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KR20230104300A - manufacturing method of titanium dioxide composite pigment and titanium dioxide composite pigment manufactured through the same - Google Patents

manufacturing method of titanium dioxide composite pigment and titanium dioxide composite pigment manufactured through the same Download PDF

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Publication number
KR20230104300A
KR20230104300A KR1020210191922A KR20210191922A KR20230104300A KR 20230104300 A KR20230104300 A KR 20230104300A KR 1020210191922 A KR1020210191922 A KR 1020210191922A KR 20210191922 A KR20210191922 A KR 20210191922A KR 20230104300 A KR20230104300 A KR 20230104300A
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South Korea
Prior art keywords
titanium dioxide
composite pigment
dioxide composite
tio
pigment
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Application number
KR1020210191922A
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Korean (ko)
Inventor
조현대
김종근
권민정
김미서
황준필
이예슬
Original Assignee
주식회사 코스메카코리아
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Priority to KR1020210191922A priority Critical patent/KR20230104300A/en
Priority to PCT/KR2022/019525 priority patent/WO2023128347A1/en
Priority to CN202211677462.8A priority patent/CN116376324A/en
Publication of KR20230104300A publication Critical patent/KR20230104300A/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C09C1/0021—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a core coated with only one layer having a high or low refractive index
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29—Titanium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02—Preparations containing skin colorants, e.g. pigments
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3615—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C1/363—Drying, calcination
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043—Drying, calcination
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/42—Colour properties
    • A61K2800/43—Pigments; Dyes
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    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
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Abstract

Disclosed are a method for producing a titanium dioxide composite pigment, and a titanium dioxide composite pigment produced thereby. According to the method for producing a titanium dioxide composite pigment and a titanium dioxide composite pigment produced thereby according to the present invention, it is possible to: improve efficacy by modifying the surface of a high refractive index inorganic composite pigment through a process of coating the pigment with a film forming agent; bring about the effects of improved dispersion, adhesion, and durability of the inorganic composite pigment in an oil-in-water form; and provide a gel-like titanium dioxide composite pigment which satisfies the user feeling of use and appears to have a highly moist exterior. In addition, the titanium dioxide composite pigment has a smooth appearance, good spreadability, and a light and refreshing feel when applied to the skin, and can achieve effective UV protection by increasing SPF and PA levels due to having high dispersion and stability in a formulation.

Description

이산화티탄 복합안료 제조방법 및 이를 통해 제조된 이산화티탄 복합안료{manufacturing method of titanium dioxide composite pigment and titanium dioxide composite pigment manufactured through the same}Titanium dioxide composite pigment manufacturing method and titanium dioxide composite pigment manufactured through the same {manufacturing method of titanium dioxide composite pigment and titanium dioxide composite pigment manufactured through the same}

본 발명은 이산화티탄 복합안료 제조방법 및 이를 통해 제조된 이산화티탄 복합안료에 관한 것으로, 더욱 상세하게는 분산력, 부착력 및 지속성이 향상되고, 코팅 처리 공정을 통해 안료 표면을 개질하여 매끄러운 성상을 구현함으로써 발림성과 사용감을 라이트하고 산뜻하게 발현할 수 있으며, SPF와 PA 수치를 높여 자외선 차단 성능이 뛰어난 이산화티탄 복합안료 제조방법 및 이를 통해 제조된 이산화티탄 복합안료에 관한 것이다.The present invention relates to a method for preparing a titanium dioxide composite pigment and a titanium dioxide composite pigment produced through the same, and more particularly, by improving dispersion, adhesion and durability, and by realizing a smooth property by modifying the surface of the pigment through a coating treatment process. It relates to a method for producing a titanium dioxide composite pigment that can express light and refreshing feeling of application and use, and has excellent UV blocking performance by increasing SPF and PA levels, and a titanium dioxide composite pigment manufactured through this method.

아름다움을 추구하는 여성의 본능은 어제, 오늘의 일이 아니지만, 최근 들어 자신을 더욱 예뻐 보이게 하기 위한 체형 관리나 미용 또는 화장품에 대한 관심이 더욱 높아지는 추세에 있다.Women's instinct to pursue beauty is not a thing of yesterday or today, but recently, interest in body shape management, beauty, or cosmetics to make themselves look prettier is on the rise.

그리고 여성뿐만 아니라 남성들도 피부관리를 위해 화장품에 관심을 두게 됨에 따라 화장품 시장은 계속해서 확대되고 있으며, 다양한 종류의 화장품이 시장에 출시되고 있다.In addition, as men as well as women are interested in cosmetics for skin care, the cosmetics market continues to expand, and various types of cosmetics are being launched into the market.

일반적으로 화장품은 크게 기초 화장품, 메이크업 베이스와 색조 화장품 등으로 나눌 수 있고, 고형, 액상 또는 겔상의 화장료로 제조되며, 이들을 보관하는 화장품 용기도 다양하게 적용되고 있다.In general, cosmetics can be largely divided into basic cosmetics, makeup base and color cosmetics, etc., and are made of solid, liquid or gel cosmetics, and cosmetic containers for storing them are also applied in various ways.

