TWI391175B - Oil in water emulsion composition and method for manufacturing thereof - Google Patents

Oil in water emulsion composition and method for manufacturing thereof Download PDF

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TWI391175B
TWI391175B TW095105185A TW95105185A TWI391175B TW I391175 B TWI391175 B TW I391175B TW 095105185 A TW095105185 A TW 095105185A TW 95105185 A TW95105185 A TW 95105185A TW I391175 B TWI391175 B TW I391175B
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water
emulsion composition
oil
composition
viscosity
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TW200633755A (en
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Yuji Sonoda
Toshio Ishida
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Kurita Water Ind Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

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Description

水中油性乳膠組成物及其製造方法Oily emulsion composition in water and preparation method thereof

本發明是有關於一種水中油性乳膠組成物之技術,且特別是有關於一種不添加乳化劑之新穎的水中油性乳膠組成物與該組成物之製造方法。BACKGROUND OF THE INVENTION 1. Field of the Invention This invention relates to a technique for oily emulsion compositions in water, and more particularly to a novel aqueous oil emulsion composition without the addition of an emulsifier and a method of making the composition.

如今,水中油性(oil in water)乳膠組成物,於抄紙步驟等各種製造步驟、工作步驟,或是於排水處理步驟中作為發泡抑制劑(消泡劑)等而被廣泛應用。通常,此種組成物是於油相成分中添加乳化劑與水,並使油相成分分散於水中而構成。Nowadays, an oil in water latex composition is widely used as a foaming inhibitor (antifoaming agent) in various manufacturing steps, work steps, and the like in a papermaking step. Usually, such a composition is composed by adding an emulsifier and water to an oil phase component, and dispersing an oil phase component in water.

已知,於水中油性乳膠組成物所構成之消泡劑中,能顯示出良好效果的消泡劑為含有高級醇(higher alcohol)成分之組成物(例如參照日本專利文獻1)。但是,由於此種消泡劑於儲存中會急劇增加黏性而固化成乳油(cream)狀,故而其操作性惡化。因此,以高級醇為基礎之水中油性乳膠組成物,大多是用於高黏度且處於穩定態(乳油、凝膠等)之產品。It is known that an antifoaming agent which exhibits a good effect in an antifoaming agent composed of an oily latex composition in water is a composition containing a higher alcohol component (for example, refer to Japanese Patent Laid-Open Publication No. Hei. However, since such an antifoaming agent is sharply increased in viscosity during storage and solidified into a creamy shape, its workability is deteriorated. Therefore, the oil-based emulsion composition based on higher alcohols is mostly used for products having high viscosity and being in a stable state (emulsification, gel, etc.).

此種包含高級醇的水中油性乳膠,於作為連續相之水相中會生成結晶液體或凝膠而增大黏度,以使系統實現穩定化(參照非日本專利文獻1)。可推測包含高級醇之水中油性乳膠的消泡劑於儲存中所產生之黏度增大的現象,是由於生成此種結晶液體或凝膠的緣故。Such an oil-in-water emulsion containing a higher alcohol forms a crystal liquid or a gel in an aqueous phase as a continuous phase to increase the viscosity to stabilize the system (see Non-Japanese Patent Publication 1). It is presumed that the phenomenon that the viscosity of the defoaming agent containing the oily emulsion of the higher alcohol in the storage increases during storage is due to the formation of such a crystal liquid or gel.

可藉由對與高級醇組合之油劑、乳化劑、其他調配劑進行鑽研,而能夠於某種程度上避免此黏度增大現象。例如,於日本專利文獻2中所揭示的,以水中油性乳膠為基礎,油相為由高級醇、糖醇(sugar alcohol)、酯(ester)、石蠟(wax)等混合物所組成之消泡劑。但是,由如此複雜之調配成分所組成之消泡劑,由於其調配上的限制而難以成為通用產品。The viscosity increase can be avoided to some extent by studying oil agents, emulsifiers, and other formulating agents combined with higher alcohols. For example, as disclosed in Japanese Patent Document 2, the oil phase is an antifoaming agent composed of a mixture of a higher alcohol, a sugar alcohol, an ester, a wax, and the like, based on an oily emulsion in water. . However, an antifoaming agent composed of such a complicated compounding component is difficult to be a general-purpose product due to limitations in blending.

日本專利文獻1:特開昭48-62683號公報日本專利文獻2:特開08-257305號公報非日本專利文獻1:乳化/分散技術應用手冊、科學論壇發行(1987年),第131頁Japanese Patent Publication No. JP-A-48-62683A Japanese Patent Publication No. Hei 08-257305 (Non-Japanese Patent Publication No. JP-A No. JP-A No. 08-257305)

通常,會要求液體產品在儲存中具有穩定的物理性質(如黏度)、可迅速從儲存容器中取出,以及使用簡便的注藥幫浦即可以獲得穩定之排出量等操作性質。即使對於以高級醇為基礎之水中油性乳膠消泡劑,亦要求其具有作為液體產品之產品穩定性,而且期望其不受到調配方面之限制,並能夠長期保存。In general, liquid products are required to have stable physical properties (such as viscosity) during storage, can be quickly removed from the storage container, and the use of a simple injection pump can achieve stable operational properties such as discharge. Even in the case of a higher alcohol-based aqueous oil emulsion defoamer, it is required to have product stability as a liquid product, and it is expected that it is not limited by the formulation and can be stored for a long period of time.

