KR20040094491A - A method for producing highly purified chitin - Google Patents
A method for producing highly purified chitin Download PDFInfo
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- KR20040094491A KR20040094491A KR1020030028279A KR20030028279A KR20040094491A KR 20040094491 A KR20040094491 A KR 20040094491A KR 1020030028279 A KR1020030028279 A KR 1020030028279A KR 20030028279 A KR20030028279 A KR 20030028279A KR 20040094491 A KR20040094491 A KR 20040094491A
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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Abstract
Description
본 발명은, 게 또는 새우 등 갑각류의 갑각을 알칼리 용액으로 가수분해하고 묽은 염산으로 처리하는 통상적인 방법에 의해 제조된 키틴 분말에, K2Cr2O7또는 KMnO4를0.1~5.0 중량% 함유하는 수용액을 2~5배량(w/w) 첨가하여 1-3일 동안 침적시키고, 상기 키틴 수용액에 옥살산을 0.1~3.0 중량% 함유하는 수용액을 키틴 분말 대비 10~20배량(w/w) 첨가하여 반응시킨 후 동결건조시키고, 건조된 분말을 2N-염산 용액에 1일 동안 침적시킨 후 증류수로 6~7회 세척하고, 에탄올, 에테르 및 증류수로 교대로 세척함으로써 고품질, 고순도의 정제 키틴을 제조하는 방법에 관한 것이다.The present invention contains 0.1 to 5.0% by weight of K 2 Cr 2 O 7 or KMnO 4 in chitin powder prepared by a conventional method of hydrolyzing crustacean such as crab or shrimp with an alkaline solution and treating with dilute hydrochloric acid. 2 to 5 times (w / w) of the aqueous solution was added and deposited for 1-3 days, and 10 to 20 times (w / w) of the chitin powder was added to the aqueous solution containing 0.1 to 3.0% by weight of oxalic acid in the chitin solution. After lyophilization, the dried powder was immersed in 2N hydrochloric acid solution for 1 day, washed 6-7 times with distilled water, and washed alternately with ethanol, ether and distilled water to prepare high-quality purified chitin. It is about how to.
키틴(chitin)은 새우, 게, 가재 등의 갑각류 껍질, 갑충(甲蟲)의 갑피(甲皮) 등 절지동물의 외골격, 연체동물의 기관, 곰팡이, 효모, 버섯등의 진균류의 세포벽등에 포함된 무코다당의 한종류이다. 생체내에서는 당단백질로서 존재한다. 키틴은 N-아세틸-D-글루코사민 잔당 (GlcNAc)n이 β-1,4결합한 선상 고분자로서 D-글루코사민 잔당(GlcN)n이 일부 포함되어 있다. 이것은 동물체내에서 생분해 될 수 있고 항원성 고분자가 거의 없다. 키틴질은 갑각류, 곤충류, 패류를 시작으로 주로 하등동물의 외피골격 성분으로서 자연계에 널리 분포하고 있는데, 지구상의 생물생산량은 년간 10억톤으로도 1000억톤으로도 말해진다. 이것은 셀룰로오스에 버금가는 양으로 바이오매스 자원으로서 중요하다. 현재 키틴의 원료로서 이용되어지는 게나 새우껍질 등은 건조중량으로서 25-35%가 키틴으로 되어 있고 그 외에 탄산칼슘(CaCO3)를 주체로 하는 회분 20-50%, 단백질을 10-40%, 그 외에 약간의 지질, 색소 등을 포함하고 있다. 이것들의 비율은 게와 새우의 종류 및 부위에 따라 다르다. 일반적으로 새우껍질 편이 키틴질의 비율이 높고 왕게는 칼슘분이 많다. 또 갑각과 등부분은 칼슘함량이 높고, 배쪽 부분은 단잭질이 많기 때문에 일반적으로 키틴함량이 높은 다리부분 껍질이 사용되어지는 경우가 많다. 이것들의 껍질에서 단백질, 회분, 색소 등을 용출 제거시켜 남은 산.알카리 불용물이 키틴이다.Chitin is a muco included in shells of shellfish such as shrimp, crabs and crayfish, exoskeleton of arthropods such as beetles' shells, organs of mollusks, fungi, yeasts, and mushrooms. It is a kind of polysaccharide. It is present as a glycoprotein in vivo. Chitin is a linear polymer in which N-acetyl-D-glucosamine residue (GlcNAc) n is β-1,4-linked and contains some D-glucosamine residue (GlcN) n. It can be biodegraded in animals and there are few antigenic polymers. Chitin is widely distributed in the natural world, including crustaceans, insects, and