WO2013187549A1 - Method for measuring mixing ratio of cellulose-based fiber mixed product using chemical carbonization method - Google Patents

Method for measuring mixing ratio of cellulose-based fiber mixed product using chemical carbonization method Download PDF

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WO2013187549A1
WO2013187549A1 PCT/KR2012/005006 KR2012005006W WO2013187549A1 WO 2013187549 A1 WO2013187549 A1 WO 2013187549A1 KR 2012005006 W KR2012005006 W KR 2012005006W WO 2013187549 A1 WO2013187549 A1 WO 2013187549A1
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cellulose
measuring
mixing ratio
sample
based fiber
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PCT/KR2012/005006
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French (fr)
Korean (ko)
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김영률
이상락
양중식
진성룡
문형준
서용환
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한국섬유기술연구소
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/36—Textiles
    • G01N33/367—Fabric or woven textiles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/36—Textiles

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  • the present invention relates to a method of measuring the mixing ratio of a cellulosic fiber mixed product using a carbonization method, and more specifically, to a method of measuring the mixing rate by carbonizing only a cellulose-based fiber after immersing a sample of a cellulosic fiber mixed product in a carbonization composition. It is about.
  • Fiber mixing rate refers to the weight percentage of each composition fiber relative to the total composition of the product in which the two or more fibers are mixed. At present, it is compulsory to attach fiber labeling information to all garments under the Industrial Products Quality Control Act. Since the price of apparel products is determined by the specific material content, fiber blending is recognized as an important factor in determining the price, performance and quality of the product.
  • the fiber mixing rate is an essential test item when testing and inspecting textile products, and the test demand is very high, and high accuracy of the measurement result is required.
  • a sample including a yarn constituting one unit of a design is taken from a fiber product in which tissues knitted or composed of different kinds of fibers are knitted.
  • KS K 0210 5. Mechanical Separation Method
  • the dissolution method discriminates the composition of the mixed product, dissolves one of the compositions with the selected solution, weighs the remaining amount, calculates the ratio of the dissolved composition in the weight loss component, and dissolves the fiber of the larger one first.
  • Microscopy is used for products with mixed fibers to which neither the mechanical separation method nor the dissolution method can be applied.
  • the dissolution method is used, and the soluble fibrous material is natural fiber such as cellulose, protein (wool, silk, etc.), cellulose is a high concentration of sulfuric acid solution, and protein is sodium hydroxide solution. It is dissolved by using a water bath or heating. In addition, an aqueous sulfuric acid solution or an aqueous sodium hydroxide solution is also used at the time of washing.
  • KS K 0210 (6.2.2 70% Sulfuric Acid Method) can be summarized.
  • 70% sulfuric acid at 23 ⁇ 25 °C is added at a rate of 100 ml per 1g of sample.
  • Shake for about 10 minutes filter by suction with a crucible filter, collect the residue, wash with 70% sulfuric acid and water at the same temperature as before dissolving, neutralize with 50 times of 1% ammonia, and suction filter with a crucible filter.
  • the process of measuring the mixing rate of a cellulose fiber by washing with water, drying the residue, cooling, and measuring the weight is disclosed.
  • KS K 0210 6.2.12 5% Sodium Hydroxide Method
  • KS K 0210 6.2.12 5% Sodium Hydroxide Method
  • the contents of KS K 0210 can be summarized as follows.Put the specimen in a beaker, add 5% sodium hydroxide solution at a rate of 50 ml per 1 g of specimen, and stir for 15 minutes in boiling water After dissolving the wool or silk, filtration by suction with a crucible filter, the residue is collected, washed with warm water, neutralized with 2% hydrochloric acid dilution, suction filtration with a crucible filter, washed with water, dried and cooled. The process of measuring the mixing rate of protein fiber by measuring the weight is published.
  • the present inventors have studied and tried to develop a method for accurately measuring the mixing ratio of a cellulosic fiber mixed product in a short time without using a high concentration of an acid solution, and as a result, in a carbonizing composition comprising a metal salt, a thickener and an overdrying agent After immersing the sample, the present invention was completed by discovering that only the cellulose fibers can be carbonized and removed by heat treatment, so that the mixing ratio can be measured by changing the weight.
  • an object of the present invention is to provide a method for measuring the mixing ratio by immersing a sample in a carbonizing composition comprising a specific metal salt, a thickener and an anti-drying agent and confirming the weight change by heat treatment.
  • a carbonization composition comprising a metal salt, a thickener and an anti-drying agent
  • Characterized by the method of measuring the mixing rate of the cellulosic fiber mixed product comprising the step of washing and drying the heat-treated sample, and measuring the weight.
  • the mixing rate measuring method of the present invention is simple and simple, and can process a large amount of samples in a short time.
  • the method does not dissolve the target fiber using a solvent or use harmful substances such as strong acid or strong alkali, the test can be conducted in an environmentally friendly manner, and its accuracy is also excellent, and it is widely used in the textile industry for fast and accurate results.
  • 1 is a process chart according to the mixing rate measuring method of the cellulosic fiber mixed products of the present invention.
  • Figure 2 shows that the carbonization composition is added to the cellulose-based fiber and heat treated, (a) is cotton, (b) is lyocell, (c) is modal and (d) is viscose rayon.
