KR20080042638A - Manufacturing method of silica gel colors composition color master - Google Patents
Manufacturing method of silica gel colors composition color master Download PDFInfo
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- KR20080042638A KR20080042638A KR1020060112035A KR20060112035A KR20080042638A KR 20080042638 A KR20080042638 A KR 20080042638A KR 1020060112035 A KR1020060112035 A KR 1020060112035A KR 20060112035 A KR20060112035 A KR 20060112035A KR 20080042638 A KR20080042638 A KR 20080042638A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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Abstract
Description
[도면]은 본 발명의 마스터베치 제조 공정도임[Drawing] is a master batch manufacturing process diagram of the present invention
도면 1 : 정량 공정도Figure 1: Quantitative Process Flow Chart
도면 2 : 투입 공정도Figure 2: Input Process Diagram
도면 3 : 혼합 공정도Figure 3: Mixing Process Diagram
도면 4 : 투입 공정도Figure 4: Input Process Diagram
도면 5 : 압출 공정도Figure 5: Extrusion Process Diagram
도면 6 : 냉각 공정도Figure 6: Cooling Process Diagram
도면 7 : 컷트 공정도Figure 7: Cut Process Diagram
도면 8 : 포장 공정도Figure 8: Packing Process Diagram
본 발명은 실리카겔 안료조성물 마스터베치 제조 방법에 관한 것으로 보다 상세하게 설명하면 현재 각종 수지 등에 기능성을 높일 수 있는 광물질이나 항균제를 이용하여 기능성 수지를 제조하는 선기술들이 개발되고 있다. 광물질분말로는 황토, 음이온광물질분말, 게르마늄, 맥반석, 세라믹, 옥, 숯 등의 분말을 플라스틱수지에 혼합하여 상기 광물질이 가지고 있는 원적외선 방출효과 또는 음이온 방출효과, 탈취 등의 기능을 얻을 수 있는 플라스틱 또는 마스터베치 형태로 제조하여 널리 사용하는 선기술들을 찾아 볼 수 있다. 특히 은(Ag)을 수지에 항균 처리하는 은항균제 제조 방법 등을 다양하게 찾아 볼 수 있다.The present invention relates to a method for producing a silica gel pigment composition masterbatch, and in more detail, current technologies for manufacturing functional resins using minerals or antimicrobial agents that can increase the functionality of various resins and the like have been developed. As the mineral powder, plastics such as ocher, anionic mineral powder, germanium, elvan, ceramic, jade, and charcoal may be mixed with the plastic resin to obtain the functions of far-infrared radiation, anion, and deodorization of the mineral. Alternatively, you can find a wide range of advanced technologies manufactured in the form of a masterbatch. In particular, silver (Ag) can be found in various ways, such as antimicrobial preparation of silver antibacterial treatment.
상기와 같이 선행기술은 대부분 은(銀)콜로이드용액을 상기 광물질분말과 수지에 혼합하여 수지 제조 공정에서 상기 기능성 분말과 은나노용액을 분산시켜 각종 기능성 수지를 제조하는 방법이 주종을 이루고 있다. 광물질분말이나 수지에 침적하면서 마스터베치 또는 수지제품을 생산했을 때 특히 은나노 입자가 수지에 고르게 분산되지 않고 특히 수지에 착염하기 위하여 안료를 사용하였을 때 수지나 광물질분말이 은나노 입자가 고르게 분산되어 있다 하여도 안료에는 항균 처리되어 있지 않아 상품에 많은 문제점이 야기되고 있다.As described above, the method of preparing various functional resins is mainly performed by dispersing the functional powder and the silver nano solution in the resin manufacturing process by mixing the silver colloidal solution with the mineral powder and the resin. When producing masterbatch or resin product by depositing on mineral powder or resin, especially silver nano particles are not evenly dispersed in resin, especially when pigment is used for complexing to resin, silver or particles are evenly dispersed. In addition, the pigment is not antibacterial treatment, causing a lot of problems in the product.