shellfish, mainly as inferior skeletons of lower animals. The biomass on Earth is said to be 1 billion tons or 100 billion tons per year. This is important as a biomass resource in an amount comparable to cellulose. Currently, crab and shrimp shells, which are used as raw materials for chitin, have dry weight of 25-35% of chitin. In addition, 20-50% of ash, mainly calcium carbonate (CaCO 3 ), 10-40% of protein, In addition, it contains some lipids and pigments. The ratio of these depends on the type and part of the crab and shrimp. In general, shrimp shells have a high percentage of chitin, and king crabs contain a lot of calcium. In addition, the carapace and the back part is high in calcium, the abdomen is a lot of sweet jackal, because the chitin-rich leg shell is usually used. The acid and alkali insolubles left by elution of proteins, ash and pigments from these shells are chitin.
키틴은 용도에 대해 점도, 순도, 착색의 점도, 입도등이 다르고 여러가지의 제품이 생산되고 있다. 백색 무정형의 분말이지만, 황백색, 혹은 담적색으로 착색되어 있는 것이 많다. 약간의 특이한 냄새가 있다. 비선광도는 [ ]D = -15°(진한 염산中)이다. 키틴은 분자내의 아세틸 아미노기의 분자간 수소결합에 의해 강고한 결정구조를 형성하고 있어서 극히 난용성으로 물, 에탄올, 에테르 등의 일반적 유기용매, 묽은 산, 묽은 알칼리용액 뿐 아니라 셀룰로오스용제인 동암모니아 시약에도 용해되지 않는다. 진한 염산, 진한 황산, 질산 등에는 녹지 않지만 그 때 일부가 분해되어 분자량이 저하된다. 이 난용성은 성형가공 등 키틴의 이용 면에서 불리하기 때문에 용제의 탐색이 행해져 개미산, 디클로로초산, 트리클로로초산/디클로로에탄, 디메틸아세트아미드(DMA)/염화리튬(LiCl), DMA/N-메틸피로리돈(NMP)/염화리튬, 메탄술폰산, 헥사플루오르이소프로판올, 헥사플루오르아세톤, 디메틸포름아미드/N2O4등이 알려져 있다. 키틴과 키토산도, 시차주사열량계(示差走査熱量計)에 의한 측정에서 분말상태에서 각각 275℃, 280℃에서 열분해가 최대가 된다. 키틴의 구성 성분인 N-아세틸-D-글루코사민의 융점은 약 190℃이다.Chitin differs in viscosity, purity, coloring viscosity, particle size, and the like, and various products have been produced. Although it is a white amorphous powder, it is many colored yellowish white or light red. There is a slight peculiar smell. Specific light intensity is [] D = -15 ° (in concentrated hydrochloric acid). Chitin forms a strong crystal structure by intermolecular hydrogen bonding of acetyl amino groups in the molecule, and is extremely poorly soluble in water, ethanol, ether and other organic solvents, dilute acids and dilute alkaline solutions, as well as in cellulose solvents, ammonia reagents. Does not dissolve It is insoluble in concentrated hydrochloric acid, concentrated sulfuric acid, nitric acid, etc., but part of it is decomposed and molecular weight decreases. This poor solubility is disadvantageous in terms of the use of chitin, such as molding, so that a solvent is searched for formic acid, dichloroacetic acid, trichloroacetic acid / dichloroethane, dimethylacetamide (DMA) / lithium chloride (LiCl), DMA / N-methyl Pyridone (NMP) / lithium chloride, methanesulfonic acid, hexafluoroisopropanol, hexafluoroacetone, dimethylformamide / N 2 O 4 and the like are known. Pyrolysis is the maximum at 275 ° C and 280 ° C in powder form, respectively, as measured by chitin, chitosanity, and differential scanning calorimetry. The melting point of N-acetyl-D-glucosamine, which is a component of chitin, is about 190 ° C.