  • Example 3 is a photograph before treatment of the multi-island textile fabric used in Example 3.
  • Figure 4 is a photograph after the heat treatment after adding the carbonizing composition to the multi-island teaching fabric.
  • FIG. 5 is a photograph after heat treatment of a multi-island textile fabric and washing with water.
  • the carbonizing composition includes a metal salt, a thickener and an anti-drying agent, and is used for immersion of the sample in a volume of preferably 0.5 to 2.0 ml, more preferably 0.7 to 1.0 ml with respect to 1 g of the sample.
  • the metal salt may be one or a mixture of two or more selected from aluminum sulfate, sodium hydrogen sulfite and ferric sulfate, and the compound is preferably used in the form of a hydrate, more preferably aluminum sulfate hydrate is used. It is good to be.
  • the metal salt is preferably 20 to 80% by weight, preferably 30 to 70% by weight, more preferably 40 to 60% by weight in the total carbonization composition.
  • the thickener may be a compound well known in the art that can control the viscosity, preferably one selected from guar gum, tara gum and carboxy methyl cellulose. Mixtures of two or more may be used.
  • the thickener is preferably 10 to 50% by weight, preferably 20 to 40% by weight in the total carbonization composition.
  • the thickening agent is adjusted to prepare a carbonizing composition having a viscosity of about 1,000 to 10,000 cps.
  • the anti-drying agent is used to prevent excessive carbonization of the fabric by over-drying, glycerin, polyethylene glycol may be used.
  • the anti-drying agent may be used 1 to 30% by weight, preferably 5 to 20% by weight in the total carbonization composition.
  • the carbonizing composition may include a penetrant, an antifoaming agent, and other additives, the content of which may be appropriately adjusted by those skilled in the art.
  • the carbonizing composition is preferably in the range of pH 1-4, more preferably in the range of pH 1-2 is more advantageous for the carbonization of cellulose-based fibers.
  • the dried sample obtained by drying in an oven and having a dry weight (M1) measured is immersed in the carbonizing composition to allow the carbonizing composition to penetrate the sample. At this time, it is preferable to go through the padding process so that the composition is more easily penetrated.
  • the padding may be made so that the pick-up rate is 60 to 100%, preferably 70 to 90%, and is made using a padder, a ringer, or the like, which is generally used in the art. Can be.
  • the composition for carbonization After allowing the composition for carbonization to penetrate the sample through the above process, it is carbonized by heat treatment (S3).
  • the heat treatment is preferably performed for about 1 to 5 minutes, more preferably about 2 to 3 minutes at 120 ⁇ 200 °C, preferably 150 ⁇ 170 °C.
  • the heat treatment may be performed through a heat transfer machine or a hot air dryer, which are widely used in the art, and the cellulose fiber is carbonized to produce ash by the heat treatment process.
  • the ash produced by washing the carbonized sample with running water or the like is removed, and preferably, the ash is removed using a mesh having a pore size of 150 ⁇ m or less. After the carbonized ash is removed and the remaining sample is dried for 10 to 20 minutes in an oven 100 ⁇ 120 °C and measure the dry weight (M2) of the dried sample (S4).
  • the mixing ratio of the cellulose-based fiber mixed product may be calculated using the dry weight (M1) and the dry weight (M2) of the final sample before treatment, and the formula 1 shows a method of calculating the mixing ratio.
  • Cotton, lyocell, modal and viscose rayon samples of cellulose fiber materials were immersed in the carbonizing composition, and then heat-treated at 160 ° C. for 5 minutes.
  • the carbonized form according to the heat treatment is shown in FIG. 2, and as shown in FIG. 2, the cellulose-based fiber was confirmed to be carbonized by the penetration and heat treatment of the carbonization composition.
  • the multi-island textile fabric including six fibers was immersed in the carbonization composition of Example 1, and then heat-treated at 160 ° C. for 5 minutes.
  • FIG. 4 The shape of the heat-treated multi-island textile fabric is shown in FIG. 4, and the result of washing with flowing water is shown in FIG. 5.
  • the cotton fabric is carbonized by the heat treatment and washing with water, and the cotton fabric is removed by washing with water, but the other fabrics remain as it is.
  • the mixing rate measuring method of the present invention is simple and simple, and can process a large amount of samples in a short time.
  • the method does not dissolve the target fiber using a solvent or use harmful substances such as strong acid or strong alkali, the test can be conducted in an environmentally friendly manner, and its accuracy is also excellent, and it is widely used in the textile industry for fast and accurate results.

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Abstract

The present invention relates to a method for measuring the mixing ratio of a cellulose-based fiber mixed product using a chemical carbonization method, and more particularly, to a method for measuring the mixing ratio by immersing a cellulose-based fiber mixed product sample in a carbonization composition and then heat-treating same to carbonize only the cellulose-based fiber. The method for measuring the mixing ratio of the present invention is simple, convenient, and can treat multiple samples within a short period of time. Also, the method does not dissolve the target fiber by using a solvent or harmful substances such as strong acid, and thus testing can be eco-friendly and yield high accuracy. Accordingly, the method can have a wide range of applications in the fiber industry where accurate results are desired in a swift manner.