본 발명은 이러한 문제점을 해결할 수 있는 기술핵심을 살펴보면 은나노콜로이드를 증발효과를 높일 수 있고 수지나 광물질분말의 수많은 다공질 속에 상기 은나노 입자가 치환시켜 도금형태로 코팅하여 강력한 은나노 광물질 분말을 제조하는 기술을 설명하면 다음과 같다.The present invention is to look at the technical core that can solve this problem can increase the evaporation effect of silver nano colloids and the silver nano particles are replaced by a number of porous particles of resin or mineral powder coating in the form of plating to produce a strong silver nano mineral powder The explanation is as follows.
본 발명자가 이미 대한민국 특허를 등록한 특허 0399481호의 발명의 명칭 '브롬화합물을 이용한 새로운 은항균제인 은염 제조 방법' 에 관한 무기 은항균제로 방법에 제조된 은염을 이용하여 상기 은염에 과산화수소를 촉매로 하여 강력한 은항균제를 제조한 다음 은콜로이드 용액에 함유된 수분을 줄이기 위하여 에틸알코올 과 이소프로필알코올 용매로 사용하여 휘발성이 우수한 은나노 항균제를 제조하여 사용하는 데 상기 은용액에 과산화수소를 혼합했을 때 다음과 같은 메커니즘을 찾아 볼 수 있다.Inorganic silver antimicrobial agent related to 'Method for producing silver salt, a new silver antimicrobial agent using bromine compound,' which the inventors have already registered a Korean patent, has a strong effect of hydrogen peroxide on the silver salt as a catalyst. In order to reduce the moisture contained in the silver colloidal solution, the silver antibacterial agent is used as a solvent of ethyl alcohol and isopropyl alcohol to prepare a highly volatile silver nano antimicrobial agent, and when hydrogen peroxide is mixed with the silver solution, Can be found.
과산화수소와 은용액이 결합할 경우 active oxygen compounds이 발생되고 다른 점은 은과 과산화수소 분자 간의 상호작용의 힘에 의해 radical와 anion은 강력한 운동에너지(kine energy)을 갖게 된다. 그래서 과산화수소보다 10∼100배 강하게 세포벽을 통과하게 되고 음전하(anion)를 띤 -O-O-H도 높아진 운동에너지로 세포벽을 파괴할 수 있다.When oxygen peroxide and silver solution combine, active oxygen compounds are generated. The difference is that radical and anion have strong kine energy due to the interaction between silver and hydrogen peroxide molecules. Therefore, it passes through the cell wall 10 to 100 times stronger than hydrogen peroxide, and negatively charged -O-O-H also can destroy the cell wall with higher kinetic energy.
상기와 같이 제조된 은용액은 살균력이 우수하고 수지나 광물질분말에 침지될 경우 건조효과와 침투력이 우수한 것을 확인할 수 있다.The silver solution prepared as described above has excellent sterilizing power and can be confirmed to have excellent drying effect and penetration power when immersed in resin or mineral powder.
탈취력이 우수한 실리카겔은 투명과 반투명 입자로 되어 있는데 본 발명은 투명 실리카겔을 사용하는 것이 바람직하다. 상기 결정은 실리카겔 1g이 150㎡ 이상 표면적을 가지고 있고 아황산가스의 흡착력과 수분 흡착력이 좋고 저온일수록 효과는 더욱 크다. 상기 실리카겔을 분쇄한 분말에 기능성 광물질분말(게르마늄, 토르말린, 맥반석, 옥 등) 50%로 혼합 믹스하여 건조하면 PH8.5정도의 약 알칼리 용액을 얻을 수 있다.Silica gel having excellent deodorizing power is composed of transparent and semi-transparent particles, but the present invention preferably uses transparent silica gel. 1g of silica gel has a surface area of 150 m 2 or more, the better the adsorption power and the water adsorption power of sulfurous acid gas, and the lower the temperature, the greater the effect. When the silica gel is pulverized, mixed with 50% functional mineral powder (germanium, tourmaline, elvan, jade, etc.) and dried, a weak alkaline solution having a pH of about 8.5 can be obtained.
