KR100578501B1 - A method for producing organic acid salts and chitin from crustacean shell using organic acids - Google Patents

A method for producing organic acid salts and chitin from crustacean shell using organic acids Download PDF

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KR100578501B1
KR100578501B1 KR1020040091579A KR20040091579A KR100578501B1 KR 100578501 B1 KR100578501 B1 KR 100578501B1 KR 1020040091579 A KR1020040091579 A KR 1020040091579A KR 20040091579 A KR20040091579 A KR 20040091579A KR 100578501 B1 KR100578501 B1 KR 100578501B1
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박노동
정우진
국주희
김길용
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전남대학교산학협력단
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    • 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

본 발명은 갑각류의 껍질로부터 유기산칼슘을 제조하는 방법에 관한 것이다. 더욱 상세하게는 본 발명은 갑각류의 껍질로부터 키틴의 제조공정 중 부산물로서 발생하는 칼슘을 보다 효율적으로 회수하여 활용하기 위한 방법에 관한 것으로, 본 발명의 방법에 따르면, 갑각류의 껍질에 유기산을 첨가하고 일정 시간 반응시킨 것을 여과시켜 상등액과 껍질은 제거하고 그 여과액을 정제하여 간편하고 효율적으로 유기산칼슘을 얻을 수 있다.The present invention relates to a method for producing calcium carbonate from shells of crustaceans. More specifically, the present invention relates to a method for more efficiently recovering and utilizing calcium generated as a by-product of chitin production from shells of crustaceans. According to the method of the present invention, organic acids are added to shells of shellfish and After the reaction for a certain time, the supernatant and the shell are removed, and the filtrate can be purified to simply and efficiently obtain the organic calcium acid.

갑각류 껍질, 유기산, 구연산, 말산, 칼슘, 의료용 소재Crustacean shell, organic acid, citric acid, malic acid, calcium, medical material

Description

유기산을 이용하여 갑각류로부터 유기산칼슘 및 키틴을 제조하는 방법 {A method for producing organic acid salts and chitin from crustacean shell using organic acids}A method for producing organic acid salts and chitin from crustacean shell using organic acids}

도 1은 키틴 제조공정에서 갑각류의 탈회 및 유기산염 생산에 대한 일반적 공정도를 나타낸 그림이다.1 is a diagram showing a general process for deliming of crustaceans and organic acid production in chitin production process.

본 발명은 갑각류의 껍질로부터 유기산칼슘을 제조하는 방법에 관한 것이다. 더욱 상세하게는 본 발명은 갑각류의 껍질로부터 키틴의 제조공정 중 부산물로서 발생하는 칼슘을 보다 효율적으로 회수하여 활용하기 위한 방법에 관한 것으로, 본 발명의 방법에 따르면, 갑각류의 껍질에 유기산을 첨가하고 반응시킨 것을 여과시켜 상등액과 껍질은 제거하고 그 여과액을 정제하여 간편하고 효율적으로 유기산칼슘을 얻을 수 있다.The present invention relates to a method for producing calcium carbonate from shells of crustaceans. More specifically, the present invention relates to a method for more efficiently recovering and utilizing calcium generated as a by-product of chitin production from shells of crustaceans. According to the method of the present invention, organic acids are added to shells of shellfish and The reaction was filtered to remove the supernatant and the shell, and the filtrate was purified to easily and efficiently obtain organic calcium acid.

게나 새우 등 갑각류의 껍질에는 키틴, 칼슘 등 산업상 유용한 성분이 풍부하게 존재하며, 이중 갑각류의 껍질로부터 키틴을 분리·제조하는 방법에 관해서는 많은 연구가 진행된 바 있다. 일반적인 키틴의 제조 공정은, 갑각류의 껍질을 염산 (HCl)에 담가 탄산칼슘을 용출함으로써 회분을 제거한 다음, 알칼리와 함께 가열함으로써 단백질을 제거하는 것으로 이루어진다. 이러한 키틴의 제조 공정 중에는, 최종산물로서 얻어지는 키틴 외에 다량의 부산물이 발생하는데, 이러한 부산물을 유용하게 회수하여 이용하기 위한 여러 연구도 진행된 바 있다.Crustaceans such as crabs and shrimps are rich in industrially useful ingredients such as chitin and calcium, and many studies have been conducted on how to isolate and manufacture chitin from shells. A typical chitin production process consists of dipping shells of crustaceans in hydrochloric acid (HCl) to remove ash by eluting calcium carbonate and then heating with alkali to remove proteins. In the manufacturing process of the chitin, a large amount of by-products are generated in addition to the chitin obtained as the final product, and various studies have been conducted for the useful recovery and use of these by-products.