Description

화학적 탄화법을 이용한 셀룰로스계 섬유 혼용제품의 혼용률 측정방법Method for Measuring the Mixing Rate of Cellulose Fiber Blended Products Using Chemical Carbonization
본 발명은 탄화법을 이용한 셀룰로스계 섬유 혼용제품의 혼용률 측정방법에 관한 것으로서, 보다 구체적으로 셀룰로스계 섬유 혼용제품 시료를 탄화용 조성물에 침지한 후 열처리하여 셀룰로스계 섬유만을 탄화시킴으로써 혼용률을 측정하는 방법에 관한 것이다.The present invention relates to a method of measuring the mixing ratio of a cellulosic fiber mixed product using a carbonization method, and more specifically, to a method of measuring the mixing rate by carbonizing only a cellulose-based fiber after immersing a sample of a cellulosic fiber mixed product in a carbonization composition. It is about.
섬유 혼용률이란 2가지 이상의 섬유가 혼용된 제품의 전체 조성에 대한 각 조성 섬유의 중량 백분율을 의미한다.　 현재 국내에서는 공산품 품질관리법에 따라 모든 의류에 섬유 혼용률에 대한 정보를 조성섬유표시(Fiber label)로 부착하여 첨부하도록 의무화되어 있다. 특정 소재 함량에 따라 의류 제품의 가격이 결정되므로 섬유 혼용률은 제품의 가격, 성능 및 품질을 결정짓는 중요 요소로 인식되고 있다. Fiber mixing rate refers to the weight percentage of each composition fiber relative to the total composition of the product in which the two or more fibers are mixed. At present, it is compulsory to attach fiber labeling information to all garments under the Industrial Products Quality Control Act. Since the price of apparel products is determined by the specific material content, fiber blending is recognized as an important factor in determining the price, performance and quality of the product.
따라서 섬유제품의 시험, 검사시 섬유 혼용률은 필수적인 시험항목으로서 시험 수요가 매우 크며, 그 측정 결과에 대한 높은 정확도가 요구되고 있다. Therefore, the fiber mixing rate is an essential test item when testing and inspecting textile products, and the test demand is very high, and high accuracy of the measurement result is required.
현재 상기 섬유 혼용률을 측정하는 방법으로서 기계적 분리법, 용해법, 현미경법 등이 알려져 있다. Currently, mechanical separation, dissolution, microscopy and the like are known as methods for measuring the fiber content.
먼저, 기계적 분리법은 섬유종류가 다른 실로 짠 조직이 편성 또는 구성되어 있는 섬유제품에서 의장 1단위를 구성하는 실을 포함한 시료를 채취하고, 이것을 풀어서 섬유 종류별로 실을 분리한 다음 실의 무게를 백분율로 나타내는 방법이다(KS K 0210, 5. 기계적 분리법).First, in the mechanical separation method, a sample including a yarn constituting one unit of a design is taken from a fiber product in which tissues knitted or composed of different kinds of fibers are knitted. (KS K 0210, 5. Mechanical Separation Method).
다음, 용해법은 혼용제품의 조성을 감별한 후, 선택한 용액으로 한쪽의 조성을 용해하여 잔여분의 무게를 측정하고, 용해한 조성의 비율은 감량분에서 계산하며 보통 비율이 큰 쪽의 섬유를 먼저 용해한다(KS K 0210, 6. 용해법).Next, the dissolution method discriminates the composition of the mixed product, dissolves one of the compositions with the selected solution, weighs the remaining amount, calculates the ratio of the dissolved composition in the weight loss component, and dissolves the fiber of the larger one first. K 0210, 6. Dissolution method).
상기 기계적 분리법 및 용해법 어느 쪽의 시험방법도 적용할 수 없는 섬유 혼용 제품에는 현미경법을 사용한다. Microscopy is used for products with mixed fibers to which neither the mechanical separation method nor the dissolution method can be applied.
상기 방법 중 일반적으로는 용해법을 사용하고 있으며, 주로 용해되는 섬유소재는 셀룰로스계, 단백질계(양모, 견 등)등의 천연섬유계로서 셀룰로스계는 고농도의 황산 수용액, 단백질계는 수산화나트륨 수용액을 사용하여 중탕 또는 가열함으로써 용해한다. 또한, 수세시에도 황산 수용액이나 수산화나트륨 수용액을 사용하게 된다. Generally, the dissolution method is used, and the soluble fibrous material is natural fiber such as cellulose, protein (wool, silk, etc.), cellulose is a high concentration of sulfuric acid solution, and protein is sodium hydroxide solution. It is dissolved by using a water bath or heating. In addition, an aqueous sulfuric acid solution or an aqueous sodium hydroxide solution is also used at the time of washing.
보다 구체적으로 KS K 0210 (6.2.2 70% 황산법)에 게시된 내용을 요약하면, 마개가 부착된 삼각플라스크에 시료 1g당 100㎖의 비율로 23 ~ 25℃의 70% 황산을 넣어 진탕기에서 약 10분간 흔들어주고, 도가니형 필터로 흡인 여과 후, 잔여분을 수집하며, 용해전과 동일한 온도의 70% 황산 및 물로 수세하고, 50배량의 1% 암모니아로 중화한 후, 도가니형 필터로 흡인 여과 후 물로 수세하여 잔여분 건조, 냉각 후, 무게를 측정함으로써 셀룰로스계 섬유의 혼용률을 측정하는 과정이 게시되어 있다. More specifically, the contents of KS K 0210 (6.2.2 70% Sulfuric Acid Method) can be summarized. In a shaker-type Erlenmeyer flask, 70% sulfuric acid at 23 ~ 25 ℃ is added at a rate of 100 ml per 1g of sample. Shake for about 10 minutes, filter by suction with a crucible filter, collect the residue, wash with 70% sulfuric acid and water at the same temperature as before dissolving, neutralize with 50 times of 1% ammonia, and suction filter with a crucible filter. The process of measuring the mixing rate of a cellulose fiber by washing with water, drying the residue, cooling, and measuring the weight is disclosed.