상기 분말에 은나노 입자를 흡착시키면 광물질분말의 수많은 다공질 속의 내부와 외부에 도금형태로 은이 이온화되어 마찰이나 세척에도 떨어지지 않는 항균력이 우수한 기능성 은나노 항균 광물질을 얻을 수 있다. 특히 실리카겔의 수많은 다공질속에 은나노 입자가 코팅되었을 때 항균 및 살균효과가 있는 것을 확인할 수 있다. 상기 분말을 제조한 다음 PE수지 또는 마스터베치 제조 수지에도 은나노용액을 침지시켜 은나노 항균 수지를 제조한 다음 상기 수지 1,000g 비율에 상기 은나노 실리카겔분말 200g을 혼합하여 본 발명의 기능성 마스터베치를 제조하는 것이 특징이다.When the silver nanoparticles are adsorbed on the powder, silver is ionized in the form of plating on the inside and the outside of numerous porous particles of the mineral powder, thereby obtaining a functional silver nano antibacterial mineral having excellent antimicrobial power that does not drop even in friction or washing. In particular, it can be seen that the antimicrobial and bactericidal effects are obtained when silver nanoparticles are coated in numerous porous layers of silica gel. After preparing the powder, the silver nano solution was also immersed in a PE resin or a master beet resin to prepare a silver nano antimicrobial resin, and then the silver nano silica gel powder was mixed in a ratio of 1,000 g of the resin to prepare the functional master bezel of the present invention. It is characteristic.
상기와 같이 마스터베치를 제조하여 필름을 제조했을 때 식품포장지 또는 농업용 온상 필름을 사용하거나 차일막 PP수지사 등을 제조했을 때 비닐에 결뢰현상이 일어나지 않고 각종 항균, 원적외선, 음이온 기능성 수지를 제조할 수 있는 것이 특징이다When manufacturing a film by manufacturing the master bezel as described above, when using a food wrapping paper or agricultural hot-bed film, or when manufacturing a child film PP resin, etc., it is possible to produce various antibacterial, far-infrared, anionic functional resins without the occurrence of a binder phenomenon in vinyl. It is characterized by being
종래의 선기술들을 살펴 볼 것 같으면 다음과 같다.Looking at the conventional prior art is as follows.
인용특허 1. 특허등록 번호 10-0582464호
발명의 명칭: 은콜로이드용액을 수지 원료 칩에 항균 처리하는 방법Name of invention: Method of antimicrobial treatment of silver colloidal solution on resin raw material chip
인용특허 2. 특허등록 번호 10-0629114호Cited Patent 2. Patent Registration No. 10-0629114
발명의 명칭 : 은이온 항균마스타베치 제조 방법Name of invention: Silver ion antibacterial masterbatch production method
인용특허 3. 특허공개 번호 2001-0089042호
발명의 명칭 : 광물을 첨가한 기능성 섬유 제조 방법 및 이로부터 제조된 섬 유Name of the Invention: Method for preparing functional fiber with minerals and fiber prepared therefrom
상기 인용 특허 1, 2번은 본 발명자가 받은 특허로서 본 발명에서는 상기 기술 일부를 응용하면서 그 기술의 목적과 효과를 높이는 방법의 기술을 제공한 것이 특징이다. 또한 인용 특허 3번은 다양한 광물질을 사용하고 있으나 상기 광물질은 대부분 원적외선을 방출하는 기능을 가지고 있고 본 발명에서 사용 목적으로 목적을 달성하기 위한 음이온, 실리카겔의 기능과 새로운 은콜로이드를 제조하여 다양한 기능을 얻을 수 있는 기능성 마스터베치 제조방법과는 효능과 목적의 기술에 차이가 있다고 볼 수 있다.The above-cited
항균, 탈취, 제습, 음이온, 원적외선 기능을 얻을 수 있는 기능성 마스터베치를 제조하여 각종 수지 제품에 보다 효율적인 효과를 얻을 수 있는 기능성 마스터베치 제조 기술을 제공할 수 있는 것이 본 발명이 이루고자하는 기술 과제의 목적이다.It is possible to provide a functional masterbatch manufacturing technology capable of producing more effective effects on various resin products by manufacturing a functional masterbatch capable of obtaining antibacterial, deodorizing, dehumidifying, anion, and far infrared rays. Purpose.