최근에는 보습, 미백, 주름개선, 자외선 차단, 여드름 완화, 아토피 완화, 항염증이나 각질용해 등 다양한 기능을 수행할 수 있는 기능성 화장품도 널리 소비되고 있다.Recently, functional cosmetics that can perform various functions such as moisturizing, whitening, wrinkle improvement, UV protection, acne relief, atopy relief, anti-inflammation or keratolysis are also widely consumed.

한편, 일반적인 의미에서 안료는 물질에 색을 발현시키는 색소를 일컫는다. 염료는 물에 녹는 색소로서 섬유나 종이에 스며들게 해서 고착(固着)시키는 데 반해 안료는 물이나 기름 등에 녹지 않는 미세한 분말의 고체로서 도료(塗料), 그림물감, 인쇄잉크, 플라스틱, 고무 등에 섞어서 쓴다.On the other hand, in a general sense, a pigment refers to a pigment that expresses color in a material. Dyes are water-soluble pigments that permeate and adhere to fibers or paper, while pigments are fine powdery solids that are insoluble in water or oil and are used by mixing with paints, paints, printing inks, plastics, rubber, etc. .

안료는 무기(無機)안료와 유기(有機)안료로 분류하며 무기안료는 열이나 햇볕 하에서 안정적이고 색이 변하지 않는 특징이 있고, 유기안료는 염료를 물에 녹지 않는 형태로 만든 것으로 색도 선명하고 종류가 많다.Pigments are classified into inorganic pigments and organic pigments. Inorganic pigments are stable and do not change color under heat or sunlight, and organic pigments are made of dyes insoluble in water, and have vivid colors and types There are many.

이러한 안료는 색조화장품에 많이 사용되는데 그 주된 목적은 피부를 알맞게 피복해서 채색을 부여하는 것이다. 즉 피부의 "검버섯"이나 "주근깨" 등을 감추어 좋아하는 색채를 입히는 한편, 피지 등의 피부분비물을 흡수해서 얼굴에 기름이 흐르는 것을 막아주어 건강하고 매력적인 용모를 만드는 것이다. These pigments are widely used in color cosmetics, and their main purpose is to appropriately coat the skin and impart color. In other words, it hides "age spots" or "freckles" of the skin to give the desired color, while absorbing skin secretions such as sebum to prevent oil from flowing on the face to create a healthy and attractive appearance.

그런데 안료를 적용함에 있어서, 화장품으로서의 위생적, 감각적 요소를 함께 고려해야 한다. 그러므로 화장품용 안료에 요구되는 조건은 피부에 무해인 것은 물론 법적으로 규제된 품목, 규격, 시험법, 사용기준에 적합한 품질이어야 한다.However, in applying pigments, hygiene and sensory factors as cosmetics should be considered together. Therefore, the conditions required for cosmetic pigments are not only harmless to the skin, but also of quality suitable for legally regulated items, specifications, test methods, and usage standards.

색조 화장품은 유기안료, 무기안료(체질안료, 백색안료, 유색안료, 펄안료) 등으로 된 혼합분체를 여러가지 기재 속에 분산시킨 것이다. 기재를 만드는 원료는 유지, 납, 탄화수소, 지방산, 고급알콜, 합성에스테르유 등의 유성 원료와 다가 알콜, 수용성 고분자 등의 수성원료 및 계면활성제(유화제, 분산제) 등이다. 이들 원료를 조합해서 여러가지 형상의 화장품이 만들어진다. Color cosmetics are obtained by dispersing mixed powders of organic pigments and inorganic pigments (constituent pigments, white pigments, colored pigments, pearl pigments) in various substrates. The raw materials used to make the substrate include oil-based raw materials such as fats and oils, lead, hydrocarbons, fatty acids, higher alcohols, and synthetic ester oils, water-based raw materials such as polyhydric alcohols and water-soluble polymers, and surfactants (emulsifiers and dispersants). Cosmetics of various shapes are made by combining these raw materials.

색조 화장품에서 안료의 역할은 유기안료, 무기안료로 제품의 색조를 조정하고 백색안료는 색조 외에 피복력을 컨트롤하기 위해 사용된다. 체질안료나 그밖의 분말은 안료의 희석제로서 색조를 조정함과 함께 제품에 신전성, 부착성, 광택 또는 그 제품의 체형을 유지할 목적으로 사용된다. The role of pigments in color cosmetics is to adjust the color of products with organic and inorganic pigments, and white pigments are used to control the covering power in addition to color. Extender pigments or other powders are used as pigment diluents to adjust the color tone and to maintain extensibility, adhesion, gloss or body shape of the product.