또한 KS K 0210 (6.2.12 5% 수산화나트륨법)에 게시된 내용을 요약하면, 시험편을 비이커에 넣고 시험편 1g당 50㎖의 비율로 5% 수산화나트륨 용액을 넣어 끓는 물 속에서 15분간 저어서 양모 또는 견을 용해시키며, 도가니형 필터로 흡인 여과 후, 잔여분을 수집하고, 따뜻한 물로 수세하고, 2% 염산 희석액으로 중화하며, 도가니형 필터로 흡인 여과 후 물로 수세하여 잔여분을 건조, 냉각 후, 무게를 측정함으로써 단백질계 섬유의 혼용률을 측정하는 과정이 게시되어 있다.　 In addition, the contents of KS K 0210 (6.2.12 5% Sodium Hydroxide Method) can be summarized as follows.Put the specimen in a beaker, add 5% sodium hydroxide solution at a rate of 50 ml per 1 g of specimen, and stir for 15 minutes in boiling water After dissolving the wool or silk, filtration by suction with a crucible filter, the residue is collected, washed with warm water, neutralized with 2% hydrochloric acid dilution, suction filtration with a crucible filter, washed with water, dried and cooled. The process of measuring the mixing rate of protein fiber by measuring the weight is published.
그러나 이와 같이 고농도의 산, 알칼리 용액을 중탕, 가열함에 따라 냄새가 발생하고, 약제 취급의 관리 및 위험으로 인하여 시험 환경이 매우 열악하며, 처리 시간이 길고 한번에 많은 양의 시료 처리가 불가능한 문제가 있었다. 또한, 타 섬유가 용해될 가능성이 있어서 그 측정 결과의 신뢰성에도 문제가 있을 수 있다.However, there is a problem that odor is generated by heating and heating a high concentration of acid and alkaline solution, and the test environment is very poor due to the management and risk of drug handling, and the processing time is long and it is impossible to process a large amount of samples at one time. . In addition, there is a possibility that other fibers are dissolved, there may be a problem in the reliability of the measurement results.
따라서 단순하고 간편한 방법으로, 짧은 시간 내에 정확하면서도 환경친화적으로 시험을 진행할 수 있는 새로운 섬유 혼용률의 측정방법 개발이 요구되는 실정이다. Therefore, there is a need for a new and simple method for measuring the blending rate of the fiber, which can be carried out in a simple and convenient manner in a short time with accurate and environmentally friendly tests.
이에 본 발명자들은 고농도의 산 용액을 사용하지 아니하면서도 짧은 시간 내에 정확하게 셀룰로스계 섬유 혼용제품의 혼용률을 측정하는 방법을 개발하고자 연구, 노력한 결과, 금속염, 증점제 및 과건조방지제를 포함하는 탄화용 조성물에 시료를 침지한 후, 열처리하면 셀룰로스계 섬유만이 탄화되어 제거될 수 있어, 중량의 변화를 통하여 혼용률을 측정할 수 있음을 발견함으로써 본 발명을 완성하게 되었다.　 Accordingly, the present inventors have studied and tried to develop a method for accurately measuring the mixing ratio of a cellulosic fiber mixed product in a short time without using a high concentration of an acid solution, and as a result, in a carbonizing composition comprising a metal salt, a thickener and an overdrying agent After immersing the sample, the present invention was completed by discovering that only the cellulose fibers can be carbonized and removed by heat treatment, so that the mixing ratio can be measured by changing the weight.
따라서 본 발명은 특정 금속염, 증점제 및 과건조방지제를 포함하는 탄화용 조성물에 시료를 침지하고 열처리하여 중량 변화를 확인함으로써 혼용률을 측정할 수 있는 방법을 제공하는 것을 그 목적으로 한다. Therefore, an object of the present invention is to provide a method for measuring the mixing ratio by immersing a sample in a carbonizing composition comprising a specific metal salt, a thickener and an anti-drying agent and confirming the weight change by heat treatment.
본 발명은, The present invention,
셀룰로스계 섬유가 혼용된 시료를 건조시키고, 시료의 처리전 중량을 측정하는 단계;Drying a sample in which cellulosic fibers are mixed, and measuring a weight before processing the sample;
금속염, 증점제 및 과건조방지제를 포함하는 탄화용 조성물에 상기 시료를 침지하는 단계; Immersing the sample in a carbonization composition comprising a metal salt, a thickener and an anti-drying agent;
상기 침지된 시료를 열처리하는 단계; 및Heat treating the immersed sample; And
열처리된 시료를 수세 및 건조시키고, 중량을 측정하는 단계를 포함하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법을 그 특징으로 한다.Characterized by the method of measuring the mixing rate of the cellulosic fiber mixed product comprising the step of washing and drying the heat-treated sample, and measuring the weight.