예를 들어 한국등록특허 제0405958호 "갑각류 또는 키틴 제조부산물로부터 색소를 분리하는 방법 및 이를 주원료로 하는 어류 또는 산란계용 착색제 조성물"은 갑각류로부터 키틴의 제조공정 중 탈칼슘화 공정과 탈단백 공정에서 발생하는 부산물인 폐수를 수집하고 이로부터 유용한 색소를 분리하여 이용하는 방법에 관한 기술이다.For example, Korean Patent No.0405958, "Method for Separating Pigments from Crustaceans or Chitin by-products and Fish or Laying-based Colorant Compositions Based on Its" in the decalcification and deproteinization processes of chitin from crustaceans. It is a technique for collecting wastewater as a by-product generated and separating useful pigments therefrom.

한편 키틴 제조공정 중 탈칼슘화 공정에서 발생하는 주요 부산물로는 칼슘 성분이 있는데, 이를 회수하여 유용하게 활용하는 방법에 관한 연구도 진행된 바 있다.On the other hand, the main by-product of the decalcification process in the chitin manufacturing process is a calcium component, a study on how to recover it and utilize it usefully.

종래 갑각류로부터 키틴의 제조공정 중 칼슘을 회수하는 방법으로는, 갑각류의 껍데기를 염산(HCl) 수용액으로 처리하여 염화칼슘 수용액화하고 이를 여과지로 흡입 여과시켜 고형물을 제거한 후 여과된 수용액에 가성소다를 처리하여 염화칼슘을 수산화칼슘으로 변화시켜서 침전시켜 회수하거나, 또는 수산화칼슘 수용액에 탄산가스를 반응시켜 탄산칼슘을 얻는 방법이 사용되었다.In the conventional method of recovering calcium in the production of chitin from crustaceans, shells of crustaceans are treated with aqueous hydrochloric acid (HCl) to form calcium chloride solution, which is filtered through suction with filter paper to remove solids, and then caustic soda is treated in the filtered aqueous solution. A method of obtaining calcium carbonate by converting calcium chloride into calcium hydroxide to precipitate and recovering it, or by reacting carbon dioxide with an aqueous solution of calcium hydroxide, was used.

그러나 상기한 방법은 수산화칼슘 및 탄산칼슘만을 얻는 방법으로서 공정 절차가 매우 비효율적이고, 얻어진 칼슘이 무기칼슘이므로 유기칼슘에 비해 생체 흡수율이 떨어져 이용상 불리한 점이 있었다.However, the above-mentioned method is a method of obtaining only calcium hydroxide and calcium carbonate, which is very inefficient, and because the obtained calcium is inorganic calcium, its bioabsorption rate is lower than that of organic calcium.

따라서 본 발명자들은 갑각류로부터 유기칼슘을 얻을 수 있는 효율적이고 간편한 공정을 개발하고자 연구하였으며, 갑각류의 껍질을 유기산 처리하는 것을 특징으로 하는 본 발명을 완성하게 되었다.Therefore, the present inventors have studied to develop an efficient and convenient process for obtaining organic calcium from shellfish, and have completed the present invention characterized in that the shell of shellfish is treated with organic acid.

본 발명은 갑각류 껍질에 유기산을 적정 농도로 희석하여 첨가한 다음 일정 시간 반응시키고, 반응물을 여과시켜 상등액과 껍질을 제거하고, 여과액을 와트만페이퍼로 여과시켜 정제함으로써 유기산칼슘을 얻는 방법에 관한 것으로, 상기와 같은 방법에 의하여 간편하고 효율적으로, 또한 친환경적으로 생체이용률이 뛰어난 유기칼슘을 얻는 기술적 과제를 달성하게 되었다.The present invention relates to a method of obtaining an organic calcium by diluting an organic acid in an appropriate concentration of crustacean shell, and then reacting for a predetermined time, filtering the reactant to remove the supernatant and the shell, and filtering and filtering the filtrate with Whatman paper. By the above method, the technical problem of achieving organic calcium having excellent bioavailability is easily and efficiently and environmentally friendly.