키틴 및 키틴으로부터 제조되는 키토산, 이들의 저분자 올리고당 등은 식품보존제, 식품 물성 조절 및 중금속 제거뿐만 아니라 콜레스테롤 저하작용, 면역증진효과, 장내세균인 Bifidus의 생장촉진, 화상치료 등 의약용으로도 널리 이용되며 최근 주목을 받고 있다.Chitosan and chitosan prepared from chitin and their low-molecular oligosaccharides are widely used for food preservatives, control of food properties and elimination of heavy metals, as well as for lowering cholesterol, enhancing immune effects, promoting growth of enteric bacteria, Bifidus, and treating burns. And recently attracting attention.
현재, 이 키틴의 공업적 생산이 활발히 이루어지고 있으나, 그 원료의 대부분은 게 또는 새우껍질이며, 갯가재의 껍질이나 오징어의 갑도 일부 이용되고 있다.At present, the industrial production of this chitin is active, but most of the raw materials are crab or shrimp shells, and shellfish shellfish and shellfish cuttlefish are also partially used.
이들 원료로부터 키틴을 단리함에 있어서, 난용성인 키틴을 용해할 수 있는 경제적이고 적절한 용매는 알려져 있지 않다. 따라서 키틴을 얻는 일반적인공업적 방법으로서, 게 또는 새우 외피 중의 탄산칼슘과 단백질을 물에 가용화하여 외피로부터 제거함으로써 키틴을 얻는 방법이 행하여지고 있다. 구체적으로는 (1) 게 또는 새우의 외피를 알칼리 수용액 중에서 가열하여 단백질을 알칼리 가수분해한 후 분해된 단백질을 수세하여 제거하고; (2) 키틴을 포함한 불용물을 묽은 염산 수용액속에 침지하여 불용물속의 탄산칼슘을 수용성의 염화칼슘으로 바꾼 다음 수세 제거함으로써 불용물인 키틴을 얻는 2단계의 공정으로 이루어진다. 이 때, 묽은 알칼리 용액 처리와 묽은 염산 처리의 순서가 반대인 경우도 있다.In isolating chitin from these raw materials, an economical and suitable solvent capable of dissolving poorly soluble chitin is not known. Therefore, as a general industrial method for obtaining chitin, a method of obtaining chitin by solubilizing calcium carbonate and protein in a crab or shrimp shell and removing it from the shell is performed. Specifically, (1) the shell of the crab or shrimp is heated in an aqueous alkali solution to alkali hydrolyze the protein, and the digested protein is washed with water to remove it; (2) An insoluble matter containing chitin is immersed in dilute hydrochloric acid solution to replace calcium carbonate in insoluble matter with water-soluble calcium chloride, followed by washing with water to obtain insoluble matter chitin. At this time, the order of a diluted alkaline solution process and a diluted hydrochloric acid process may be reversed.
상기와 같이, 원료에서 단백질과 탄산칼슘을 제거하는 방법으로 제조된 키틴은, 잔존하는 무기질 등 불순물을 함유하고 있으며 알칼리 가수분해 과정 중에 중금속이 포함될 수 있어, 품질상의 균일성이 부족하여 공업제품으로서 문제가 있었다.As described above, the chitin prepared by the method of removing protein and calcium carbonate from the raw material contains impurities such as remaining minerals and may contain heavy metals during the alkali hydrolysis process. There was a problem.