본 발명의 혼용률 측정방법은 단순하고 간편하면서도, 짧은 시간 내 많은 양의 시료를 처리할 수 있다. 또한, 상기 방법은 용제를 사용하여 대상 섬유를 용해하거나, 강산, 강알칼리 등의 유해 물질을 사용하지 않으므로 친환경적으로 시험을 진행할 수 있으며, 그 정확도 역시 우수한 바, 신속하고 정확한 결과를 원하는 섬유 업계에서 널리 적용될 수 있을 것이다. The mixing rate measuring method of the present invention is simple and simple, and can process a large amount of samples in a short time. In addition, since the method does not dissolve the target fiber using a solvent or use harmful substances such as strong acid or strong alkali, the test can be conducted in an environmentally friendly manner, and its accuracy is also excellent, and it is widely used in the textile industry for fast and accurate results. Could be applied.
도 1은 본 발명의 셀룰로스계 섬유 혼용제품의 혼용률 측정방법에 따른 공정도이다. 1 is a process chart according to the mixing rate measuring method of the cellulosic fiber mixed products of the present invention.
도 2는 셀룰로스계 섬유에 탄화용 조성물을 가하고 열처리한 것을 나타낸 것으로, (a)는 면, (b)는 리오셀, (c)는 모달 및 (d)는 비스코스 레이온을 나타낸다. Figure 2 shows that the carbonization composition is added to the cellulose-based fiber and heat treated, (a) is cotton, (b) is lyocell, (c) is modal and (d) is viscose rayon.
도 3은 실시예 3에서 사용된 다섬 교직포의 처리전 사진이다. 3 is a photograph before treatment of the multi-island textile fabric used in Example 3.
도 4는 다섬 교직포에 탄화용 조성물을 가하고 열처리한 후의 사진이다. Figure 4 is a photograph after the heat treatment after adding the carbonizing composition to the multi-island teaching fabric.
도 5는 다섬 교직포를 열처리하고, 물로 수세한 후의 사진이다.5 is a photograph after heat treatment of a multi-island textile fabric and washing with water.
본 발명의 이점 및 특징, 그리고 그것들을 달성하는 방법은 상세하게 후술되어 있는 실시 예들을 참조하면 명확해질 것이다. 그러나, 본 발명은 이하에서 게시되는 실시 예들에 한정되는 것이 아니라 서로 다른 다양한 형태로 구현될 것이며, 단지 본 실시 예들은 본 발명의 게시가 완전하도록 하며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 발명의 범주를 완전하게 알려주기 위해 제공되는 것이며, 본 발명은 청구항의 범주에 의해 정의될 뿐이다. Advantages and features of the present invention and methods for achieving them will be apparent with reference to the embodiments described below in detail. However, the present invention is not limited to the embodiments disclosed below, but may be implemented in various forms, and only the present embodiments are intended to complete the disclosure of the present invention, and the general knowledge in the art to which the present invention pertains. It is provided to fully convey the scope of the invention to those skilled in the art, and the present invention is defined only by the scope of the claims.
이하, 본 발명의 셀룰로스계 섬유 혼용제품의 혼용률 측정방법을 구체적으로 설명하면 다음과 같다.Hereinafter, the mixing rate measuring method of the cellulosic fiber mixed product of the present invention will be described in detail.
먼저 혼용률을 측정하고자 하는 셀룰로스계 섬유가 혼용된 시료를 건조한 후 건조중량(M1)을 측정한다(S1). 이 때, 상기 시료를 105 ± 2 ℃ 오븐에서 1시간 30분 이상 건조한 건조중량(M1)을 측정하는 것이 바람직하다.First, after drying the sample mixed with the cellulose-based fiber to measure the mixing rate (M1) to measure the dry weight (S1). At this time, it is preferable to measure the dry weight (M1) which dried the said sample in 105 +/- 2 degreeC oven for 1 hour 30 minutes or more.
다음, 탄화용 조성물에 상기 시료를 침지하는 과정을 거친다(S2). 상기 탄화용 조성물은 금속염, 증점제 및 과건조방지제를 포함하며, 시료 1 g에 대하여 바람직하게는 0.5 ~ 2.0 ml, 더욱 바람직하게는 0.7 ~ 1.0 ml의 부피로 상기 시료의 침지에 사용한다. Next, the process of immersing the sample in the carbonization composition (S2). The carbonizing composition includes a metal salt, a thickener and an anti-drying agent, and is used for immersion of the sample in a volume of preferably 0.5 to 2.0 ml, more preferably 0.7 to 1.0 ml with respect to 1 g of the sample.
상기 금속염은 황산알루미늄, 아황산수소나트륨 및 황산제2철 중에서 선택된 1종 또는 2종 이상의 혼합물이 사용될 수 있고, 상기 화합물은 수화물의 형태로 사용되는 것이 바람직하며, 더욱 바람직하게는 황산알루미늄수화물이 사용되는 것이 좋다.　 상기 금속염은 전체 탄화용 조성물 내 20 ~ 80 중량%, 바람직하게는 30 ~ 70 중량%, 더욱 바람직하게는 40 ~ 60 중량%가 사용되는 것이 좋다.The metal salt may be one or a mixture of two or more selected from aluminum sulfate, sodium hydrogen sulfite and ferric sulfate, and the compound is preferably used in the form of a hydrate, more preferably aluminum sulfate hydrate is used. It is good to be. The metal salt is preferably 20 to 80% by weight, preferably 30 to 70% by weight, more preferably 40 to 60% by weight in the total carbonization composition.