因此,本發明主要目的在於提供一種不受調配之限制、儲存中不發生黏度增大、固化等現象,進而具有良好之保存穩定性的水中油性乳膠消泡劑組成物。Accordingly, it is a primary object of the present invention to provide an oil-in-water emulsion defoamer composition which is not restricted by the formulation, does not cause an increase in viscosity during storage, cures, and the like, and further has good storage stability.

本發明提供一種能夠達成上述目的之水中油性乳膠組成物以及該組成物之適當的製造方法。The present invention provides an oil-in-water emulsion composition capable of achieving the above object and an appropriate production method of the composition.

基於上述目的或其他目的,本發明提供一種水中油性乳膠組成物,包括:油相成分,其包含碳原子數為12~30之高級醇;以及難溶於水之親水性無機微粒子。其中,前述油相成分之微粒子是被前述親水性無機微粒子包覆之狀態而分散在水中。於本組成物中,前述難溶於水之親水性無機微粒子能夠發揮與乳化劑同樣之功能,使油相成分乳膠化。亦即,本發明能夠提供一種不使用一切乳化劑之水中油性乳膠組成物。Based on the above object or other objects, the present invention provides an oil-in-water emulsion composition comprising: an oil phase component comprising a higher alcohol having 12 to 30 carbon atoms; and a hydrophilic inorganic microparticle having poor water solubility. The fine particles of the oil phase component are dispersed in water in a state of being coated with the hydrophilic inorganic fine particles. In the present composition, the hydrophilic inorganic fine particles which are hardly soluble in water can exhibit the same function as the emulsifier, and the oil phase component can be made into a latex. That is, the present invention can provide an oil-in-water emulsion composition which does not use all emulsifiers.

又,在本發明之一實施例中,難溶於水之前述親水性無機微粒子的平均粒子直徑小於1μm,或是將碳酸鈣作為前述親水性無機微粒子。Further, in an embodiment of the present invention, the hydrophilic inorganic fine particles which are hardly soluble in water have an average particle diameter of less than 1 μm or calcium carbonate as the hydrophilic inorganic fine particles.

基於上述目的或其他目的,本發明再提出一種水中油性乳膠組成物之製造方法,至少分2個步驟進行。首先第第1步驟為,將包含碳原子數為12~30之高級醇的油相成分與難溶於水的親水性無機微粒子之混合物進行加熱熔融,且藉由邊攪拌邊添加熱水而獲得凝膠狀混合物;以及,第2步驟為,進一步將熱水加入前述凝膠狀混合物,並進行攪拌。Based on the above object or other objects, the present invention further provides a method for producing an oily emulsion composition in water, which is carried out in at least two steps. First, in the first step, a mixture of an oil phase component containing a higher alcohol having 12 to 30 carbon atoms and a hydrophilic inorganic fine particle which is poorly soluble in water is heated and melted, and a hot water is added while stirring. The gelatinous mixture; and, in the second step, further adding hot water to the gelatinous mixture and stirring.

在本發明之一較佳實施例中,藉由在前述第一步驟後便停止攪拌,即使不進行如間歇攪拌之麻煩步驟,油相與水相亦不分離,而可通過凝膠狀態導入均勻分散系統,使黏度降低。In a preferred embodiment of the present invention, the stirring is stopped after the first step, and even if the troublesome step such as intermittent stirring is not performed, the oil phase and the aqueous phase are not separated, and the gel state can be uniformly introduced. Disperse the system to reduce viscosity.

本發明之水中油性乳膠組成物,其分散狀態是,油相成分之微粒子被親水性無機微粒子包覆而形成穩定之雙重結構。因此,處理液之起泡抑制效果良好,並且於產品保存中不發生黏度增大變化,所以隨時間經過的穩定性良好。即,由於本組成物中未添加乳化劑,故而可抑制由於形成結晶液體所引起之隨時間經過的黏度增加。The oil-in-water emulsion composition of the present invention has a dispersed state in which fine particles of an oil phase component are coated with hydrophilic inorganic fine particles to form a stable double structure. Therefore, the foaming suppression effect of the treatment liquid is good, and the viscosity increase change does not occur during product storage, so the stability over time is good. That is, since no emulsifier is added to the composition, the increase in viscosity over time due to the formation of the crystallization liquid can be suppressed.

又,無需添加乳化劑,且替代其發揮乳化作用之難溶於水之親水性無機微粒子價格低廉,所以可達成組成物藥劑之低成本化。Further, since it is not necessary to add an emulsifier, and the water-insoluble hydrophilic inorganic fine particles which exhibit an emulsification effect are inexpensive, the cost of the composition can be reduced.

為讓本發明之上述和其他目的、特徵和優點能更明顯易懂,下文特舉較佳實施例,並配合所附圖式,作詳細說明如下。The above and other objects, features and advantages of the present invention will become more <RTIgt;

以下就本發明之較佳實施方式進行說明。另外,以下所說明之實施方式,是表示本發明的較佳實施例。利用這些實施方式以說明本發明的實施例,然而並非用以狹義地限定本發明。Hereinafter, preferred embodiments of the present invention will be described. Further, the embodiments described below are preferred embodiments of the present invention. The embodiments are described to illustrate embodiments of the invention, but are not intended to limit the invention.