본 발명여의 실리카겔 및 기능성 광물질 안료조성물을 이용한 은나노 마스터베치 제조 및 그 방법에 있어서 상세하게 설명하면 다음과 같다.Hereinafter, a detailed description will be given of a silver nano masterbatch using the silica gel and the functional mineral pigment composition of the present invention and a method thereof.
[실시예1]Example 1
제1공정1st process
은지금 200g을 용해조에 넣고 열을 주면서 질산을 첨가시켜 은을 용해하면 280㎖의 질산이 소모된다. 또한 염화제1석 100g을 염산 100㎖에 녹여 상기 은용액 에 합성 교반한다. 상기 은용액을 PH를 중성으로 조절하기 위하여 가성소다용액(PH13) 500g에 산화아연 150g을 용해하여 상기 은용액과 합성하면서 PH7.5가 되게 하여 수분을 증발시켜 분말파우더의 은염을 얻는다. 상기 은염 150g을 에틸알코올 500㎖와 이소프로필알코올 350㎖에 혼합 믹스하여 분해시키면서 브롬소오다 3g을 넣고 용해한 은용액을 유리비커에 넣고 밀폐시킨 다음 햇볕에 3시간 동안 노출시켜 24시간 후 산화물을 여과하여 알코올형 은나노콜로이드 제조 공정Now, 200 g of silver is added to the dissolving bath and nitric acid is added while heating to dissolve silver. This consumes 280 ml of nitric acid. Further, 100 g of stannous chloride is dissolved in 100 ml of hydrochloric acid, and then synthesized and stirred in the silver solution. In order to adjust the silver solution to neutral pH, 150g of zinc oxide was dissolved in 500g of caustic soda solution (PH13), and synthesized with the silver solution to make PH7.5 to evaporate water to obtain silver salt of powder powder. 150 g of the silver salt was mixed with 500 ml of ethyl alcohol and 350 ml of isopropyl alcohol, and then decomposed. 3 g of bromine was added. The dissolved silver solution was placed in a glass beaker, sealed, exposed to sun for 3 hours, and the oxide was filtered after 24 hours. Alcohol type silver nano colloid manufacturing process
제2공정2nd process
실리카겔을 분쇄한 분말 500g 비율에 토르말린분말 200g, 게르마늄분말 100g, 맥반석 100g, 옥분말 100g, 안료 500g을 혼합 믹스하여 1,000g을 제조하는 공정Process of preparing 1,000 g by mixing and mixing 200 g of tourmaline powder, 100 g of germanium powder, 100 g of ganbanite, 100 g of jade powder, and 500 g of pigment in a 500 g ratio of pulverized silica gel.
제3공정3rd process
가성소오다용액 (PH8.5) 1,000g을 제2공정의 안료조성물 1,000g에 완전히 침지시킨 다음 90℃의 열을 유지하면서 상기 분말을 건조시켜 분쇄한 분말 1,000g을 제조하는 공정1,000 g of caustic soda solution (PH8.5) is completely immersed in 1,000 g of the pigment composition of the second step, followed by drying the powder while maintaining the heat at 90 ° C. to prepare 1,000 g of the ground powder.
제4공정4th process
제1공정의 은용액 500g을 제3공정의 안료조성물 1,000g 스텐통에 넣고 완전히 은용액이 침지되도록 교반하면 은이 안료조성물 알칼리염과 이온화되어 도금형태로 코팅된다. 상기 분말을 90℃의 열을 유지하면서 건조하여 다시 분쇄하여 은나노 안료조성물 제조하는 공정500 g of the silver solution of the first step is put into the 1,000 g of the pigment composition of the third step and stirred to completely immerse the silver solution. The silver is ionized with the alkali salt of the pigment composition and coated in a plating form. Drying the powder while maintaining the heat of 90 ℃ to grind again to prepare a silver nano pigment composition
제5공정5th process
가성소오다용액(PH8.5) PE수지 1,000g을 침지시켜 건조하여 약 알칼리 PE수지를 제조하는 공정Process of manufacturing weak alkaline PE resin by dipping 1,000 g of caustic soda solution (PH8.5) PE resin
제6공정6th process
제1공정의 은용액 500g을 제5공정의 PE수지에 침지시키면 은나노 입자가 이온화 형태로 PE수지에 코팅하는 공정When 500g of the silver solution of the first step is immersed in the PE resin of the fifth step, the silver nanoparticles are coated on the PE resin in an ionized form.