한편 상기 증점제는 점도를 조절할 수 있는 당 업계에 널리 알려진 화합물이 사용될 수 있으며, 바람직하게는 구아검(guar gum), 타라검(tara gum) 및 카복시메틸셀룰로스(carboxy methyl cellulose) 중에서 선택된 1종 또는 2종 이상의 혼합물이 사용될 수 있다.　 상기 증점제는 전체 탄화용 조성물 내 10 ~ 50 중량%, 바람직하게는 20 ~ 40 중량%가 사용되는 것이 좋다. 상기 증점제를 조절하여 1,000 ~ 10,000 cps 정도의 점도를 가지는 탄화용 조성물을 제조한다. Meanwhile, the thickener may be a compound well known in the art that can control the viscosity, preferably one selected from guar gum, tara gum and carboxy methyl cellulose. Mixtures of two or more may be used. The thickener is preferably 10 to 50% by weight, preferably 20 to 40% by weight in the total carbonization composition. The thickening agent is adjusted to prepare a carbonizing composition having a viscosity of about 1,000 to 10,000 cps.
상기 과건조방지제는 과건조에 의한 직물의 과도한 탄화를 방지하고자 사용되며, 글리세린, 폴리에틸렌글리콜 등이 사용될 수 있다. 상기 과건조방지제는 전체 탄화용 조성물 내 1 ~ 30 중량%, 바람직하게는 5 ~ 20 중량%가 사용될 수 있다.The anti-drying agent is used to prevent excessive carbonization of the fabric by over-drying, glycerin, polyethylene glycol may be used. The anti-drying agent may be used 1 to 30% by weight, preferably 5 to 20% by weight in the total carbonization composition.
상기 탄화용 조성물은 침투제, 소포제 기타 첨가제를 포함할 수 있으며, 이의 함량은 당 업자에 의하여 적절하게 조절될 수 있다.　 The carbonizing composition may include a penetrant, an antifoaming agent, and other additives, the content of which may be appropriately adjusted by those skilled in the art.
또한, 상기 탄화용 조성물은 pH 1 ~ 4 범위에 있는 것이 바람직하며, 더욱 바람직하게는 pH 1 ~ 2범위에 있는 것이 셀룰로스계 섬유의 탄화에 보다 유리하다. In addition, the carbonizing composition is preferably in the range of pH 1-4, more preferably in the range of pH 1-2 is more advantageous for the carbonization of cellulose-based fibers.
오븐에서 건조되어 건조중량(M1)이 측정된 건조 시료를 상기 탄화용 조성물에 침지시켜 탄화용 조성물이 시료에 침투되도록 한다. 이 때 조성물이 보다 용이하게 침투되도록 패딩하는 과정을 거치는 것이 바람직하다. 상기 패딩은 픽업(pick-up)률이 60 ~ 100%, 바람직하게는 70 ~ 90% 가 되도록 이루어지는 것이 좋으며, 당 업계에서 일반적으로 사용되는 패더(padder), 링거(wringer) 등을 사용하여 이루어질 수 있다. The dried sample obtained by drying in an oven and having a dry weight (M1) measured is immersed in the carbonizing composition to allow the carbonizing composition to penetrate the sample. At this time, it is preferable to go through the padding process so that the composition is more easily penetrated. The padding may be made so that the pick-up rate is 60 to 100%, preferably 70 to 90%, and is made using a padder, a ringer, or the like, which is generally used in the art. Can be.
상기 과정을 통하여 시료에 탄화용 조성물이 침투되도록 한 후, 이를 열처리하여 탄화시킨다(S3). 상기 열처리는 120 ~ 200 ℃, 바람직하게는 150 ~ 170 ℃에서 약 1 ~ 5분, 더욱 바람직하게는 약 2 ~ 3분 동안 이루어지는 것이 좋다. 상기 열처리는 당 업계에서 널리 사용되는 열전사기 또는 열풍건조기 등을 통하여 이루어질 수 있으며, 상기 열처리 과정에 의하여 셀룰로스계 섬유는 탄화되어 재가 생성된다. After allowing the composition for carbonization to penetrate the sample through the above process, it is carbonized by heat treatment (S3). The heat treatment is preferably performed for about 1 to 5 minutes, more preferably about 2 to 3 minutes at 120 ~ 200 ℃, preferably 150 ~ 170 ℃. The heat treatment may be performed through a heat transfer machine or a hot air dryer, which are widely used in the art, and the cellulose fiber is carbonized to produce ash by the heat treatment process.
다음, 상기 탄화된 시료를 흐르는 물 등으로 수세하여 생성된 재를 제거하며, 바람직하게는 공극의 크기가 150 ㎛ 이하의 망체를 이용하여 재를 제거하는 것이 바람직하다. 탄화된 재가 제거되고 남은 시료를 100 ~ 120℃ 오븐에서 10 ~ 20분간 건조시킨 다음 건조된 시료의 건조중량(M2)을 측정한다(S4). Next, the ash produced by washing the carbonized sample with running water or the like is removed, and preferably, the ash is removed using a mesh having a pore size of 150 μm or less. After the carbonized ash is removed and the remaining sample is dried for 10 to 20 minutes in an oven 100 ~ 120 ℃ and measure the dry weight (M2) of the dried sample (S4).
