KR20010025932A - Preparation method by ultrasonication of microcrystalline chitosan - Google Patents

Preparation method by ultrasonication of microcrystalline chitosan Download PDF

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KR20010025932A
KR20010025932A KR1019990037005A KR19990037005A KR20010025932A KR 20010025932 A KR20010025932 A KR 20010025932A KR 1019990037005 A KR1019990037005 A KR 1019990037005A KR 19990037005 A KR19990037005 A KR 19990037005A KR 20010025932 A KR20010025932 A KR 20010025932A
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chitosan
solution
crystalloid
powder
fine
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KR1019990037005A
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Korean (ko)
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문상돈
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문상돈
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024Homoglycans, 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
    • C08B37/00272-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003Chitin, 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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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Materials For Medical Uses (AREA)

Abstract

PURPOSE: A manufacturing process of fine crystalloid chitosan through ultrasonic treatment is provided, which is so economical method that high water retention value, various type of paste or powder, bio-degradability, bio-activity, high reactivity and chelating property are gained. CONSTITUTION: The manufacturing process is composed of: shaking chitosan powder in acetic acid solution at 20deg.C for 4 hours to get polymer solution, and removing insoluble chitosan particles by filtering the polymer solution; pyrolyzing the chitosan solution at 70deg.C for 1-3 hours by irradiating ultrasonic wave, and cooling immediately; undergoing the process of polymer coagulation of glucosamine, titrating chitosan solution with NaOH solution and controlling the pH to be 8.0 at 20±0.1deg.C while shaking at 150rpm to prepare fine crystalloid chitosan hydrogel; washing the precipitate with distilled water, drying the hydrogel at 60deg.C with a vacuum dryer or an air spray dryer; and obtaining fine crystalloid chitosan powder.

Description

초음파처리를 통한 미세결정질 키토산 제조방법.{Preparation method by ultrasonication of microcrystalline chitosan}{Preparation method by ultrasonication of microcrystalline chitosan}

미세결정질 키토산의 제조공정 영향을 미치는 인자 키토산 초기성질, 분해공정, 응집공정, 건조공정을 통한 경제적인 제조방법.Factors Affecting the Manufacturing Process of Microcrystalline Chitosan Economical manufacturing method through initial properties of chitosan, decomposition process, flocculation process and drying process.

미세결정질 키토산의 제조는 유기산 수용액으로부터 글루코사민 고분자 응집에 의해 제조할 수 있다. 용액으로부터 발생한 두 가지 발생한 형태는The preparation of microcrystalline chitosan can be prepared by glucosamine polymer aggregation from an aqueous organic acid solution. Two types of outbreaks from solution

1) 수용액에 분산한 젤라틴 같은 특성은 보수성값(water retention valve)이 보통범위가 500-2,000%이다.1) Gelatin-like properties dispersed in aqueous solution usually have a water retention valve of 500-2,000%.

2) 파우더의 보수성값 범위는 200-800%이다.2) The water retention value range of the powder is 200-800%.

미세결정질 셀룰로오스이래 발견된 새로운 미세결정질 고분자로서 둘다 천연에서 합성되었고, 미세결정질 고분자 제조방법은 물리적, 화학적 공정에 의한 추출과 용액으로부터 고분자의 응집, 또는 분산, 응고, 침전, 결정화 방법에 의해서 제조될 수 있다.New microcrystalline polymers discovered since microcrystalline cellulose are both synthesized in nature, and microcrystalline polymer production methods can be prepared by extraction by physical and chemical processes and by agglomeration or dispersion, coagulation, precipitation and crystallization of polymers from solution. Can be.

미세결정질 키틴은 처음으로 미세결정질 셀룰로오스 공정에서 고안된 염산을 사용하여 가수분해와 분해에 의한 비질서한 상을 제거하여 제조한다. 또한 2-프로판올 용액에 인산을 첨가 후 가수분해 공정을 통해 더 효과적인 미세결정질 키틴을 제조할 수 있다.Microcrystalline chitin is prepared for the first time using hydrochloric acid designed in the microcrystalline cellulose process to remove the disordered phase by hydrolysis and degradation. In addition, the addition of phosphoric acid to the 2-propanol solution through the hydrolysis process can be produced a more effective microcrystalline chitin.

키토산은(poly-d-glucosamine)은 키틴을 알카리용액하에서 N-탈아세틸화 반응에 온도 산출에 따라서 지금까지 미세결정질 형태는 충분하지 않다.Poly-d-glucosamine is a microcrystalline form of chitin according to the temperature calculation for the N-deacetylation reaction under alkaline solution.

미세결정질 키토산 제조공정 의미는 고분자 응집, 응고, 중화적정 현상수를 포함하여 알칼리 용액의 재생이다. 생산물의 특성은 주로 초기 원료 물질로부터 다른 거대분자구조이다.The process for producing microcrystalline chitosan means the regeneration of the alkaline solution, including polymer coagulation, coagulation and neutralization titration water. The properties of the product are large macromolecular structures, which differ mainly from the initial raw materials.

미세결정질 키토산 특성은 제조공정의 여러 가지 인자에 의존한다.Microcrystalline chitosan properties depend on many factors in the manufacturing process.