제7공정7th process
제4공정의 안료조성물 300g 비율에 제 6공정의 PE수지 1,000g을 마스터베치 제조 공정 도면에 따라 설명하면 상기 PE수지를 도면 정량 공정(1)에서 1,000g을 정량한 다음 투입공정(2)으로 수지조성물을 투입한 다음 혼합공정(3)에서 고르게 혼합한 다음 일정한 양을 투입공정(4)에서 압출공정(5)으로 압출된 수지가 냉각공정(6)을 거쳐 일정한 규격으로 약 길이 3mm, 직경 2mm 정도로 컷트공정(7)에서 본 발명의 마스터베치 칩이 제조되어 포장공정(8)에서 포장되는 실리카겔분말 및 광물질 안료조성물 은나노 마스터베치를 제조하는 방법이 특징이다.When the 1,000 g of the PE resin of the sixth process is described according to the master batch manufacturing process drawing in the ratio of 300 g of the pigment composition of the fourth process, the PE resin is quantified in the drawing quantification process (1), and then the feeding process (2) is performed. After the resin composition was added, the mixture was evenly mixed in the mixing process (3), and then a predetermined amount was added to the extrusion process (5) in the extrusion process (5). Masterbatch chips of the present invention are prepared in the cutting process (7) to about 2mm, characterized in that the silica gel powder and the mineral pigment composition silver nano masterbatch to be packed in the packaging process (8).
상기와 같이 제조된 마스터베치를 항균검사와 음이온, 원적외선 방출 시험을 테스트한 결과는 다음과 같다.The results of testing the antimicrobial test and anion, far-infrared emission test prepared as described above is as follows.
〈 항균시험 결과 〉〈Antibacterial Test Results〉
〈원적외선 시험 결과〉<Far infrared ray test result>
〈음이온 시험 결과)<Anion test results)
상기와 같이 항균시험 테스트 결과 대장균과 황색포도상구균이 48시간 후 세균감소율이 99.9%되는 것을 확인할 수 있고 음이온이 공기 1cc당 520정도 방출되고 원적외선이 0.90%정도 우수한 기능이 방출되는 것을 확인할 수 있다.As described above, as a result of the antibacterial test test, E. coli and Staphylococcus aureus can confirm that the bacterial reduction rate is 99.9% after 48 hours, and anion is released about 520 per 1cc of air, and far infrared rays are about 0.90%.
상기와 같이 제조된 본 발명의 기능성 마스터베치로 각종 수지 등을 제조했을 때 기존 수지에서 찾아 볼 수 없는 항균, 탈취, 제습, 음이온, 원적외선 등의 기능효과가 있는 수지를 제공받을 수 있는 것이 특징이다.When manufacturing a variety of resins, such as the functional masterbatch of the present invention prepared as described above is characterized in that it can be provided with a resin having a functional effect such as antibacterial, deodorant, dehumidification, anion, far-infrared rays not found in existing resin .
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CN114231146A (en) * | 2021-12-22 | 2022-03-25 | 广东溢达纺织有限公司 | Impregnation slurry, impregnation rope end and preparation method thereof |
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CN114231146A (en) * | 2021-12-22 | 2022-03-25 | 广东溢达纺织有限公司 | Impregnation slurry, impregnation rope end and preparation method thereof |
CN114231146B (en) * | 2021-12-22 | 2022-10-18 | 广东溢达纺织有限公司 | Impregnation slurry, impregnation rope end and preparation method thereof |
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