한편, 기능성 화장품 중의 하나인 자외선차단 화장품은 자외선을 흡수, 산란 및 반사 등을 통해 차단하는 무기 자외선차단제, 유기 자외선차단제가 함유되어 있다.On the other hand, sunscreen cosmetics, which are one of functional cosmetics, contain inorganic sunscreens and organic sunscreens that block ultraviolet rays through absorption, scattering, and reflection.

유기 자외선차단제는 자외선을 흡수하여 피부에 도달하는 자외선의 양을 줄여주는 방식으로 빛을 차단하는 반면, 무기 자외선차단제는 자외선을 반사, 산란하여 피부를 보호하는 방식이다. Organic sunscreen blocks light by absorbing ultraviolet rays and reducing the amount of ultraviolet rays reaching the skin, while inorganic sunscreen protects the skin by reflecting and scattering ultraviolet rays.

무기 자외선차단제는 그 예로 산화아연 (ZnO), 이산화티탄(TiO₂)을 들 수 있다. 백탁현상, 피부 발림성이 좋지 않은 단점이 있으나, 자외선을 포함한 태양광선에 대해 비활성이 크고 안전성이 우수하다. 그리고 피부에 흡수 또는 축적되지 않으므로 피부자극이나 알러지를 유발하지 않는다.Examples of inorganic sunscreens include zinc oxide (ZnO) and titanium dioxide (TiO₂). It has the disadvantages of white turbidity and poor skin application, but it is highly inactive against sunlight including ultraviolet rays and has excellent safety. And since it is not absorbed or accumulated in the skin, it does not cause skin irritation or allergy.

본 발명자는 그동안의 연구를 통해 자외선차단 효과를 갖는 이산화티탄 복합안료 제조방법을 개발하였으며, 이를 통해 분산력, 부착력 및 지속성이 향상되고, 코팅 처리 공정을 통해 안료 표면을 개질하여 매끄러운 성상을 구현함으로써 발림성과 사용감을 라이트하고 산뜻하게 발현할 수 있으며, SPF와 PA 수치를 높여 자외선 차단 성능이 뛰어난 이산화티탄 복합안료를 제공할 수 있게 되었다.The inventors of the present invention have developed a method for producing a titanium dioxide composite pigment having an ultraviolet ray blocking effect through previous studies, and through this, the dispersion, adhesion and durability are improved, and the surface of the pigment is modified through the coating treatment process to realize a smooth property, thereby improving the spreadability. It is possible to provide a titanium dioxide composite pigment with excellent sunscreen performance by increasing the SPF and PA levels and providing a light and fresh feeling of use.

본 발명의 실시예들은 고굴절률의 무기성 복합안료에 피막형성제를 코팅처리하는 공정을 통해 안료의 표면을 개질하여 효능을 향상시키고자 한다.Embodiments of the present invention are intended to improve the efficacy by modifying the surface of the pigment through a process of coating the film forming agent on the inorganic composite pigment of high refractive index.

또한, 수중유형에서의 무기성 복합안료의 분산력 향상 및 부착력 향상 그리고 지속성 향상 등의 효과를 발현시키고자 한다.In addition, it is intended to express effects such as improved dispersion, improved adhesion, and improved durability of inorganic composite pigments in water type.

또한, 소비자의 사용감을 만족시키고 외관의 수분감이 높아보이는 젤 성상의 이산화티탄 복합안료를 제공하고자 한다.In addition, it is intended to provide a gel-like titanium dioxide composite pigment that satisfies the user's feeling of use and has a high appearance of moisture.

또한, 매끄러운 성상을 띄며 발림성이 좋고 피부 도포 시 후감이 라이트하고 산뜻한 이산화티탄 복합안료를 제공하고자 한다.In addition, it is intended to provide a titanium dioxide composite pigment that has a smooth appearance, good spreadability, and a light aftertaste when applied to the skin.

또한, 제형 내에서의 분산도와 안정도가 높아짐에 따라 SPF 와 PA 수치를 상승시켜 효과적인 자외선 차단을 실현하고자 한다.In addition, as the degree of dispersion and stability in the formulation increases, the SPF and PA levels are increased to realize effective sun protection.

본 발명의 일측면에 따르면, (a) 증류수에 이산화티탄을 첨가하고 교반하여 분산하는 단계; (b) 사염화티탄 수용액과 10wt% 내지 30wt% 농도의 수산화나트륨 수용액을 상기 분산된 이산화티탄에 첨가하고 교반하여 수산화티탄 코팅을 진행하는 단계; (c) 상기 수산화티탄 코팅이 완료된 용액을 정치시켜 발생한 백색 침전물을 증류수를 사용하여 세척하고 여과하는 단계; (d) 상기 여과된 분체를 건조하는 단계; 및, (e) 상기 수산화티탄 복합 분체를 700℃ 내지 950℃에서 소결하여 이산화티탄 복합안료를 형성하는 단계;를 포함하는 이산화티탄 복합안료 제조방법이 제공될 수 있다.According to one aspect of the present invention, (a) adding titanium dioxide to distilled water and dispersing by stirring; (b) adding an aqueous solution of titanium tetrachloride and an aqueous solution of sodium hydroxide having a concentration of 10wt% to 30wt% to the dispersed titanium dioxide and stirring to proceed with titanium hydroxide coating; (c) washing and filtering the white precipitate generated by standing the titanium hydroxide-coated solution with distilled water; (d) drying the filtered powder; And, (e) forming a titanium dioxide composite pigment by sintering the titanium hydroxide composite powder at 700 ° C to 950 ° C; a method for preparing a titanium dioxide composite pigment may be provided.