상기 셀룰로스계 섬유 혼용제품의 혼용률은 상기 처리전 건조중량(M1)과 최종 시료의 건조중량(M2)을 이용하여 계산될 수 있으며, 하기 수학식 1에 혼용률의 계산 방법을 나타내었다. The mixing ratio of the cellulose-based fiber mixed product may be calculated using the dry weight (M1) and the dry weight (M2) of the final sample before treatment, and the formula 1 shows a method of calculating the mixing ratio.
수학식 1
Figure PCTKR2012005006-appb-M000001
 Equation 1
Figure PCTKR2012005006-appb-M000001
상기 방법을 통하여 셀룰로스계 섬유 소재인 면, 마, 리오셀, 모달 및 비스코스 레이온 등이 혼용된 제품에서 셀룰로스계 섬유의 혼용률을 용이하게 측정해 낼 수 있다.Through this method, it is possible to easily measure the mixing rate of cellulose-based fibers in a product in which cotton, hemp, lyocell, modal and viscose rayon, which are cellulose-based fiber materials, are mixed.
이하, 본 발명을 실시 예에 의해 구체적으로 설명하겠는 바, 다음 실시 예는 본 발명을 예시하는 것일 뿐, 본 발명의 내용이 하기 실시 예에 한정되는 것은 아니다.　 Hereinafter, the present invention will be described in detail with reference to Examples, but the following Examples are merely illustrative of the present invention, and the content of the present invention is not limited to the following Examples.
실시 예 1 : 탄화용 조성물의 제조Example 1 Preparation of Carbonization Composition
황산알루미늄수화물 45 중량%, 구아검 40 중량%, 글리세린 10 중량%, 내산성 침투제 3 중량% 및 내산성 소포제 2 중량%를 혼합하여 시료를 탄화시킬 탄화용 조성물을 제조하였다. 45% by weight of aluminum sulfate hydrate, 40% by weight of guar gum, 10% by weight of glycerin, 3% by weight of acid resistant penetrant and 2% by weight of acid resistant antifoam were prepared to prepare a carbonizing composition to carbonize the sample.
실시 예 2 : 셀룰로스계 섬유의 탄화 실험Example 2 Carbonization Experiment of Cellulose Fiber
셀룰로스계 섬유 소재인 면, 리오셀, 모달 및 비스코스 레이온 시료를 상기 탄화용 조성물에 침지 시킨 후, 이를 160℃에서 5분간 열처리하였다. Cotton, lyocell, modal and viscose rayon samples of cellulose fiber materials were immersed in the carbonizing composition, and then heat-treated at 160 ° C. for 5 minutes.
상기 열처리에 따른 탄화된 형태를 도 2에 나타내었으며, 상기 도 2에서 보는 바와 같이 셀룰로스계 섬유는 탄화용 조성물의 침투 및 열처리에 의하여 탄화되는 것을 확인할 수 있었다. The carbonized form according to the heat treatment is shown in FIG. 2, and as shown in FIG. 2, the cellulose-based fiber was confirmed to be carbonized by the penetration and heat treatment of the carbonization composition.
실시 예 3 : 다섬 교직포(Multi test fabric)의 탄화 실험Example 3 Carbonization Experiment of Multi Test Fabric
도 3과 같이 6개의 섬유를 포함하는 다섬 교직포를 상기 실시 예 1의 탄화용 조성물에 침지한 후 이를 160℃에서 5분간 열처리하였다. As shown in FIG. 3, the multi-island textile fabric including six fibers was immersed in the carbonization composition of Example 1, and then heat-treated at 160 ° C. for 5 minutes.
열처리된 다섬 교직포의 형태를 도 4에 나타내었으며, 이를 흐르는 물에 수세한 결과를 도 5에 나타내었다. The shape of the heat-treated multi-island textile fabric is shown in FIG. 4, and the result of washing with flowing water is shown in FIG. 5.
상기 도 4 및 도 5에서 보는 바와 같이, 상기 열처리 및 수세에 의하여 면 직물은 탄화되어 수세에 의하여 제거되나, 다른 직물들은 그대로 남아있는 것을 확인할 수 있었다. As shown in FIG. 4 and FIG. 5, the cotton fabric is carbonized by the heat treatment and washing with water, and the cotton fabric is removed by washing with water, but the other fabrics remain as it is.
상기 실시 예 2 및 3의 결과로부터, 본 발명의 측정방법에 의하여 셀룰로스계 섬유만이 탄화되고 남은 섬유의 중량을 통하여 혼용률을 용이하게 계산할 수 있음을 확인할 수 있었다.　 From the results of Examples 2 and 3, it was confirmed that only the cellulose-based fiber was carbonized by the measuring method of the present invention and the mixing ratio could be easily calculated through the weight of the remaining fiber.