미세결정질 키토산 성질 = (가, 나, 다, 라.‥)Microcrystalline Chitosan Properties = (A, B, C, D)

가 = 키토산 초기 성질, 나 = 분해공정 인자, 다 = 응집공정 인자, 라 = 건조공정 인자A = initial property of chitosan, b = decomposing process factor, c = coagulation process factor, d = drying process factor

공정은 글루코사민 고분자 응집, 키토산염의 중화적정 발생사 응고 그리고 침전된 히드로겔이 수반된다.The process involves glucosamine polymer agglomeration, neutralization titration of chitoates, and precipitated hydrogels.

미세결정질 키토산 제조는 키토산 분말 0.5-2w/w% 농도의 2-4%부피농도 아세트산 수용액에 20℃에서 4시간 교반하여 고분자 용액을 얻는다.The preparation of microcrystalline chitosan was stirred for 4 hours at 2-4% by volume acetic acid aqueous solution of chitosan powder at 0.5-2w / w% concentration to obtain a polymer solution.

고분자 용액을 여과하여 녹지 않는 키토산 입자를 제거한다.The polymer solution is filtered to remove insoluble chitosan particles.

키토산 용액을 열분해 공정으로서 초음파 기를 이용한다.The chitosan solution is used as an ultrasonic wave as a pyrolysis process.

초음파 항온조 온도 70℃에서 1-3시간, 초음파 15-35㎑로 조사하여 열분해 한다. 열분해 후 즉시 냉각한다. 미세결정질 키토산 히드로겔 제조는 글루코사민 고분하자응집를 거쳐 NaOH수용액 2.95-29.5%농도로 키토산 용액 20±0.1℃에서 150rpm으로 교반하면서 pH8.0까지 적정한다.Pyrolysis is performed by ultrasonic irradiation at 70 ℃ for 1-3 hours and ultrasonic 15-35 초음파. Cool immediately after pyrolysis. The preparation of microcrystalline chitosan hydrogel is titrated to pH 8.0 while stirring at 150 rpm at 20 ± 0.1 ° C. in a chitosan solution with a NaOH aqueous solution of 2.95-29.5% via glucosamine polyhedron coagulation.

침전된 생산물은 증류수로 수세하여 세정하고, 히드로겔 생산물은 60℃에서 진공건조 또는 에어스프레이 건조기로 건조하면 미세결정질 키토산파우더를 얻을 수 있다.The precipitated product is washed with distilled water and washed, and the hydrogel product is dried by vacuum drying or air spray dryer at 60 ° C. to obtain a microcrystalline chitosan powder.

미세결정질 키토산 경제적으로 제조할 수 있다.Microcrystalline chitosan can be produced economically.

미세결정질 키토산 특징Microcrystalline Chitosan Features

- 높은 수소결합 능력-High hydrogen bonding capacity

- 높은 고유의 표면-High intrinsic surface

- 높은 보수성값-High conservative value

- 분산 안전성Distributed safety

- 고체형태의 결정도 지수 95%-95% crystallinity index in solid form

- 다양한 형태의 겔같은 페이스트, 파우더-Gel-like pastes and powders in various forms

- 생분해성-Biodegradable

- 생활성도-Lifeliness

- 직접적으로 필름 형성 능력-Film forming ability directly

- 높은 반응성, 킬레이트 성질High reactivity, chelate properties

Claims (1)

초음파처리를 통한 미세결정질 키토산 제조방법Microcrystalline Chitosan Production Method by Ultrasonication
KR1019990037005A 1999-09-01 1999-09-01 Preparation method by ultrasonication of microcrystalline chitosan KR20010025932A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100418682B1 (en) * 2001-05-22 2004-02-11 장태순 Method for Isolation and purification of high molecular weight chitosan by using ultrasonic processing
KR20040018890A (en) * 2002-08-27 2004-03-04 최종욱 The method of manufacturing chitin oligoer powder and food composition comprising chitin oligomer powder for improving liver activity
KR100445667B1 (en) * 2001-04-11 2004-08-21 임우진 Manufacturing method for water-soluble chitosan having high molecular weight
CN103204956A (en) * 2013-04-11 2013-07-17 天津天狮生物发展有限公司 Preparation method of chitosan
CN114988951A (en) * 2022-06-21 2022-09-02 广西南宁昇华农业科技有限公司 Water-soluble fertilizer for improving fruit quality

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100445667B1 (en) * 2001-04-11 2004-08-21 임우진 Manufacturing method for water-soluble chitosan having high molecular weight
KR100418682B1 (en) * 2001-05-22 2004-02-11 장태순 Method for Isolation and purification of high molecular weight chitosan by using ultrasonic processing
KR20040018890A (en) * 2002-08-27 2004-03-04 최종욱 The method of manufacturing chitin oligoer powder and food composition comprising chitin oligomer powder for improving liver activity
CN103204956A (en) * 2013-04-11 2013-07-17 天津天狮生物发展有限公司 Preparation method of chitosan
CN103204956B (en) * 2013-04-11 2016-09-07 天津天狮生物发展有限公司 A kind of preparation method of chitosan
CN114988951A (en) * 2022-06-21 2022-09-02 广西南宁昇华农业科技有限公司 Water-soluble fertilizer for improving fruit quality

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