상기 (a) 단계 내지 (d) 단계 공정의 반응식은, TiO2 + TiOCl2+ 2NaOH → TiO(OH)2/TiO2 + Na+Cl- 일 수 있다.The reaction formula of steps (a) to (d) may be TiO 2 + TiOCl 2 + 2NaOH → TiO(OH) 2 /TiO 2 + Na+Cl - .

상기 (e) 단계 공정 반응식은, TiO(OH)2 /TiO2 → TiO2 + H2O 일 수 있다.The reaction equation for step (e) may be TiO(OH) 2 /TiO 2 → TiO 2 + H 2 O.

본 발명에 따른 이산화티탄 복합안료 제조방법은 상기 이산화티탄 복합안료 90wt% 내지 98wt%와 수용성 폴리머 물질 또는 실리콘, 실란, 실리콘 공중합체 2wt% 내지 10wt%를 헨셀믹서에 넣고 분산처리하는 단계;를 더 포함하여 이루어질 수 있다.The titanium dioxide composite pigment manufacturing method according to the present invention further comprises the step of dispersing 90 wt% to 98 wt% of the titanium dioxide composite pigment and 2 wt% to 10 wt% of a water-soluble polymer material or silicone, silane, or silicone copolymer into a Henschel mixer. can be made including

본 발명에 따른 이산화티탄 복합안료 제조방법은 상기 분산처리된 분체를 건조하는 단계;를 더 포함하여 이루어질 수 있다.The titanium dioxide composite pigment manufacturing method according to the present invention may further include a step of drying the dispersion-treated powder.

본 발명에 따른 이산화티탄 복합안료 제조방법은 상기 건조된 분체를 추가 분쇄하여 친수성 또는 소수성을 부여하는 단계;를 더 포함하여 이루어질 수 있다.The titanium dioxide composite pigment manufacturing method according to the present invention may further include a step of additionally pulverizing the dried powder to impart hydrophilicity or hydrophobicity.

또한, 상기한 제조방법에 의해 제조된 이산화티탄 복합안료가 제공될 수 있다.In addition, a titanium dioxide composite pigment prepared by the above manufacturing method may be provided.

본 발명의 실시예들은 고굴절률의 무기성 복합안료에 피막형성제를 코팅처리하는 공정을 통해 안료의 표면을 개질하여 효능을 향상시킬 수 있다.Embodiments of the present invention can improve the efficacy by modifying the surface of the pigment through a process of coating the film forming agent on the inorganic composite pigment of high refractive index.

또한, 수중유형에서의 무기성 복합안료의 분산력 향상 및 부착력 향상 그리고 지속성 향상 등의 효과를 발현시킬 수 있다.In addition, it is possible to express effects such as improved dispersion, improved adhesion, and improved durability of inorganic composite pigments in water type.

또한, 소비자의 사용감을 만족시키고 외관의 수분감이 높아보이는 젤 성상의 이산화티탄 복합안료를 제공할 수 있다.In addition, it is possible to provide a gel-like titanium dioxide composite pigment that satisfies the user's feeling of use and has a high appearance of moisture.

또한, 매끄러운 성상을 띄며 발림성이 좋고 피부 도포 시 후감이 라이트하고 산뜻한 이산화티탄 복합안료를 제공할 수 있다.In addition, it is possible to provide a titanium dioxide composite pigment having a smooth property, good spreadability, and a light aftertaste when applied to the skin.

또한, 제형 내에서의 분산도와 안정도가 높아짐에 따라 SPF 와 PA 수치를 상승시켜 효과적인 자외선 차단을 실현할 수 있다.In addition, as the degree of dispersion and stability in the formulation increases, SPF and PA levels can be increased to realize effective sun protection.