首先,作為本發明之水中油性乳膠組成物的較佳實施方式,水中油性乳膠組成物包括:油相成分,含有碳原子數為12~30之高級醇,以及難溶於水之親水性無機微粒子。First, as a preferred embodiment of the oil-in-water emulsion composition of the present invention, the oil-in-water emulsion composition includes an oil phase component, a higher alcohol having 12 to 30 carbon atoms, and a hydrophilic inorganic fine particle which is insoluble in water. .

此組成物中,難溶於水之親水性無機微粒子可發揮與乳化劑同樣之作用,使含有碳原子數為12~30之高級醇的油相成分乳膠化,故而完全不需向本組成物中添加乳化劑。In the composition, the hydrophilic inorganic fine particles which are hardly soluble in water exert the same function as the emulsifier, and the oil phase component containing the higher alcohol having 12 to 30 carbon atoms is gelled, so that it is not required to be present in the composition. Add emulsifier to it.

本實施方式之組成物中,較佳的是,含有碳原子數為12~30之高級醇(高級脂肪族醇)的油相成分的佔有量,其小於等於整個組成物的50wt%。藉由使含有碳原子數為12~30之高級脂肪族醇的油相成分之佔有量,其小於等於50wt%,可使所獲得之水中油性乳膠組成物保持更低之黏度,其結果是可以顯著提高操作性。另外,於本組成物中,對於油相成分中之碳原子數為12~30之高級脂肪族醇的佔有量並無特別限制,較佳的是其為40~85 wt%。In the composition of the present embodiment, it is preferred that the amount of the oil phase component containing a higher alcohol (higher aliphatic alcohol) having 12 to 30 carbon atoms is less than or equal to 50% by weight of the entire composition. By making the oil phase component containing a higher aliphatic alcohol having 12 to 30 carbon atoms less than or equal to 50% by weight, the obtained oily latex composition can be kept at a lower viscosity, and as a result, Significantly improved operability. Further, in the present composition, the amount of the higher aliphatic alcohol having 12 to 30 carbon atoms in the oil phase component is not particularly limited, and it is preferably 40 to 85 wt%.

此處,作為本組成物中所採用之碳原子數為12~30之高級醇,例如為:十二醇(lauryl alcohol)、十四醯醇(myristyl alcohol)、十六醇(cetyl alcohol)、十八醇(stearyl alcohol)、油醇(oleyl alcohol)、二十醇(eicosyl alcohol)、二十二醇(behenyl alcohol)、二十四醇(tetracosyl alcohol)、二十六碳醇(ceryl alcohol)、三十醇(melissyl alcohol)等。這些高級醇,無論哪一種皆可單獨使用,或者使用兩種或兩種以上的組成。Here, as the higher alcohol having 12 to 30 carbon atoms used in the present composition, for example, lauryl alcohol, myristyl alcohol, cetyl alcohol, Stearyl alcohol, oleyl alcohol, eicosyl alcohol, behenyl alcohol, tetracosyl alcohol, ceryl alcohol , melissyl alcohol, and the like. Any of these higher alcohols may be used singly or in combination of two or more.

又,作為高級醇,可使用來自於天然植物油脂的醇,或者亦可使用合成醇。再者,也能夠使用合成醇之粗精製物。另外,在將本組成物作為消泡劑使用之情形下,基於確保其具有充分的消泡性之觀點,使用碳原子散為16~24之高級醇為較佳。Further, as the higher alcohol, an alcohol derived from natural vegetable oils and fats may be used, or a synthetic alcohol may also be used. Further, a crude refined product of synthetic alcohol can also be used. Further, in the case where the composition is used as an antifoaming agent, it is preferred to use a higher alcohol having a carbon atom dispersion of 16 to 24 from the viewpoint of ensuring sufficient defoaming property.

作為油相成分中高級醇以外的成分,其例如是:碳原子數為1~22的1~3價之醇與碳原子數為12~22的脂肪酸酯、礦物油以及石蠟(parafin wax)等之碳化氫等。另外,對於油相成分中之高級醇以外之成分的佔有量並無特別限制,但較佳的是其為15~60 wt%。The component other than the higher alcohol in the oil phase component is, for example, a 1-3 valent alcohol having 1 to 22 carbon atoms, a fatty acid ester having 12 to 22 carbon atoms, mineral oil, and parafin wax. Such as hydrocarbons. Further, the amount of the component other than the higher alcohol in the oil phase component is not particularly limited, but it is preferably 15 to 60% by weight.

其次,本組成物所採用之“難溶於水之親水性無機微粒子”,例如為:碳酸鈣(calcium carbonate)、高嶺土(kaolin)、滑石(talc)、氫氧化鋁(aluminum hydroxide)、氧化鈦(titanium oxide)、氧化鋁(aluminum oxide)等。選擇哪種親水性無機微粒子,例如,可考慮本組成物之處理液中預先存在之無機微粒子的種類而決定。Next, the "water-insoluble hydrophilic inorganic fine particles" used in the composition are, for example, calcium carbonate, kaolin, talc, aluminum hydroxide, titanium oxide. (titanium oxide), aluminum oxide (aluminum oxide), and the like. Which hydrophilic inorganic fine particles are selected, for example, can be determined in consideration of the type of inorganic fine particles preliminarily present in the treatment liquid of the composition.