본 발명은 갑각류의 껍질로부터 유기산칼슘을 제조하는 방법에 관한 것이다. 더욱 상세하게는 본 발명은 갑각류의 껍질로부터 키틴의 제조공정 중 부산물로서 발생하는 칼슘을 보다 효율적으로 회수하여 활용하기 위한 방법에 관한 것으로, 본 발명의 방법에 따르면, 갑각류의 껍질에 유기산을 첨가하고 일정 시간 반응시킨 것을 여과시켜 상등액과 껍질은 제거하고 그 여과액을 정제하여 간편하고 효율적으로 유기산칼슘을 얻을 수 있다.The present invention relates to a method for producing calcium carbonate from shells of crustaceans. More specifically, the present invention relates to a method for more efficiently recovering and utilizing calcium generated as a by-product of chitin production from shells of crustaceans. According to the method of the present invention, organic acids are added to shells of shellfish and After the reaction for a certain time, the supernatant and the shell are removed, and the filtrate can be purified to simply and efficiently obtain the organic calcium acid.

본 발명에서는 유기산을 이용하여 갑각류 껍질을 녹이고 분해시켜 순도가 높은 유기산칼슘을 얻을 수 있다. 유기산으로는 구연산칼슘, 말산칼슘, 젖산칼슘, 초산칼슘, 피루브산칼슘, 글루콘산칼슘 등을 이용할 수 있으며, 첨가되는 유기산의 농도는 1-10%가 바람직하고 유기산 첨가 후 반응에 필요한 방치 시간은 12-36시간 이 바람직하다.In the present invention, organic calcium can be obtained by dissolving and decomposing crustacean shells using organic acids. As the organic acid, calcium citrate, calcium malate, calcium lactate, calcium acetate, calcium pyruvate, calcium gluconate, etc. may be used, and the concentration of the organic acid added is preferably 1-10%. -36 hours is preferred.

갑각류의 껍질에 유기산을 투입한 후 증류수를 붓고 유기산 농도를 조절하여 일정 시간 반응시키면, 탄산가스가 거품과 함께 발생하며 탄산칼슘이 분해되고 유기산칼슘이 형성된다. 반응물을 여과시켜 상등액과 갑각류 껍질은 제거하고, 여과액을 정제하여 유기산칼슘을 얻을 수 있는데, 이때 남은 탈회분 갑각류 껍질은 탈단백 공정을 거쳐 키틴을 제조하는데 이용할 수 있다.After the organic acid is added to the shell of the crustacean, distilled water is poured and the organic acid is adjusted to react for a predetermined time. Carbon dioxide is generated together with bubbles, calcium carbonate is decomposed and organic calcium is formed. The reaction product is filtered to remove supernatant and crustacean shells, and the filtrate can be purified to obtain organic calcium calcium. The remaining deashed crustacean shell can be used to prepare chitin through a deproteinization process.

이러한 방법에 의해 얻어진 유기산칼슘은 무기칼슘에 비해 생체이용률이 뛰어나 항응고제(anticoagulation), 골다공증(osteoporosis) 방지제 등으로 유용하게 이용할 수 있을 뿐만 아니라, 본 발명의 제조방법은 염산을 처리하는 기존 방법에 비해 공정이 효율적이고 간편하며 환경 오염이 적다.The organic acid calcium obtained by such a method has excellent bioavailability compared to inorganic calcium, so that it can be usefully used as an anticoagulation agent, an osteoporosis prevention agent, and the like. The process is efficient and simple, and there is little environmental pollution.

따라서 본 발명은 폐기물인 갑각류 껍질의 자원으로서의 이용 가치를 한층 더 발전시켰으며, 생체이용률이 뛰어난 유기칼슘을 의료용 소재 또는 공산품 제조의 원료로 사용할 수 있고, 환경오염을 감소시키는 등 여러 가지 유리한 효과를 나타낸다.Therefore, the present invention has further developed the value of use as a resource of crustacean shell, which is a waste, and can use organic calcium having excellent bioavailability as a raw material for the manufacture of medical materials or industrial products, and reduce environmental pollution. Indicates.

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 1Example 1

약 5g의 게 껍질을 깨끗한 소금물에 넣고 1시간 끊여 미생물을 살균하고 각 종 오물을 제거한 다음 200 mL 비이커에 넣고 여기에 1.5-4.5g의 구연산을 넣고 증류수 50 ml를 첨가하여 (구연산 농도 3.0-9.0%) 게 껍질이 전부 용액에 잠기도록 했다.Put about 5g of crab shell in clean brine and cut for 1 hour to sterilize microorganisms, remove all kinds of dirt, put in 200 mL beaker, add 1.5-4.5g citric acid and add 50ml of distilled water (citric acid concentration 3.0-9.0 %) All the crab shells were submerged in solution.