도 1은 본 발명의 일 실시예에 따른 이산화티탄 복합안료 제조방법의 공정을 나타낸 순서도
도 2는 비교예1(Control A)의 분산정도를 나타낸 이미지
도 3은 비교예2(Control B)의 분산정도를 나타낸 이미지
도 4는 실험예1(실험 A)의 분산정도를 나타낸 이미지
도 5는 실험예2(실험 B)의 분산정도를 나타낸 이미지
도 6은 비교예1, 비교예2, 실험예1 및 실험예2의 SPF와 PA 수치를 나타낸 그래프1 is a flowchart showing a process of a method for producing a titanium dioxide composite pigment according to an embodiment of the present invention.
2 is an image showing the degree of dispersion of Comparative Example 1 (Control A)
3 is an image showing the degree of dispersion of Comparative Example 2 (Control B)
4 is an image showing the degree of dispersion of Experimental Example 1 (Experiment A)
5 is an image showing the degree of dispersion of Experimental Example 2 (Experiment B)
Figure 6 is a graph showing the SPF and PA values of Comparative Example 1, Comparative Example 2, Experimental Example 1 and Experimental Example 2

이하, 첨부한 도면들을 참조하여 본 발명의 바람직한 실시예들을 상세히 설명하기로 한다. 그러나 본 발명은 여기서 설명되는 실시예들에 한정되지 않고 다른 형태로 구체화될 수도 있다. 오히려, 여기서 소개되는 실시예들은 개시된 내용이 철저하고 완전해질 수 있도록, 그리고 당업자에게 본 발명의 사상이 충분히 전달될 수 있도록 하기 위해 제공되는 것이다. 명세서 전체에 걸쳐서 동일한 참조번호들은 동일한 구성요소들을 나타낸다.Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided so that the disclosed content will be thorough and complete, and the spirit of the present invention will be sufficiently conveyed to those skilled in the art. Like reference numbers indicate like elements throughout the specification.

도 1은 본 발명의 일 실시예에 따른 이산화티탄 복합안료 제조방법의 공정을 나타낸 순서도이고, 도 2는 비교예1(Control A)의 분산정도를 나타낸 이미지이며, 도 3은 비교예2(Control B)의 분산정도를 나타낸 이미지이다. 도 4는 실험예1(실험 A)의 분산정도를 나타낸 이미지이고, 도 5는 실험예2(실험 B)의 분산정도를 나타낸 이미지이며, 도 6은 비교예1, 비교예2, 실험예1 및 실험예2의 SPF와 PA 수치를 나타낸 그래프이다.1 is a flow chart showing a process for manufacturing a titanium dioxide composite pigment according to an embodiment of the present invention, FIG. 2 is an image showing the degree of dispersion of Comparative Example 1 (Control A), and FIG. 3 is Comparative Example 2 (Control A). It is an image showing the degree of dispersion of B). Figure 4 is an image showing the degree of dispersion of Experimental Example 1 (Experiment A), Figure 5 is an image showing the degree of dispersion of Experimental Example 2 (Experiment B), Figure 6 is Comparative Example 1, Comparative Example 2, Experimental Example 1 And it is a graph showing the SPF and PA values of Experimental Example 2.

도 1 내지 도 6을 참조하면, 본 발명의 일 실시예에 따른 이산화티탄 복합안료 제조방법은 크게 (a) 증류수에 이산화티탄을 첨가하고 교반하여 분산하는 단계(S100); (b) 사염화티탄 수용액과 10wt% 내지 30wt% 농도의 수산화나트륨 수용액을 상기 분산된 이산화티탄에 첨가하고 교반하여 수산화티탄 코팅을 진행하는 단계(S200); (c) 상기 수산화티탄 코팅이 완료된 용액을 정치시켜 발생한 백색 침전물을 증류수를 사용하여 세척하고 여과하는 단계(S300); (d) 상기 여과된 분체를 건조하는 단계(S400); 및, (e) 상기 수산화티탄 복합 분체를 700℃ 내지 950℃에서 소결하여 이산화티탄 복합안료를 형성하는 단계(S500);를 포함하는 이산화티탄 복합안료 제조방법이 제공될 수 있다.1 to 6, the method for producing a titanium dioxide composite pigment according to an embodiment of the present invention largely includes the steps of (a) adding titanium dioxide to distilled water and dispersing by stirring (S100); (b) adding an aqueous solution of titanium tetrachloride and an aqueous solution of sodium hydroxide at a concentration of 10wt% to 30wt% to the dispersed titanium dioxide and stirring to proceed with titanium hydroxide coating (S200); (c) washing and filtering the white precipitate generated by standing the titanium hydroxide coated solution with distilled water (S300); (d) drying the filtered powder (S400); And, (e) forming a titanium dioxide composite pigment by sintering the titanium hydroxide composite powder at 700 ° C to 950 ° C (S500); a method for preparing a titanium dioxide composite pigment may be provided.

먼저, 증류수에 이산화티탄을 첨가하고 70℃ 내지 90℃ 온도에서 교반하여 진행한다(S100). 그리고 사염화티탄 수용액과 알칼리원으로써 10wt% 내지 30wt% 농도의 수산화나트륨 수용액을 상기 분산된 이산화티탄에 첨가하고, 70℃ 내지 90℃ 온도에서 교반하여 수산화티탄 코팅을 진행한다(S200).First, titanium dioxide is added to distilled water and stirred at a temperature of 70 ° C to 90 ° C to proceed (S100). In addition, an aqueous solution of titanium tetrachloride and an aqueous solution of sodium hydroxide having a concentration of 10 wt% to 30 wt% as an alkali source are added to the dispersed titanium dioxide, and stirred at a temperature of 70 ° C to 90 ° C to proceed with titanium hydroxide coating (S200).