較好的是,此親水性無機微粒子之含有量,佔組成物重量的5~20 wt%。藉由在系統內確保形成保護膜之微粒子具有充分的量,而可使乳膠粒子變小。Preferably, the content of the hydrophilic inorganic fine particles is 5 to 20% by weight based on the weight of the composition. The latex particles can be made smaller by ensuring that the fine particles forming the protective film have a sufficient amount in the system.

又,主要是基於使乳膠粒子變得更小之觀點,前述親水性無機微粒子是採用平均粒子直徑小於1μm者為較佳。再者,基於有效防止親水性無機微粒子沈澱之觀點,較好的是,使平均粒子直徑小於1μm之難溶於水的親水性無機微粒子的含有量,其小於等於整個組成物重量的10 wt%。Further, it is mainly based on the viewpoint that the latex particles are made smaller, and the hydrophilic inorganic fine particles are preferably those having an average particle diameter of less than 1 μm. Further, from the viewpoint of effectively preventing precipitation of hydrophilic inorganic fine particles, it is preferred that the content of the poorly water-soluble hydrophilic inorganic fine particles having an average particle diameter of less than 1 μm is less than or equal to 10 wt% of the entire composition. .

於本實施方式之組成物中,難溶於水之親水性無機微粒子亦可與疏水性無機微粒子或不溶性有機微粒子組合使用。於此情形下,疏水性無機微粒子或不溶性有機微粒子被乳膠微粒子積極地捕獲,故而其不展現保護膜之功能。In the composition of the present embodiment, the hydrophilic inorganic fine particles which are hardly soluble in water may be used in combination with the hydrophobic inorganic fine particles or the insoluble organic fine particles. In this case, the hydrophobic inorganic fine particles or the insoluble organic fine particles are actively captured by the latex fine particles, so that they do not exhibit the function of the protective film.

另外,於本實施方式之組成物中,根據需要可使其含有增黏劑。作為此增黏劑可採用高分子多醣類、合成高分子化合物等。藉由使其含有增黏劑,可抑制組成物之相分離而實現穩定化。Further, the composition of the present embodiment may contain a tackifier as needed. As the tackifier, a polymer polysaccharide, a synthetic polymer compound, or the like can be used. By including a tackifier, it is possible to suppress phase separation of the composition and achieve stabilization.

本實施方式之組成物之用途無特別限定,但於抄紙、塗刷等造紙步驟等各種生產步驟、工作步驟、活性污泥或排放等各種排水處理步驟等,特別是發泡成為問題之所有步驟,都可作為發泡抑制劑來使用。The use of the composition of the present embodiment is not particularly limited, but various production steps such as papermaking steps such as papermaking and painting, work steps, various drainage treatment steps such as activated sludge or discharge, and the like, in particular, all steps of foaming become a problem. Both can be used as a foaming inhibitor.

特別在抄紙步驟等之無機微粒子即便混入亦不成問題之系統,能夠作為發泡抑制劑而恰當地適用。尤其,於抄紙步驟等中,於原料紙漿(pulp slurry)中的填料大多含有碳酸鈣,故而使用碳酸鈣作為難溶於水之親水性無機微粒子為較佳。In particular, a system in which inorganic fine particles such as a papermaking step are not problematic even if mixed therein can be suitably used as a foaming inhibitor. In particular, in the papermaking step or the like, the filler in the pulp slurry mostly contains calcium carbonate. Therefore, it is preferred to use calcium carbonate as the hydrophilic inorganic fine particles which are hardly soluble in water.

本實施方式中組成物之添加量無特別限制,但通常較好的是對於處理液添加0.1~1000 mg/L,而特別更佳的是添加1~100 mg/L。The amount of the composition to be added in the present embodiment is not particularly limited, but it is usually preferred to add 0.1 to 1000 mg/L to the treatment liquid, and it is particularly preferable to add 1 to 100 mg/L.

本實施方式之水中油性乳膠組成物具有良好之消泡效果,並且於產品保存中完全不發生黏度增大,故而對隨時間經過而產生之品質劣化無需特別考慮,可穩定地使用。The oil-in-water emulsion composition of the present embodiment has a good defoaming effect and does not cause an increase in viscosity during storage of the product. Therefore, it is not necessary to particularly consider the quality deterioration caused by the passage of time, and it can be used stably.

該水中油性乳膠組成物,藉由以下步驟達成乳化而實現製造,亦即:進行對包含碳原子數為12~30之高級醇的油相成分與難溶於水的親水性無機微粒子之混合物進行加熱熔融,一邊攪拌一邊供給熱水,由此獲得凝膠狀混合物之步驟;以及將熱水加入前述凝膠狀混合物中進行再攪拌之步驟。The oily emulsion composition in water is produced by emulsification by the following steps, that is, a mixture of an oil phase component containing a higher alcohol having 12 to 30 carbon atoms and a hydrophilic inorganic fine particle which is poorly soluble in water is carried out. The step of heating and melting, supplying hot water while stirring, thereby obtaining a gel-like mixture; and adding hot water to the gelled mixture for further stirring.

