprises one or more selected from the group consisting of polysaccharides, proteins, peptides, (meth)acrylic acid polymers, polyvinyl alcohol polymers and polyvinyl pyrrolidone. 如請求項1或2之粒子分散用凝膠,其中上述粒子分散用凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。The particle dispersion gel of claim 1 or 2, wherein the content of the polymer (A) in the particle dispersion gel is 0.01 mass % to 20.0 mass %. 一種粒子分散凝膠,其包含如請求項1至12中任一項之粒子分散用凝膠、及分散於上述粒子分散用凝膠中之粒子(C)。A particle dispersion gel comprising the particle dispersion gel according to any one of claims 1 to 12, and particles (C) dispersed in the particle dispersion gel. 如請求項13之粒子分散凝膠,其中上述粒子(C)包含選自由藥物、香料、抗菌劑、殺菌劑、細胞、金屬粒子、無機物粒子、聚合物粒子、觸媒、抗病毒劑及防黴劑所組成之群中之一種或兩種以上。The particle dispersion gel of claim 13, wherein the particles (C) comprise one or more selected from the group consisting of drugs, fragrances, antibacterial agents, fungicides, cells, metal particles, inorganic particles, polymer particles, catalysts, antiviral agents and antifungal agents. 如請求項13或14之粒子分散凝膠,其中藉由雷射繞射散射法測得之上述粒子(C)之中值粒徑D 50為0.01 μm以上10 μm以下。 The particle dispersion gel of claim 13 or 14, wherein the median particle size D50 of the above-mentioned particles (C) measured by laser diffraction scattering method is not less than 0.01 μm and not more than 10 μm. 一種粒子分散用凝膠之製造方法,其係用以製造如請求項1至12中任一項之粒子分散用凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)及上述溶劑(B)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散用凝膠。 A method for producing a particle dispersion gel, which is used to produce a particle dispersion gel as claimed in any one of claims 1 to 12, and comprises the following steps: obtaining a gel by mixing the polymer (A) and the solvent (B); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel. 如請求項16之粒子分散用凝膠之製造方法,其中於對上述凝膠狀物進行混練之步驟中,使用輥磨機對上述凝膠狀物進行混練。A method for producing a gel for particle dispersion as claimed in claim 16, wherein in the step of kneading the gel-like material, a roller mill is used to knead the gel-like material. 一種粒子分散凝膠之製造方法,其係用以製造如請求項13至15中任一項之粒子分散凝膠之製造方法,且 包括如下步驟:藉由將上述聚合物(A)、上述溶劑(B)及上述粒子(C)加以混合而獲得凝膠狀物;及藉由對上述凝膠狀物進行混練,而獲得具有立體網狀結構之粒子分散凝膠。 A method for producing a particle dispersion gel, which is used to produce a particle dispersion gel as described in any one of claims 13 to 15, and includes the following steps: obtaining a gel by mixing the polymer (A), the solvent (B) and the particles (C); and obtaining a particle dispersion gel having a three-dimensional network structure by kneading the gel. 如請求項18之粒子分散凝膠之製造方法,其中上述粒子分散凝膠藉由上述聚合物(A)形成立體網狀結構,且於上述網狀結構內含有上述溶劑(B), 上述粒子(C)內包於上述網狀結構內。 A method for manufacturing a particle dispersion gel as claimed in claim 18, wherein the particle dispersion gel forms a three-dimensional network structure by the polymer (A), and the network structure contains the solvent (B), and the particles (C) are contained in the network structure. 如請求項18或19之粒子分散凝膠之製造方法,其中於對上述凝膠狀物進行混練之步驟中,使用輥磨機對上述凝膠狀物進行混練。A method for producing a particle-dispersed gel as claimed in claim 18 or 19, wherein in the step of kneading the gel-like substance, a roller mill is used to knead the gel-like substance. 如請求項18或19之粒子分散凝膠之製造方法,其中上述粒子分散凝膠中之上述聚合物(A)之含量為0.01質量%以上20.0質量%以下。A method for producing a particle dispersion gel as claimed in claim 18 or 19, wherein the content of the polymer (A) in the particle dispersion gel is greater than 0.01 mass % and less than 20.0 mass %.
TW112129726A 2022-08-08 2023-08-08 Gel for particle dispersion, particle dispersion gel, method for producing gel for particle dispersion and method for producing particle dispersion gel TW202412631A (en)

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