그후 상기 수산화티탄 코팅이 완료된 용액을 정치시켜 발생한 백색 침전물을 증류수를 사용하여 세척하고 여과시킨다(S300). 그리고 상기 여과된 분체를 건조기에 넣고, 60℃ 내지 100℃에서 18시간 건조한다(S400).Thereafter, the white precipitate generated by standing the titanium hydroxide coated solution is washed with distilled water and filtered (S300). Then, the filtered powder is put in a dryer and dried at 60° C. to 100° C. for 18 hours (S400).

그후 상기 수산화티탄 복합 분체를 700℃ 내지 950℃에서 소결하여 산화물을 형성함으로써 이산화티탄 복합안료를 형성한다(S500).Thereafter, the titanium dioxide composite powder is sintered at 700 ° C to 950 ° C to form an oxide to form a titanium dioxide composite pigment (S500).

이때, 상기 S100 단계 내지 S400 단계 공정의 반응식은, TiO2 + TiOCl2+ 2NaOH → TiO(OH)2/TiO2 + Na+Cl- 이고, 상기 S500 단계의 공정 반응식은, TiO(OH)2 /TiO2 → TiO2 + H2O 이다.At this time, the reaction equation of the steps S100 to S400 is TiO 2 + TiOCl 2 + 2NaOH → TiO(OH) 2 /TiO 2 + Na+Cl - , and the reaction equation of the step S500 is TiO(OH) 2 / TiO 2 → TiO 2 + H 2 O.

한편, 상기와 같이 형성된 이산화티탄 복합 안료에 친수성 및 소수성 특성 부여 표면처리하는 공정은 다음과 같이 진행된다. 즉, 이하의 과정은 상기 이산화티탄 복합안료에 피막형성제를 코팅처리하는 공정에 해당한다.Meanwhile, a process of surface treatment to impart hydrophilic and hydrophobic characteristics to the titanium dioxide composite pigment formed as described above proceeds as follows. That is, the following process corresponds to a process of coating the titanium dioxide composite pigment with a film forming agent.

먼저, 상기 이산화티탄 복합 안료 90wt% 내지 98wt%와 수용성 폴리머 물질 또는 실리콘, 실란, 실리콘 공중합체를 2wt% 내지 10wt%를 헨셀믹서에 넣고 5초간 3회 분산처리를 통해 코팅을 진행한다(S600).First, 90 wt% to 98 wt% of the titanium dioxide composite pigment and 2 wt% to 10 wt% of a water-soluble polymer material or silicone, silane, or silicone copolymer are put into a Henschel mixer, and coating is performed through dispersion treatment three times for 5 seconds (S600) .

그후 상기 코팅된 분체를 60℃ 내지 100℃에서 18시간 건조한다(S700). 그리고 건조 후에는 코팅된 수용성 폴리머 또는 실리콘, 실란, 실리콘 공중합체의 영향으로 응집된 분체를 추가로 분쇄하여 친수성 내지 소수성을 부여한다(S800).Thereafter, the coated powder is dried at 60° C. to 100° C. for 18 hours (S700). After drying, the coated water-soluble polymer or powder aggregated under the influence of silicone, silane, or silicone copolymer is additionally pulverized to impart hydrophilicity or hydrophobicity (S800).

이하에서는 일반적인 무기안료와 본 발명의 일 실시예에 따른 이산화티탄 복합안료 및 그에 대한 피막 코팅을 진행한 경우를 비교한 실험결과를 설명한다.Hereinafter, experimental results comparing a general inorganic pigment with a titanium dioxide composite pigment according to an embodiment of the present invention and a case in which film coating is performed will be described.

먼저 실험 시료는 다음과 같다.First, the experimental sample is as follows.

Figure pat00001
Figure pat00001

그리고 위 실험 시료의 각각의 실험 처방은 다음과 같다.In addition, each experimental prescription of the above experimental sample is as follows.

Figure pat00002
Figure pat00002

실험 시료 중 Blank는 안료가 적용되지 않은 실험 시료이고, Control A(비교예1)는 일반적인 무기안료(CR-50)가 적용된 경우이다. Control B(비교예2)는 본 발명에 따른 이산화티탄 복합안료를 표면처리 없이 적용한 예이고, 실험 A(실험예1)는 250nm 사이즈의 이산화티탄 복합안료에 피막형성제 5%를 적용한 것이며, 실험 B(실험예2)는 160nm 사이즈의 이산화티탄 복합안료에 피막형성제 5%를 적용한 것이다.Among the experimental samples, Blank is an experimental sample to which no pigment is applied, and Control A (Comparative Example 1) is a case in which a general inorganic pigment (CR-50) is applied. Control B (Comparative Example 2) is an example in which the titanium dioxide composite pigment according to the present invention is applied without surface treatment, and Experiment A (Experimental Example 1) is an application of 5% of a film forming agent to a titanium dioxide composite pigment having a size of 250 nm. B (Experimental Example 2) is obtained by applying 5% of a film forming agent to a titanium dioxide composite pigment having a size of 160 nm.