更具體地說,首先,將油劑與難溶於水之親水性無機微粒子之混合物進行加熱熔融,一邊對其進行攪拌一邊滴下熱水,由此獲得凝膠狀混合物後,便停止攪拌。之後,添加熱水再開始攪拌,由此可順利通過凝膠狀態而獲得以均勻分散系統為目的之水中油性乳膠組成物。More specifically, first, a mixture of an oil agent and a water-insoluble hydrophilic inorganic fine particle is heated and melted, and while stirring, the hot water is dropped to obtain a gel-like mixture, and then the stirring is stopped. Thereafter, the hot water is added and stirring is started, whereby the oily emulsion composition for the purpose of uniformly dispersing the system can be obtained by smoothly passing through the gel state.

經由此種步驟而獲得之組成物,親水性無機微粒子包覆油相成分之微粒子,而以雙重結構狀態之粒子被均勻地分散於水中,幾乎見不到隨時間經過而產生之黏度變化。In the composition obtained by such a step, the hydrophilic inorganic fine particles are coated with the fine particles of the oil phase component, and the particles in the double structure state are uniformly dispersed in the water, and the viscosity change due to the passage of time is hardly observed.

另外,圖1是本發明之水中油性乳膠組成物(油相:栗田工業株式會社製『KURIRESU()』;親水性無機微粒子:碳酸鈣)用顯微鏡觀察時之圖面替代照片。藉由此照片可以觀察到以大致圓球之形狀而分散的粒子。In addition, Fig. 1 is an oil-in-water emulsion composition of the present invention (oil phase: KURIRESU (made by Kurita Industrial Co., Ltd.) )"; hydrophilic inorganic microparticles: calcium carbonate) replaced the photograph with a microscope when viewed under a microscope. From this photograph, particles dispersed in the shape of a substantially spherical shape can be observed.

〔實施例〕[Examples]

以下依據實施例進而詳細說明本發明,但本發明並不由於這些實施例而受到任何限制。The present invention will be described in detail below based on the examples, but the present invention is not limited by these examples.

於以下之實施例及比較例中,水中油性乳膠組成物之隨著時間的黏度增大變化,是將樣品靜置於25℃之恆溫水槽中,並使用B型黏度計與2號攪拌子(spindle),以30rpm之攪拌子旋轉數而進行測定。並對於剛製造後,及於10℃、20℃、30℃、40℃之各溫度條件下保存30天之樣品實施測定。In the following examples and comparative examples, the viscosity of the oily emulsion composition in water changes with time, and the sample is placed in a constant temperature water bath at 25 ° C, and a B-type viscometer and a No. 2 stirrer are used. The spindle was measured by the number of rotations of the stirrer at 30 rpm. The measurement was carried out on a sample which was stored for 30 days at each temperature condition of 10 ° C, 20 ° C, 30 ° C, and 40 ° C immediately after manufacture.

〔實施例1〕[Example 1]

將22.5重量份之碳原子數18之脂肪族醇(SASOL社,Nacol 18-98)與7.5重量份之難溶於水的親水性無機微粒子的碳酸鈣(白石工業(株式會社),Brilliant-1500)混合,並對碳原子數18之脂肪族醇之混合物進行加熱熔融。之後,一邊用渦輪葉片(turbine blade)於73℃下以圓周速度5.2m/s攪拌該熔融物,一邊將73℃之熱水滴下。變成高黏度之凝膠狀混合物時便停止攪拌,接著,繼續加入73℃之熱水且合計將其加入69.94重量份後,再開始進行攪拌。在所生成之乳化分散液中加入0.06重量份的Wahlen膠()(三晶(株式會社),K1C376)並進行冷卻,而得到水中油性乳膠組成物。此實施例1之樣品組成物隨時間經過而黏度增大試驗的結果如下〔表1〕所示。22.5 parts by weight of an aliphatic alcohol having a carbon number of 18 (SASOL, Nacol 18-98) and 7.5 parts by weight of calcium carbonate which is poorly soluble in water and hydrophilic inorganic fine particles (White Rock Industries, Inc., Brilliant-1500) Mixing and heating and melting a mixture of aliphatic alcohols having 18 carbon atoms. Thereafter, the melt was stirred at a peripheral speed of 5.2 m/s with a turbine blade at 73 ° C, and water of 73 ° C was dropped. Stirring was stopped when the gelatinous mixture of high viscosity was changed, and then, hot water of 73 ° C was further added and added to 69.94 parts by weight in total, and stirring was started. 0.06 parts by weight of Wahlen gum was added to the resulting emulsified dispersion ( (Sanjing Co., Ltd., K1C376) was cooled to obtain an oily latex composition in water. The results of the viscosity increase test of the sample composition of this Example 1 over time are shown in the following [Table 1].

如上列〔表1〕所示,本樣品之黏度,剛製作後為360mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為383、412、420、452 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above table [Table 1], the viscosity of this sample was just 360 mPa after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days are 383, 412, 420, 452 mPa. s. That is, the viscosity hardly changes with time.

〔實施例2〕[Example 2]

將22.5重量份之碳原子數為18的脂肪族醇(SASOL社,Nacol 18-98)與7.5重量份之作為難溶於水的親水性無機微粒子之氫氧化鋁(關東化學(株式會社)鹿特級,平均粒子直徑0.05μm)混合,以下藉由與實施例1同樣之方法而獲得水中油性乳膠組成物之樣品。此實施例2之樣品組成物隨時間經過而黏度增大試驗的結果如下〔表2〕所示。22.5 parts by weight of an aliphatic alcohol having a carbon number of 18 (SASOL, Nacol 18-98) and 7.5 parts by weight of aluminum hydroxide as a poorly water-soluble hydrophilic inorganic fine particle (Kanto Chemical Co., Ltd. deer) A special grade, an average particle diameter of 0.05 μm was mixed, and a sample of the oily latex composition in water was obtained by the same method as in Example 1. The results of the viscosity increase test of the sample composition of Example 2 over time were as follows [Table 2].