따라서 본 발명의 목적은, 산화제 (K2Cr2O7,KMnO4)를 이용하여 중금속 또는 잔존하는 단백질과 무기염 등을 제거하고, 사용된 산화제 및 잔존 이온은 옥살산을 이용하여 용해탈리시켜 제거하며, 염산용액 처리와 에탄올, 에테르 및 증류수로 세척하는 과정을 거침으로써 잔존하는 무기물과 유기물 등 불순물을 완전히 제거한고순도의 정제 키틴을 제공하는 데 있다.Accordingly, an object of the present invention is to remove heavy metals or remaining proteins and inorganic salts, etc. using oxidizing agents (K 2 Cr 2 O 7, KMnO 4 ), and the oxidizing agents and residual ions used are dissolved and removed by oxalic acid. In addition, through the process of hydrochloric acid solution and rinsing with ethanol, ether and distilled water to provide a high purity purified chitin to completely remove impurities such as inorganic and organic matter.
본 발명의 기술적 과제는 게 또는 새우 등 갑각류의 갑각을 알칼리 용액으로 가수분해하고 묽은 염산으로 처리하는 통상적인 방법에 의해 제조된 키틴 분말에, K2Cr2O7또는 KMnO4를0.1~5.0 중량% 함유하는 수용액을 2~5배량(w/w) 첨가하여 1-3일 동안 침적시키고, 상기 키틴 수용액에 옥살산을 0.1~3.0 중량% 함유하는 수용액을 키틴 분말 대비 10~20배량(w/w) 첨가하여 반응시킨 후 동결건조시키고, 건조된 분말을 2N-염산 용액에 1일 동안 침적시킨 후 증류수로 6~7회 세척하고, 에탄올, 에테르 및 증류수로 교대로 세척하여 고순도 정제 키틴을 제조함으로써 달성하였다.Technical problem of the present invention is 0.1 to 5.0 weight of K 2 Cr 2 O 7 or KMnO 4 in chitin powder prepared by a conventional method of hydrolyzing crustacean, such as crab or shrimp, with an alkaline solution and treating with dilute hydrochloric acid. 2 to 5 times (w / w) of aqueous solution containing% was added and deposited for 1-3 days, and the aqueous solution containing 0.1 to 3.0% by weight of oxalic acid was 10 to 20 times (w / w) of chitin powder. Lyophilized and the dried powder was immersed in 2N hydrochloric acid solution for 1 day, washed 6-7 times with distilled water, and washed alternately with ethanol, ether and distilled water to produce high purity purified chitin. Achieved.
도 1은 키틴의 구조식을 나타낸 것이다.1 shows the structural formula of chitin.
도 2는 본 발명의 정제방법으로 제조된 키틴을 적외선 스펙트럼으로 분석한 결과를 나타낸 것이다.Figure 2 shows the results of analyzing the chitin prepared by the purification method of the present invention in the infrared spectrum.
도 3은 고순도 정제 키틴의 제조공정을 단계별로 나타낸 것이다.Figure 3 shows step by step the manufacturing process of high purity purified chitin.