이를 서서히 반응시키면 탄산가스(CO2)가 거품과 함께 끊어 오르면서 탄산칼슘이 분해되기 시작한다. 이때 불순물 등은 제거되고 구연산칼슘(Calcium citrate)이 형성된다. 이러한 반응을 위해 상온에서 하룻밤 방치시켰다. 그런 다음, 상등액과 탈회분 게 껍질을 200메쉬 여과망으로 분리하여, 탈회분 게 껍질은 별도로 키틴 제조에 이용하고, 여과액은 다시 와트만여과지(#6)로 여과 후 남은 고형물을 증류수로 세척 후 와트만여과지(#6)로 재여과시켜 구연산칼슘을 정제하였다. 이를 60℃ 에서 건조시켰다. 정제된 구연산칼슘(구연산염) 함량은 하기 표 1에 나타내었다. 구연산염 회수율(%)은, "(초기 회분의 양 - 반응후 회분의 양)"으로 구해지는 용해된 탄산칼슘량에 대한 구연산염(구연산칼슘) 양의 비율로써 산정하였다.When slowly reacted, the carbon dioxide (CO 2 ) breaks up with bubbles and calcium carbonate begins to decompose. At this time, impurities and the like are removed and calcium citrate is formed. It was left overnight at room temperature for this reaction. Then, the supernatant and the demineralized crab shell are separated by a 200 mesh filter net, and the demineralized crab shell is separately used for the preparation of chitin, and the filtrate is again filtered through Whatman filter paper (# 6), and the remaining solids are washed with distilled water. Calcium citrate was purified by refiltration with Whatman filter paper (# 6). It was dried at 60 ° C. The purified calcium citrate (citrate) content is shown in Table 1 below. Citrate recovery (%) was calculated as the ratio of the amount of citrate (calcium citrate) to the amount of dissolved calcium carbonate obtained as "(initial amount of ash-amount of ash after reaction)".

갑각류 껍질의 탈회 정도 및 구연산염 생산량Degree of demineralization of crustacean shells and citrate production 구연산 농도(%)Citric Acid Concentration (%) 게껍질 양(g)Crab shell amount (g) 회분함량(%)Ash content (%) 초기 pHInitial pH 최종 pHFinal pH 반응후 건물량(g)Dry weight after reaction (g) 반응후 회분함량(%)Ash content after reaction (%) 구연산염 양(g)Citrate amount (g) 구연산염 회수율(%)Citrate recovery rate (%) 33 5.05.0 46.5646.56 1.921.92 7.747.74 4.694.69 39.9139.91 0.140.14 30.6930.69 66 5.05.0 46.5646.56 1.721.72 3.763.76 4.244.24 30.9330.93 0.510.51 50.1750.17 99 5.05.0 46.5646.56 1.621.62 2.942.94 3.793.79 23.0523.05 0.760.76 52.2652.26

실시예 2Example 2

구연산 대신 유기산인 3-6% 말산(malic acid)을 사용하여 상기 실시예 1과 같은 방법으로 처리한 결과, 얻어진 말산칼슘(말산염) 함량은 하기 표 2에 나타내었다.As a result of treatment in the same manner as in Example 1 using 3-6% malic acid instead of citric acid, the resulting calcium malate (malate) content is shown in Table 2 below.

갑각류 껍질의 탈회 정도 및 말산염 생산량Demineralization degree and malate production of crustacean shells 말산 농도(%)Malic acid concentration (%) 게껍질 양(g)Crab shell amount (g) 회분함량(%)Ash content (%) 초기 pHInitial pH 최종 pHFinal pH 반응후 건물량(g)Dry weight after reaction (g) 반응후 회분함량(%)Ash content after reaction (%) 말산염 양(g)Malate amount (g) 말산염 회수율(%)Malate recovery (%) 33 5.05.0 46.5646.56 1.891.89 7.027.02 3.243.24 35.5135.51 0.680.68 57.7557.75 66 5.05.0 46.5646.56 1.731.73 3.883.88 2.412.41 12.6912.69 0.790.79 39.0739.07 99 5.05.0 46.5646.56 1.561.56 3.663.66 1.951.95 5.135.13 0.520.52 23.3423.34

구연산 및 말산 처리 후 얻어진 건물을 1.25N NaOH로 90-100℃에서 3시간 반응 후 얻어진 키틴의 주요성분 및 수율은 하기 표 3에 나타내었다.The main components and yields of the chitin obtained after the reaction of citric acid and malic acid obtained with 1.25N NaOH at 90-100 ° C. for 3 hours are shown in Table 3 below.