이상에서는 본 발명의 실시 예를 중심으로 설명하였으나, 이는 예시적인 것에 불과하며, 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 기술자라면 이로부터 다양한 변형 및 균등한 타 실시 예가 가능하다는 점을 이해할 것이다. 따라서, 본 발명의 진정한 기술적 보호범위는 이하에 기재되는 특허청구범위에 의해서 판단되어야 할 것이다.Although the above description has been made with reference to the embodiments of the present invention, this is merely exemplary, and a person skilled in the art to which the present invention pertains will understand that various modifications and equivalent other embodiments are possible therefrom. . Therefore, the true technical protection scope of the present invention should be judged by the claims described below.
본 발명의 혼용률 측정방법은 단순하고 간편하면서도, 짧은 시간 내 많은 양의 시료를 처리할 수 있다. 또한, 상기 방법은 용제를 사용하여 대상 섬유를 용해하거나, 강산, 강알칼리 등의 유해 물질을 사용하지 않으므로 친환경적으로 시험을 진행할 수 있으며, 그 정확도 역시 우수한 바, 신속하고 정확한 결과를 원하는 섬유 업계에서 널리 적용될 수 있을 것이다.The mixing rate measuring method of the present invention is simple and simple, and can process a large amount of samples in a short time. In addition, since the method does not dissolve the target fiber using a solvent or use harmful substances such as strong acid or strong alkali, the test can be conducted in an environmentally friendly manner, and its accuracy is also excellent, and it is widely used in the textile industry for fast and accurate results. Could be applied.

Claims (7)

  1. 셀룰로스계 섬유가 혼용된 시료를 건조시키고, 시료의 처리 전 중량을 측정하는 단계;Drying a sample in which cellulosic fibers are mixed, and measuring the weight before the sample is treated;
    금속염, 증점제 및 과건조방지제를 포함하는 탄화용 조성물에 상기 시료를 침지하는 단계; Immersing the sample in a carbonization composition comprising a metal salt, a thickener and an anti-drying agent;
    상기 침지된 시료를 열처리하는 단계; 및Heat treating the immersed sample; And
    열처리된 시료를 수세 및 건조시키고, 중량을 측정하는 단계를 포함하는 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법.Washing and drying the heat-treated sample, and measuring the weight, the mixing rate of the cellulose-based fiber mixed product comprising the step of measuring the weight.
  2. 제1항에 있어서, The method of claim 1,
    상기 금속염은 황산알루미늄, 아황산수소나트륨 및 황산제2철 중에서 선택된 1종 또는 2종 이상의 혼합물인 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법.Wherein the metal salt is one or two or more selected from the group consisting of aluminum sulfate, sodium hydrogen sulfite and ferric sulfate mixture mixture measuring method of the fiber-based mixed products.
  3. 제1항에 있어서, The method of claim 1,
    상기 금속염은 탄화용 조성물 내 20 ~ 60 중량%의 범위로 포함되는 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법.The metal salt is a method for measuring the mixing ratio of the cellulose-based fiber mixed product, characterized in that it is included in the range of 20 to 60% by weight in the carbonization composition.
  4. 제1항에 있어서, The method of claim 1,
    상기 증점제는 구아검, 타라검 및 카복시메틸셀룰로스 중에서 선택된 1종 또는 2종 이상의 혼합물인 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법. The thickener is a method for measuring the mixing ratio of the cellulose-based fiber mixed product, characterized in that one or a mixture of two or more selected from guar gum, tara gum and carboxymethyl cellulose.
  5. 제1항에 있어서,The method of claim 1,
    상기 과건조방지제는 글리세린, 폴리에틸렌 글리콜 또는 이들의 혼합물인 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법. The anti-drying agent is glycerin, polyethylene glycol or a mixture of cellulose-based fiber mixed product, characterized in that a mixture thereof.
  6. 제1항에 있어서,The method of claim 1,
    상기 열처리는 120 ~ 200 ℃에서 이루어지는 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법. The heat treatment is a method for measuring the mixing ratio of the cellulose-based fiber mixed product, characterized in that at 120 ~ 200 ℃.
  7. 제1항에 있어서,The method of claim 1,
    상기 시료 1 g에 대하여 0.5 ~ 2.0 ml의 탄화용 조성물을 사용하는 것을 특징으로 하는 셀룰로스계 섬유 혼용제품의 혼용률 측정방법. Method for measuring the mixing ratio of the cellulose-based fiber mixed product, characterized in that for use in the carbonization composition of 0.5 to 2.0 ml per 1 g of the sample.
PCT/KR2012/005006 2012-06-14 2012-06-25 Method for measuring mixing ratio of cellulose-based fiber mixed product using chemical carbonization method WO2013187549A1 (en)

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KR101334170B1 (en) 2012-09-27 2013-11-28 사단법인 코티티시험연구원 Method for quantitative analysis of protein fiber mixtures of textiles by carbonization
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JP2004121229A (en) * 2002-08-27 2004-04-22 Japan Spinners Inspecting Foundation Method for identifying mixing ratio of animal hair fiber in animal hair fiber product
KR100663839B1 (en) * 2005-06-10 2007-01-02 한국섬유기술연구소 Multifunctional cellulose textile and preparation for preparing the same
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JP2004121229A (en) * 2002-08-27 2004-04-22 Japan Spinners Inspecting Foundation Method for identifying mixing ratio of animal hair fiber in animal hair fiber product
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