본 발명은 게 또는 새우 등 갑각류의 갑각을 알칼리 용액으로 가수분해하고 묽은 염산으로 처리하여 통상적인 방법에 의해 키틴 분말을 제조하는 단계; 키틴 분말에 K2Cr2O7또는 KMnO4를0.1~5.0 중량% 함유하는 수용액을 2~5배량The present invention comprises the steps of preparing a chitin powder by a conventional method by hydrolyzing the shell of crustaceans such as crab or shrimp with an alkaline solution and treated with dilute hydrochloric acid; 2 to 5 times the amount of chitin powder containing 0.1 to 5.0% by weight of K 2 Cr 2 O 7 or KMnO 4
(w/w) 첨가하여 1-3일 동안 침적시키는 단계; 상기 키틴 수용액에 옥살산을 0.1~3.0 중량% 함유하는 수용액을 키틴 분말 대비 10~20배량(w/w) 첨가하여 반응시킨 후 동결건조시키는 단계; 건조된 분말을 2N-염산 용액에 1일 동안 침적시킨 후증류수로 6~7회 세척하는 단계; 에탄올, 에테르 및 증류수로 교대로 세척하는 단계로 구성된다.(w / w) addition to deposit for 1-3 days; Reacting the aqueous solution containing 0.1 to 3.0% by weight of oxalic acid to the chitin aqueous solution by adding 10 to 20 times (w / w) to the chitin powder, followed by lyophilization; Immersing the dried powder in 2N-hydrochloric acid solution for 1 day and then washing it with distilled water 6-7 times; Alternatively washing with ethanol, ether and distilled water.
이하, 본 발명의 구체적인 구성 및 작용을 실시예에 의해 더욱 상세히 설명한다. 단, 하기의 실시예는 본 발명을 예시하기 위한 것일 뿐, 본 발명의 권리범위가 이들에만 한정되는 것은 아니다.Hereinafter, the specific configuration and operation of the present invention will be described in more detail by examples. However, the following examples are only for illustrating the present invention, and the scope of the present invention is not limited thereto.
실시예 : 고순도 정제 키틴의 제조방법Example: Preparation of High Purity Chitin
게 또는 새우 등 갑각류의 갑각을 선별하여 세척한 후 작은 칩(chip)크기로 2차 분쇄시킨 (보통 0.5-3cm 직경) 껍질을 4%의 수산화나트륨 용액에 넣고, 90℃로 14시간 처리하여 단백질을 용출, 제거한다. 이어서, 증류수로 중성이 될 때까지 세척한 후 4%의 묽은 염산 수용액에 실온에서 18시간 동안 침적시켜서 탄산칼슘 등의 회분을 제거한다.The shells of crustaceans such as crab or shrimp are screened and washed, and the shells (secondly 0.5-3 cm in diameter) that are crushed into small chips are placed in 4% sodium hydroxide solution and treated at 90 ° C for 14 hours. Elute and remove. Subsequently, the mixture is washed with distilled water until neutral and then immersed in 4% aqueous hydrochloric acid solution at room temperature for 18 hours to remove ash such as calcium carbonate.
탈이온수나 증류수로 중성이 될 때까지 세척하고 건조, 분쇄시켜 식품첨가용 키토산 제조원료로서 사용되는 공업용 키틴(practical grade chitin)을 제조한다.Wash, dry and pulverize with deionized or distilled water until neutral to prepare industrial grade chitin used as a food additive chitosan preparation.
상기와 같이 통상적인 방법으로 제조된 공업용 키틴을, 볼-밀(Ball-Mill)에 의하여 200 ㎛의 크기로 분쇄한다. 키틴 분말에 K2Cr2O7또는 KMnO4를 2 중량% 함유하는 수용액을 2배량(w/w) 첨가하고 2일 동안 침적시킴으로써, 잔존하는 단백질과 칼슘을 포함한 무기염 등의 회분 또는 알칼리 가수분해 과정 중 흡착된 중금속 등 불순물을 제거한다. 이 때 K2Cr2O7또는 KMnO4를 0.1~5.0 중량% 함유하는수용액을 사용할 수 있으며, 상기 수용액은 키틴 분말의 2~5배량(w/w)을 첨가할 수 있다.Industrial chitin prepared by the conventional method as described above is ground to a size of 200 μm by a ball-mill. 2 times (w / w) of an aqueous solution containing 2% by weight of K 2 Cr 2 O 7 or KMnO 4 was added to the chitin powder, followed by immersion for 2 days. During the decomposition process, impurities such as heavy metals adsorbed are removed. At this time, an aqueous solution containing 0.1 to 5.0% by weight of K 2 Cr 2 O 7 or KMnO 4 may be used, and the aqueous solution may add 2 to 5 times (w / w) of chitin powder.