如上列之〔表2〕所示,本樣品之黏度,剛製作後為352mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為370、403、410、425 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above table [Table 2], the viscosity of this sample was 352 mPa immediately after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days is 370, 403, 410, 425 mPa. s. That is, the viscosity hardly changes with time.

〔實施例3〕[Example 3]

將22.5重量份之碳原子數為18的脂肪族醇(SASOL社,Nacol 18-98)與7.5重量份之作為難溶於水的親水性無機微粒子的氧化鋁(關東化學(株式會社)鹿特級)混合,以下藉由與實施例1同樣之方法而獲得水中油性乳膠組成物之樣品。此實施例3之樣品組成物隨時間經過而黏度增大試驗之結果如下〔表3〕所示。22.5 parts by weight of an aliphatic alcohol (SASOL, Nacol 18-98) having a carbon number of 18 and 7.5 parts by weight of alumina as a poorly water-soluble hydrophilic inorganic fine particle (Kanto Chemical Co., Ltd.) The mixture was mixed, and a sample of the oily latex composition in water was obtained by the same method as in Example 1. The results of the viscosity increase test of the sample composition of Example 3 over time were as follows [Table 3].

如上列〔表3〕所示,本樣品之黏度剛製作後為412mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為455、461、466、503 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above table [Table 3], the viscosity of this sample was just 412 mPa after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days is 455, 461, 466, 503 mPa. s. That is, the viscosity hardly changes with time.

〔實施例4〕[Example 4]

將22.5重量份之碳原子數為18的脂肪族醇(SASOL社,Nacol 18-98)與7.5重量份之作為難溶於水的親水性無機微粒子的氧化鈦(石原產業(株式會社)TIPAQUE W-10平均粒子直徑0.04μm)混合,以下藉由與實施例1同樣之方法而獲得水中油性乳膠組成物之樣品。此實施例4之樣品組成物隨時間經過而黏度增大試驗的結果如下〔表4〕所示。22.5 parts by weight of an aliphatic alcohol (SASOL, Nacol 18-98) having a carbon number of 18 and 7.5 parts by weight of titanium oxide as a poorly water-soluble hydrophilic inorganic fine particle (Ishihara Industry Co., Ltd. TIPAQUE W A mixture of -10 average particle diameters of 0.04 μm was used, and a sample of the oily latex composition in water was obtained by the same method as in Example 1. The results of the viscosity increase test of the sample composition of this Example 4 over time are shown in the following [Table 4].

如上列〔表4〕所示,本樣品之黏度,剛製作後為383mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為405、411、445、462 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above table [Table 4], the viscosity of this sample was 383 mPa immediately after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days is 405, 411, 445, 462 mPa. s. That is, the viscosity hardly changes with time.

〔實施例5〕[Example 5]

將20重量份之碳原子數為18的脂肪族醇(SASOL社,Nacol 18-98)、5重量份之作為難溶於水的親水性無機微粒子的碳酸鈣(白石工業(株),Brilliant-1500)及5重量份之矽膠(silica gel)(日本Silica工業(株式會社)Nipsil E-22 OA)等混合,以下藉由與實施例1同樣之方法而獲得水中油性乳膠組成物之樣品。此實施例5之樣品組成物隨時間經過而黏度增大試驗的結果如下〔表5〕所示。20 parts by weight of an aliphatic alcohol having a carbon number of 18 (SASOL, Nacol 18-98), and 5 parts by weight of calcium carbonate as a poorly water-soluble hydrophilic inorganic fine particle (White Rock Industries, Inc., Brilliant- 1500) and 5 parts by weight of silica gel (Nipsil E-22 OA, Japan) were mixed, and a sample of the oily latex composition in water was obtained by the same method as in Example 1. The results of the viscosity increase test of the sample composition of this Example 5 over time are shown in the following [Table 5].

如上列〔表5〕所示,本樣品之黏度,剛製作後為322 mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為381、383、398、418 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above table [Table 5], the viscosity of this sample was 322 mPa immediately after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days is 381, 383, 398, 418 mPa. s. That is, the viscosity hardly changes with time.

〔實施例6〕[Example 6]

將20重量份之碳原子數為18的脂肪族醇(SASOL社,Nacol 18-98)、5重量份之作為難溶於水的親水性無機微粒子之碳酸鈣(白石工業(株),Brilliant-1500)及5重量份之矽烷化的矽膠(日本Silica工業(株式會社)Nipsil E-220A)等混合,以下藉由與實施例1同樣之方法而獲得水中油性乳膠組成物之樣品。此實施例6之樣品組成物隨時間經過而黏度增大試驗的結果如下〔表6〕所示。20 parts by weight of an aliphatic alcohol having a carbon number of 18 (SASOL, Nacol 18-98), and 5 parts by weight of calcium carbonate as a poorly water-soluble hydrophilic inorganic fine particle (White Stone Industry Co., Ltd., Brilliant- 1500) and 5 parts by weight of a non-alkylated tannin (Nipsil E-220A, Japan) were mixed, and a sample of the oily latex composition in water was obtained in the same manner as in Example 1. The results of the viscosity increase test of the sample composition of this Example 6 over time are shown in the following [Table 6].