갑각류 껍질의 탈회, 탈단백 정도 및 키틴의 생산량Demineralization of shellfish shells, degree of deproteinization and production of chitin 유기산 종류Organic acid type 유기산 농도(%)Organic acid concentration (%) 단백질 함량(%)Protein content (%) 회분 함량(%)Ash content (%) 아세틸화도(%)Acetylation degree (%) 분자량(MW)Molecular Weight (MW) 키틴 수율(%)Chitin yield (%) 구연산 처리Citric acid treatment 99 0.370.37 0.270.27 90.7990.79 4.5 x 108 4.5 x 10 8 22.622.6 말 산 처리Horse acid treatment 99 0.200.20 0.160.16 91.2591.25 5.0 x 108 5.0 x 10 8 24.924.9

본 발명에 의해 얻어진 유기산칼슘은 무기칼슘에 비해 생체이용률이 뛰어나 항응고제(anticoagulation), 골다공증(osteoporosis) 방지제 등으로 유용하게 이용할 수 있을 뿐만 아니라, 본 발명의 제조방법은 염산을 처리하는 기존 방법에 비해 공정이 효율적이고 간편하며 환경 오염이 적다.The organic acid calcium obtained by the present invention has excellent bioavailability compared to inorganic calcium, and thus can be usefully used as an anticoagulation agent, an osteoporosis preventing agent, etc. The process is efficient and simple, and there is little environmental pollution.

따라서 본 발명은 폐기물인 갑각류 껍질의 자원으로서의 이용 가치를 한층 더 발전시켰으며, 생체이용률이 뛰어난 유기칼슘을 다양한 의료용 소재 또는 공산 품 제조의 원료로 사용할 수 있고, 환경오염을 감소시키는 등 여러 가지 유리한 효과를 나타내므로, 이는 자원 산업상 매우 유용한 발명인 것이다.Therefore, the present invention has further developed the value of use as a resource of crustacean shell, which is a waste, and can use organic calcium having excellent bioavailability as a raw material for manufacturing various medical materials or industrial products, and reducing environmental pollution. As effective, this is a very useful invention for the resource industry.

Claims (3)

갑각류의 껍질에 유기산 1-10%를 첨가하여 12-36시간 방치하고; 반응물을 여과시켜 상등액과 갑각류 껍질을 분리·제거하고; 여과액을 와트만페이퍼로 여과시켜 정제하는 단계를 포함하는 것을 특징으로 하는, 갑각류 껍질로부터 유기산칼슘의 제조 방법.1-10% of organic acids were added to the shell of the shellfish and left for 12-36 hours; Filtering the reaction to separate and remove the supernatant and crustacean shell; And filtering the filtrate with watman paper to purify it. 갑각류 껍질에 유기산 1-10%를 첨가하여 12-36시간 방치하고; 반응물을 여과시켜 상등액과 갑각류 껍질을 분리하고; 분리된 갑각류 껍질을 탈단백하는 단계를 포함하는 것을 특징으로 하는, 갑각류 껍질로부터 키틴의 제조 방법.1-10% of organic acids were added to the shell of crustacean and left for 12-36 hours; Filtering the reaction to separate supernatant and crustacean shell; Method for producing chitin from crustacean shell, characterized in that it comprises the step of deproteinizing the separated shellfish shell. 제1항 또는 제2항에 있어서, 유기산으로 구연산 또는 말산을 첨가하는 것을 특징으로 하는 방법.The method according to claim 1 or 2, wherein citric acid or malic acid is added to the organic acid.
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KR100876921B1 (en) 2007-09-21 2009-01-07 주식회사 경희매니지먼트컴퍼니 Method for tenderizing shell of crustacean or animal horny substance
KR101206855B1 (en) 2009-12-31 2012-11-30 박응렬 Method For Obtaining Chitin And Chitosan
CN110724211A (en) * 2019-10-31 2020-01-24 汕尾市海洋产业研究院 High-value comprehensive utilization method of shrimp and crab shells based on reducing sugar catalytic oxidation and application thereof

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KR100876921B1 (en) 2007-09-21 2009-01-07 주식회사 경희매니지먼트컴퍼니 Method for tenderizing shell of crustacean or animal horny substance
KR101206855B1 (en) 2009-12-31 2012-11-30 박응렬 Method For Obtaining Chitin And Chitosan
CN110724211A (en) * 2019-10-31 2020-01-24 汕尾市海洋产业研究院 High-value comprehensive utilization method of shrimp and crab shells based on reducing sugar catalytic oxidation and application thereof
CN110724211B (en) * 2019-10-31 2021-09-17 汕尾市海洋产业研究院 High-value comprehensive utilization method of shrimp and crab shells based on reducing sugar catalytic oxidation and application thereof

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