상기 수용액에 옥살산을 1 중량% 함유하는 수용액을 키틴 분말 대비 10배량(w/w) 첨가하여 반응시킴으로써, 산화공정에서 발생한 잔존 이온 및 산화제를 탈리용해시켜 제거한 후 이를 동결건조시킨다. 이 때 옥살산을 0.1~3.0 중량% 함유하는 수용액을 사용할 수 있으며, 상기 수용액은 키틴 분말의 10~20배량(w/w)을 첨가할 수 있다.The aqueous solution containing 1% by weight of oxalic acid is added to the aqueous solution by adding 10 times (w / w) to the chitin powder to react, thereby removing and removing the remaining ions and oxidants generated in the oxidation process by lyophilization. At this time, an aqueous solution containing 0.1 to 3.0% by weight of oxalic acid may be used, and the aqueous solution may be added in an amount of 10 to 20 times (w / w) of chitin powder.
건조된 분말을 2N-염산 용액에 1일 동안 침적한 후 탈이온수나 증류수로 7회 세척함으로써, 잔존하는 칼슘, 회분 등 무기물을 완전히 제거한다.The dried powder is immersed in a 2N hydrochloric acid solution for 1 day and then washed 7 times with deionized or distilled water to completely remove the remaining minerals such as calcium and ash.
그런 다음, 이를 에탄올, 에테르 및 증류수로 교대로 세척함으로써, 잔존하는 유기물을 완전히 제거한다.It is then washed alternately with ethanol, ether and distilled water to completely remove the remaining organics.
최종적으로 이를 압착여과하고 감압하에 0℃에서 동결건조시켜 고기능 순수 정제 키틴을 수득한다.Finally it was filtered and lyophilized at 0 ° C. under reduced pressure to give a high performance pure purified chitin.
실험예 : 적외선 스펙트럼(Infrared spectrum) 분석Experimental Example: Infrared spectrum analysis
키틴의 구조는 도 1의 구조식에서와 같이 2-아세트아미드-2-디옥시-D-글루코오스(N-아세틸-β-글루코사민이라고도함)가, β-(1→4)글루코시드 결합을 사이에 두고 직쇄상으로 축합한 호모다당으로, 화학적으로는 (1,4)-2-아세트아미드-2-디옥시-β-D-글루칸의 구조를 가진다. 글루코사민기가 5000 이상 결합한 고분자로서 그 분자량은 100만 정도이다.The structure of chitin is that 2-acetamide-2-deoxy- D -glucose (also referred to as N -acetyl-β-glucosamine) between the β- (1 → 4) glucoside bonds as shown in the structural formula of FIG. Homopolysaccharide condensed in a straight chain, chemically, has a structure of (1,4) -2-acetamide-2-dioxy-β- D -glucan. A polymer having a glucosamine group bound to 5000 or more, and its molecular weight is about 1 million.