위 시료에 대한 분산정도를 비교한 실험 이미지를 도 2 내지 도 5에 도시하였다. 도 2는 비교예1 즉, 기존의 무기안료(CR-50)을 적용한 경우인데 표면이 더글거리거나 몽글몽글 뭉치는 현상이 발생하는 것을 확인할 수 있다.Experimental images comparing the degree of dispersion for the above samples are shown in FIGS. 2 to 5. FIG. 2 is Comparative Example 1, that is, a case in which an existing inorganic pigment (CR-50) is applied, and it can be seen that a phenomenon of surface smearing or lumpy lumps occurs.

그러나 도 3의 비교예2부터 즉, 이산화티탄 복합안료를 적용한 경우에는 위와 같이 더글거리거나 뭉치는 현상이 현저히 개선되는 것을 확인할 수 있다. 특히 표면처리까지 적용한 실험예1(도 4)과 실험예2(도 5)로 갈수록 분산이 잘 구현되어 더글거림과 뭉침 현상이 거의 나타나지 않는다.However, from Comparative Example 2 of FIG. 3, that is, in the case of applying the titanium dioxide composite pigment, it can be seen that the above-described smudging or clumping phenomenon is remarkably improved. In particular, the dispersion was well realized as the surface treatment was applied to Experimental Example 1 (FIG. 4) and Experimental Example 2 (FIG. 5), so that smearing and agglomeration hardly appeared.

한편, 자외선 차단력을 비교하기 위하여 동일한 실험 시료들에 대하여 SPF(Sun Protection Factor) 및 PA(Protection Factor of UVA)지수를 측정하였으며, 그 결과를 도 6의 그래프에 도시하였다.Meanwhile, in order to compare the UV blocking power, SPF (Sun Protection Factor) and PA (Protection Factor of UVA) index were measured for the same experimental samples, and the results are shown in the graph of FIG. 6 .

도 6에서 보는 바와 같이, 본 발명의 일 실시예에 따른 이산화티탄 복합안료를 적용한 경우(Control B, 실험 A, 실험 B)가 일반적인 안료를 적용한 경우(Control A, Blank)보다 SPF 및 PA 수치가 월등히 상승한 것을 확인할 수 있다.As shown in FIG. 6, when the titanium dioxide composite pigment according to an embodiment of the present invention is applied (Control B, Experiment A, Experiment B), SPF and PA values are higher than when a general pigment is applied (Control A, Blank). It can be seen that there is a significant increase.

특히, 이러한 수치는 표면처리를 진행하고 작은 사이즈의 이산화티탄 복합안료를 적용할수록 상승에 영향을 주는 것으로 나타났다.In particular, it was found that these values affect the increase as the surface treatment proceeds and the titanium dioxide composite pigment of a small size is applied.

지금까지 설명한 본 발명의 실시예들에 의한 이산화티탄 복합안료 제조방법에 따르면, 고굴절률의 무기성 복합안료에 피막형성제를 코팅처리하는 공정을 통해 안료의 표면을 개질하여 효능을 향상시킬 수 있고, 수중유형에서의 무기성 복합안료의 분산력 향상 및 부착력 향상 그리고 지속성 향상 등의 효과를 발현시킬 수 있으며, 소비자의 사용감을 만족시키고 외관의 수분감이 높아보이는 젤 성상의 이산화티탄 복합안료를 제공할 수 있다.According to the titanium dioxide composite pigment manufacturing method according to the embodiments of the present invention described so far, the surface of the pigment can be modified through a process of coating the high refractive index inorganic composite pigment with a film forming agent to improve the efficacy, , It is possible to express effects such as improved dispersion, improved adhesion, and improved durability of inorganic composite pigments in water type, and can provide titanium dioxide composite pigments in gel form that satisfy consumers' usability and appear to have high external moisture. there is.

또한, 매끄러운 성상을 띄며 발림성이 좋고 피부 도포 시 후감이 라이트하고 산뜻하며, 제형 내에서의 분산도와 안정도가 높아짐에 따라 SPF 와 PA 수치를 상승시켜 효과적인 자외선 차단을 실현할 수 있다.In addition, it has a smooth appearance, good spreadability, and a light and refreshing aftertaste when applied to the skin, and as the degree of dispersion and stability in the formulation increases, the SPF and PA levels can be increased to realize effective sun protection.