如上列〔表6〕所示,本樣品之黏度,剛製作後為331 mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為346、351、350、384 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above table [Table 6], the viscosity of this sample was 331 mPa immediately after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days is 346, 351, 350, 384 mPa. s. That is, the viscosity hardly changes with time.

〔實施例7〕[Example 7]

將22.5重量份之碳原子數為14的脂肪族醇(SASOL社,NACOL 14-98)與7.5重量份之作為難溶於水的親水性無機微粒子的碳酸鈣(白石工業(株),Brilliant-1500)混合,以下藉由與實施例1同樣之方法而獲得水中油性乳膠組成物之樣品。此實施例7之樣品組成物隨時間經過而黏度增大試驗的結果如下〔表7〕所示。22.5 parts by weight of an aliphatic alcohol having a carbon number of 14 (SASOL, NACOL 14-98) and 7.5 parts by weight of calcium carbonate as a poorly water-soluble hydrophilic inorganic fine particle (White Rock Industries, Inc., Brilliant- 1500) Mixing, a sample of the oily latex composition in water was obtained in the same manner as in Example 1 below. The results of the viscosity increase test of the sample composition of this Example 7 over time are shown in the following [Table 7].

如上列〔表7〕所示,本樣品之黏度,剛製作後為378 mPa.s,於10℃、20℃、30℃、40℃下保存30天的黏度則分別為429、426、441、468 mPa.s。亦即,黏度幾乎不隨時間經過而變化。As shown in the above column [Table 7], the viscosity of this sample was 378 mPa immediately after fabrication. s, the viscosity at 10 ° C, 20 ° C, 30 ° C, 40 ° C for 30 days is 429, 426, 441, 468 mPa. s. That is, the viscosity hardly changes with time.

[比較例1][Comparative Example 1]

取代無機微粒子作為乳化劑,而加入0.8重量份之碳原子數為12~14,且在第3~7位置之碳原子上具有羥基之第二級醇的乙烯氧化物(ethylene Oxide)30莫爾添加物(日本觸媒(株式會社),SOFUTANO()300),並對30重量份之碳原子數為18的脂肪族醇(SASOL社,Nacol 18-98)進行加熱熔融後,一邊於73℃下用渦輪葉片以圓周速度5.2m/s攪拌此熔融物,一邊添加69.14重量份之73℃的熱水而進行乳化轉相,進而對水中油性乳膠粒子進行調整。在所生成之乳化分散液中,加入0.06重量份之Wahlen膠(三晶(株式會社),K1C376)並進行冷卻而獲得水中油性乳膠組成物。此比較例1之樣品組成物之隨時間經過而黏度增大試驗的結果如以下之〔表8〕所示。Instead of the inorganic fine particles as an emulsifier, 0.8 parts by weight of ethylene oxide (ethylene Oxide) 30 moles having a carbon number of 12 to 14 and a hydroxyl group having a hydroxyl group at the 3rd to 7th carbon atoms is added. Additive (Japan Catalyst (株式会社), SOFUTANO ( 300), and 30 parts by weight of an aliphatic alcohol (SASOL, Nacol 18-98) having a carbon number of 18 was heated and melted, and then stirred at a peripheral speed of 5.2 m/s with a turbine blade at 73 ° C. The melt was emulsified and phase-introduced by adding 69.14 parts by weight of hot water of 73 ° C to adjust the oily latex particles in the water. To the resulting emulsified dispersion, 0.06 part by weight of Wahlen gum (Tricrystal Co., Ltd., K1C376) was added and cooled to obtain an oily emulsion composition in water. The results of the viscosity increase test of the sample composition of Comparative Example 1 as a function of time are shown in the following [Table 8].

如上列〔表8〕所示,本樣品之黏度結果為:於製作後進行冷卻之過程中固化為乳油狀,黏度超過10000 mpa.s。As shown in the above table [Table 8], the viscosity of the sample is as follows: it is cured to a creamy state during the cooling process after preparation, and the viscosity exceeds 10000 mpa. s.

[比較例2][Comparative Example 2]

取代無機微粒子作為乳化劑,而加入0.8重量份之碳原子數為12~14,在3~7位置的碳原子上具有羥基之第二級醇之乙烯氧化物(ethylene Oxide)30莫爾(mol)添加物(日本觸媒(株式會社),SOFUTANO 300),並將30重量份之碳原子散為14的脂肪族醇(SASOL祉,Nacol 14-98)進行加熱熔融,之後藉由與上述比較例1同樣之方法,處理此熔融物而得到水中油性乳膠組成物。此比較例2之樣品組成物之隨時間經過而黏度增大試驗的結果如以下之〔表9〕所示。Substituting inorganic fine particles as an emulsifier, adding 0.8 parts by weight of ethylene oxide (ethylene Oxide) 30 mol (mol) of a second-order alcohol having a hydroxyl group of 12 to 14 at a carbon atom of 3 to 7 Addition (Nippon Catalyst Co., Ltd., SOFUTANO 300), and heat-melting 30 parts by weight of an aliphatic alcohol (SASOL®, Nacol 14-98) having 14 carbon atoms dispersed, and then comparing with the above In the same manner as in Example 1, the melt was treated to obtain an oily latex composition in water. The results of the viscosity increase test of the sample composition of Comparative Example 2 over time were as shown in the following [Table 9].