도 2는 고기능 순수 정제키틴의 적외선 스펙트럼(Infrared spectrum)으로서키틴의 아미드기(N-H)와 수산기(OH)에 관련된 밴드를 나타낸 것이다. 1,619cm-1밴드는 수산기에 결합된 C=O진동에 의한 것으로, 1655cm-1밴드는 아미드기 진동과 결합된 C=O…N-H기로 인한 것이며 N-H 굽힘 진동이 C-N 신축 모드와 혼합되어 아미드Ⅱ(1,500cm-1) 위치에서 나타내고 있다. 또한, 다양한 CH, CH2그리고 CH3의 신축 주파수들은 2,840-2,962cm-1의 범위내에서 관찰되고 있다. 2,840cm-1에서의 약한 밴드는 대칭 CH2신축 모드에 의한 것일 수 있으며, 비대칭 CH2의 신축 모드는 2929cm-1밴드의 원인이 된다. CH2밴드 모드에 의하여 1,430cm-1이나 1,420cm-1밴드에 수직밴드가 나타난다.FIG. 2 shows the bands associated with the amide group (NH) and the hydroxyl group (OH) of chitin as an infrared spectrum of high-performance pure purified chitin. The 1,619 cm -1 band is due to C = O vibration coupled to the hydroxyl group, while the 1,655 cm -1 band is combined with C = O... It is due to the NH group and the NH bending vibration is shown in the amide II (1,500 cm −1 ) position in combination with the CN stretch mode. In addition, various stretching frequencies of CH, CH 2 and CH 3 are observed in the range of 2840-2962 cm −1 . The weak band at 2840 cm −1 may be due to the symmetrical CH 2 stretch mode, and the stretch mode of the asymmetrical CH 2 causes the 2929 cm −1 band. Vertical bands appear in the 1,430 cm -1 and 1,420 cm -1 bands by CH 2 band mode
상기와 같이 아미드기와 수산기의 흡수밴드를 조사하고, 흡수 파장과 일치시킨 결과로써 정제 키틴임을 확인할 수 있었다.As described above, the absorption band of the amide group and the hydroxyl group was examined, and it was confirmed that it was purified chitin as a result of matching the absorption wavelength.
상기 실시예를 통하여 설명한 바와 같이 통상적인 방법으로 제조된 키틴 분말에, K2Cr2O7또는 KMnO4를0.1~5.0 중량% 함유하는 수용액을 2~5배량(w/w) 첨가하여 1-3일 동안 침적시키고, 상기 키틴 수용액에 옥살산을 0.1~3.0 중량% 함유하는 수용액을 키틴 분말 대비 10~20배량(w/w) 첨가하여 반응시킨 후 동결건조시키고, 건조된 분말을 2N-염산 용액에 1일 동안 침적시킨 후 증류수로 6~7회 세척하고, 에탄올, 에테르 및 증류수로 교대로 세척함으로써 얻어진 정제 키틴은 고순도, 고품질의 키틴으로서 이는 건강식품 산업상 매우 유용한 발명인 것이다.To the chitin powder prepared by the conventional method as described through the above examples, an aqueous solution containing 0.1 to 5.0% by weight of K 2 Cr 2 O 7 or KMnO 4 was added 2 to 5 times (w / w) to 1- After immersion for 3 days, the aqueous solution containing 0.1 to 3.0% by weight of oxalic acid was added to the chitin aqueous solution and reacted by adding 10-20 times (w / w) to the chitin powder, followed by lyophilization, and the dried powder was a 2N hydrochloric acid solution. Purified chitin obtained by immersion for 1 day in distilled water and then washed with distilled water six to seven times, alternately with ethanol, ether and distilled water is a high purity, high quality chitin, which is a very useful invention in the health food industry.
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| CN100560608C (en) * | 2007-12-30 | 2009-11-18 | 浙江大学 | A kind of resource-saving type chitin clean preparation method |
| CN112209360A (en) * | 2020-10-16 | 2021-01-12 | 北京理工大学 | Shrimp shell conversion method based on sulfonic acid type eutectic solvent |
| CN113185711A (en) * | 2021-05-24 | 2021-07-30 | 贝尔纳丝新材料(江苏)有限公司 | Preparation method of acidic, neutral and alkaline stable dispersed nano chitin |
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| CN100560608C (en) * | 2007-12-30 | 2009-11-18 | 浙江大学 | A kind of resource-saving type chitin clean preparation method |
| CN112209360A (en) * | 2020-10-16 | 2021-01-12 | 北京理工大学 | Shrimp shell conversion method based on sulfonic acid type eutectic solvent |
| CN113185711A (en) * | 2021-05-24 | 2021-07-30 | 贝尔纳丝新材料(江苏)有限公司 | Preparation method of acidic, neutral and alkaline stable dispersed nano chitin |
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