상기에서는 본 발명의 일 실시예를 참조하여 설명하였지만, 해당 기술분야의 당업자는 이하에서 서술하는 특허청구범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경 실시할 수 있을 것이다. 그러므로 변형된 실시가 기본적으로 본 발명의 특허청구범위의 구성요소를 포함한다면 모두 본 발명의 기술적 범주에 포함된다고 보아야 한다.Although the above has been described with reference to an embodiment of the present invention, those skilled in the art variously modify and change the present invention within the scope not departing from the spirit and scope of the present invention described in the claims described below. You will be able to. Therefore, if the modified implementation basically includes the elements of the claims of the present invention, all of them should be considered to be included in the technical scope of the present invention.

Claims (7)

(a) 증류수에 이산화티탄을 첨가하고 교반하여 분산하는 단계;
(b) 사염화티탄 수용액과 10wt% 내지 30wt% 농도의 수산화나트륨 수용액을 상기 분산된 이산화티탄에 첨가하고 교반하여 수산화티탄 코팅을 진행하는 단계;
(c) 상기 수산화티탄 코팅이 완료된 용액을 정치시켜 발생한 백색 침전물을 증류수를 사용하여 세척하고 여과하는 단계;
(d) 상기 여과된 분체를 건조하는 단계; 및
(e) 상기 수산화티탄 복합 분체를 700℃ 내지 950℃에서 소결하여 이산화티탄 복합안료를 형성하는 단계;를 포함하는 이산화티탄 복합안료 제조방법.(a) dispersing by adding titanium dioxide to distilled water and stirring;
(b) adding an aqueous solution of titanium tetrachloride and an aqueous solution of sodium hydroxide having a concentration of 10wt% to 30wt% to the dispersed titanium dioxide and stirring to proceed with titanium hydroxide coating;
(c) washing and filtering the white precipitate generated by standing the titanium hydroxide-coated solution with distilled water;
(d) drying the filtered powder; and
(e) forming a titanium dioxide composite pigment by sintering the titanium hydroxide composite powder at 700 ° C to 950 ° C; 제1항에 있어서,
상기 (a) 단계 내지 (d) 단계 공정의 반응식은,
TiO2 + TiOCl2+ 2NaOH → TiO(OH)2/TiO2 + Na+Cl-
인 것을 특징으로 하는 이산화티탄 복합안료 제조방법.According to claim 1,
The reaction formulas of the steps (a) to (d) are,
TiO 2 + TiOCl 2 + 2NaOH → TiO(OH) 2 /TiO 2 + Na+Cl -
Method for producing a titanium dioxide composite pigment, characterized in that. 제1항에 있어서,
상기 (e) 단계 공정 반응식은,
TiO(OH)2 /TiO2 → TiO2 + H2O
인 것을 특징으로 하는 이산화티탄 복합안료 제조방법.According to claim 1,
The reaction equation of step (e) is,
TiO(OH) 2 /TiO 2 → TiO 2 + H 2 O
Method for producing a titanium dioxide composite pigment, characterized in that. 제1항에 있어서,
상기 이산화티탄 복합안료 90wt% 내지 98wt%와 수용성 폴리머 물질 또는 실리콘, 실란, 실리콘 공중합체 2wt% 내지 10wt%를 헨셀믹서에 넣고 분산처리하는 단계;를 더 포함하는 것을 특징으로 하는 이산화티탄 복합안료 제조방법.According to claim 1,
90wt% to 98wt% of the titanium dioxide composite pigment and 2wt% to 10wt% of a water-soluble polymer material or silicone, silane, silicone copolymer are put into a Henschel mixer and subjected to dispersion treatment; Preparing a titanium dioxide composite pigment further comprising method. 제4항에 있어서,
상기 분산처리된 분체를 건조하는 단계;를 더 포함하는 이산화티탄 복합안료 제조방법.According to claim 4,
Method for producing a titanium dioxide composite pigment further comprising the step of drying the dispersion-treated powder. 제5항에 있어서,
상기 건조된 분체를 추가 분쇄하여 친수성 또는 소수성을 부여하는 단계;를 더 포함하는 이산화티탄 복합안료 제조방법.According to claim 5,
Further pulverizing the dried powder to impart hydrophilicity or hydrophobicity; Method for producing a titanium dioxide composite pigment further comprising. 제1항 내지 제6항 중 어느 하나의 항에 의해 제조된 이산화티탄 복합안료.
A titanium dioxide composite pigment prepared by any one of claims 1 to 6.
KR1020210191922A 2021-12-30 2021-12-30 manufacturing method of titanium dioxide composite pigment and titanium dioxide composite pigment manufactured through the same KR20230104300A (en)

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US7905953B2 (en) * 2006-01-30 2011-03-15 Kronos International Inc Titanium dioxide pigment particles with doped, dense SiO2 skin and methods for their manufacture
KR100839892B1 (en) * 2006-10-30 2008-06-19 주식회사 선진화학 Method for preparing of spherical titanium dioxide powder
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CN104098932B (en) * 2013-04-15 2016-05-25 中国地质大学（北京） A kind of preparation method of white mineral-titanium dioxide composite powder pigment
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