如上列〔表9〕所示,本樣品之黏度結果為於製作後進行冷卻之過程中固化為乳油狀,黏度超過10000 mPa.s。As shown in the above table [Table 9], the viscosity of the sample was cured to a creamy state during the cooling after the preparation, and the viscosity exceeded 10000 mPa. s.

從以上之結果可確認,使用難溶於水之親水性無機微粒子對含有高級醇之油相成分進行乳化的實施例1~7之水中油性乳膠組成物,於10~40℃之溫度條件下保存30天後,也幾乎不發生黏度變化,顯示良好之保存穩定性。與此相對可以確認,即使是與實施例1相同之油相成分(碳原子數為18之高級醇),使用界面活化劑而進行乳化之水中油性乳膠組成物,在乳化冷卻時仍會產生黏度升高而喪失其流動性。From the above results, it was confirmed that the oily emulsion composition of Examples 1 to 7 in which the oil phase component containing the higher alcohol was emulsified by using the hydrophilic inorganic fine particles which are hardly soluble in water was stored at a temperature of 10 to 40 ° C. After 30 days, almost no change in viscosity occurred, indicating good storage stability. On the other hand, it was confirmed that even the oil phase component (higher alcohol having 18 carbon atoms) similar to that of Example 1 was emulsified by using an interfacial activator, and the viscosity was still generated when emulsified and cooled. Increase and lose its mobility.

〔產業上之可利用性〕[Industrial Applicability]

本發明之水中油性乳膠組成物,具有良好之保存穩定性,不僅可用於消泡劑,還可廣泛應用於具有隨時間經過而黏度增大之問題的乳膠產品,例如化妝品領域、食品領域等之乳膠產品等。The oil-in-water emulsion composition of the invention has good storage stability, can be used not only for defoaming agents, but also widely used in latex products having problems of increasing viscosity over time, such as cosmetics, food, etc. Latex products, etc.

圖1是本發明之水中油性乳膠組成物之用顯微鏡觀察時之圖面替代照片。BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a photograph showing a substitute of a microscope for the composition of an oily emulsion of the present invention.

Claims (6)

一種水中油性乳膠組成物,包括:油相成分,其包含碳原子數為12~30之高級醇;以及親水性無機微粒子,其難溶於水;其中,前述油相成分之微粒子以被選自於碳酸鈣、氫氧化鋁、氧化鋁、氧化鈦、高嶺土、滑石的任一者的前述親水性無機微粒子所包覆之狀態而分散在水中,且不含有一切乳化劑成分。 An oil-in-water emulsion composition comprising: an oil phase component comprising a higher alcohol having 12 to 30 carbon atoms; and hydrophilic inorganic microparticles which are hardly soluble in water; wherein the fine particles of the oil phase component are selected from The hydrophilic inorganic fine particles of any of calcium carbonate, aluminum hydroxide, aluminum oxide, titanium oxide, kaolin, and talc are dispersed in water and do not contain all emulsifier components. 如申請專利範圍第1項所述之水中油性乳膠組成物,其中,所述水中油性乳膠組成物含有增黏劑。 The oily emulsion composition according to claim 1, wherein the oily emulsion composition of the water contains a tackifier. 如申請專利範圍第1項或第2項所述之水中油性乳膠組成物,其中,前述親水性無機微粒子之平均粒子直徑小於1μm。 The oil-in-water emulsion composition according to Item 1 or 2, wherein the hydrophilic inorganic fine particles have an average particle diameter of less than 1 μm. 如申請專利範圍第1項或第2項所述之水中油性乳膠組成物,其中,所述水中油性乳膠組成物為發泡抑制劑。 The oil-in-water emulsion composition according to claim 1 or 2, wherein the oily emulsion composition in water is a foaming inhibitor. 如申請專利範圍第3項所述之水中油性乳膠組成物,其中,所述水中油性乳膠組成物為發泡抑制劑。 The oily emulsion composition according to claim 3, wherein the oily emulsion composition in water is a foaming inhibitor. 一種水中油性乳膠組成物之製造方法,包括:第一步驟,其對包含碳原子數為12~30之高級醇之油相成分與難溶於水之親水性無機微粒子的混合物進行加熱熔融,且邊攪拌邊添加熱水而獲得凝膠狀混合物;以及第二步驟,在第一步驟後便停止攪拌之後,不添加一切乳化劑,將熱水加入前述凝膠狀混合物中並進行再攪拌,使得所述油相成分被所述親水性無機微粒子所包覆的 雙重結構狀態的粒子分散於水中。A method for producing an oily emulsion composition in water, comprising: a first step of heating and melting a mixture of an oil phase component containing a higher alcohol having 12 to 30 carbon atoms and a hydrophilic inorganic fine particle which is poorly soluble in water, and Adding hot water with stirring to obtain a gel-like mixture; and a second step, after stopping the stirring after the first step, adding all the emulsifier, adding hot water to the gelatinous mixture and stirring again, so that The oil phase component is coated with the hydrophilic inorganic microparticles Particles in a dual structure state are dispersed in water.
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