KR960005426B1 - Method of preparation of carboxymethylcellulose with steam-explosion wood - Google Patents

Method of preparation of carboxymethylcellulose with steam-explosion wood Download PDF

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Publication number
KR960005426B1
KR960005426B1 KR1019920022757A KR920022757A KR960005426B1 KR 960005426 B1 KR960005426 B1 KR 960005426B1 KR 1019920022757 A KR1019920022757 A KR 1019920022757A KR 920022757 A KR920022757 A KR 920022757A KR 960005426 B1 KR960005426 B1 KR 960005426B1
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South Korea
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wood
pokswae
cmc
wood chips
stirred
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KR1019920022757A
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Korean (ko)
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KR940011483A (en
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이종윤
장준복
한상열
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이종윤
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21BFIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
    • D21B1/00Fibrous raw materials or their mechanical treatment
    • D21B1/02Pretreatment of the raw materials by chemical or physical means
    • D21B1/021Pretreatment of the raw materials by chemical or physical means by chemical means
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21BFIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
    • D21B1/00Fibrous raw materials or their mechanical treatment
    • D21B1/04Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

Wood chips are finely crushed under 25-30 kg/cm2 press. and at 220-250 deg.C for 3-9 minutes. Dis-lignification of fine crushed wood chips is achilved by mixing the chips in 1-2 % sodium chlorite sol. agitating for 2 hours at ambient temp. Next Carboxymethyl cellulose(CMC) manufacturing process follows a known method : mixing in iso-propyl alcohol, adding and NaOH mono chloro acetic anhydride cooling, filtering, mixing with MeOH, neutralizing, purifying and drying. Compared with the conventional method, the method simplifies CMC process economically by skipping the pulping of wood.

Description

폭쇄처리한 목재로 카르복시메칠셀룰로오스(CMC)를 제조하는 방법Method for preparing Carboxymethyl Cellulose (CMC) from fired wood

본 발명은 목재를 폭쇄하고 폭쇄된 목재 그대로 또는 이를 탈리그닌(lignin)처리한 다음 CMC(Carboxymethyl Cellulose)를 제조하는 CMC제조방법에 관한 것이다.The present invention relates to a CMC manufacturing method for producing a CMC (Carboxymethyl Cellulose) after crushing the wood and the lignin treatment of the crushed wood as it is.

CMC는 점성을 부여하는 물질로서 인체에 무해하므로 식품첨가물, 화장품, 합성세제, 날염, 제지 및 굴착용 첨가제등 여러분야에서 많이 사용되고 있는 것이다.CMC is a substance that gives viscosity and is harmless to the human body, so it is widely used in food additives, cosmetics, synthetic detergents, printing, papermaking and excavating additives.

그러나 종래에는 CMC를 면 또는 목재펄프를 사용하여 제조하였기 때문에 재료비가 비싸고 공정이 복잡한 문제가 있었다.However, conventionally, since the CMC is manufactured using cotton or wood pulp, the material cost is high and the process is complicated.

목화를 면으로 제조하기까지 많은 공정이 소요되며 펄프 역시 목재를 펄프화하는데 많은 공정이 필요하므로 이러한 공정을 거쳐서 된 면 또는 펄프를 다시 CMC로 제조하는 것은 전체적으로 너무나 많은 공정이 소요되어 비경제적일 뿐 아니라 목화나 펄프용 목재는 모두 폐자원이 아닌 자연자원으로서 구입비도 많이 들게 되므로 결국 이들을 CMC로 제조하는 것은 매우 비경제적인 문제가 있는 것이었다.It takes a lot of processes to make cotton into cotton and pulp also requires a lot of processes to pulverize wood, so manufacturing cotton or pulp back into CMC through such a process is too costly as a whole. However, both cotton and pulp wood are natural resources rather than waste resources, so they are expensive to purchase. Therefore, manufacturing them with CMC was a very uneconomic problem.

본 발명은 목재를 펄프화하지 않고 폭쇄처리한 다음 폭쇄처리된 그대로 또는 탈리그닌화하여 CMC를 제조하므로 종래의 제조방법에 비하여 전체공정이 훨씬 단축되어 간단할 뿐아니라 특히 목재는 간벌재나 목재를 가공하는 공장에서 나오는 폐목재를 사용하여 CMC를 제조할 수 있어 가격이 매우 저렴하게 됨은 물론 많은 폐자원을 재활용하게 되는 효과가 있는 것이다.According to the present invention, the CMC is produced by pulverizing the wood without pulping and then pulverizing it as it is or by delignining, so that the whole process is much shorter and simpler than the conventional manufacturing method. CMC can be manufactured using the waste wood from the plant, which is very inexpensive, and has the effect of recycling many waste resources.

다시말하면, 본 발명은 주로 폐목재를 일정크기로 잘라서 된 목재칩을 폭쇄기에 넣어 폭쇄하고 폭쇄된 목재 그대로 또는 탈리그닌화하고 이 탈리그닌화한 목재를 공지의 방법으로 CMC로 제조하는 것이다.In other words, the present invention is mainly to put the wood chips cut into a certain size of the waste wood in a crusher and to crush the crushed wood as it is or ligignized and the ligignized wood by CMC in a known method.

본 발명을 실시예에 따라 공정별로 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail with reference to Examples.

[제1공정][Step 1]

폐목재를 일정크기로 잘라서 된 목재칩을 폭쇄기에 넣어 폭쇄한다.The wood chips cut to a certain size are put into a crusher and crushed.

[제2공정][Step 2]

폭쇄된 목재 10gm을 1-2% 아염소산나트륨 용액 500ml와 함께 용기에 넣고 실온에서 약 2시간 교반하여 탈리그닌화 후 유리여과기로 여과하고 물로 충분히 세정하고 건조하여 탈리그닌 공정을 완료한다.10 gm of the crushed wood is placed in a container with 500 ml of 1-2% sodium chlorite solution, stirred at room temperature for about 2 hours, deligignized, filtered through a glass filter, thoroughly washed with water, and dried to complete the delignin process.

[제3공정][Step 3]

제1공정에서 폭쇄된 목재 또는 제2공정에서 탈리그닌화 한 폭쇄목재 10g을 80% 이소프로필알코올(Isopropylaloohol) 250ml에 넣고 충분히 교반한 후 실온에서 30분에 걸쳐 30% NaOH 수용액 50ml를 첨가하고 다시 60분간 교반한 다음 모노클로로초산(monochloroacetioacid) 5.5g을 30분간에 걸쳐 첨가하고 반응물을 55℃의 욕조에서 3시간 방치하여 냉각후 반응물을 유리여과기로 흡인 여과한 다음 80% 메탄올 200ml중에 교반하면서 재분산시킨후 과잉의 알카리를 제거하기 위하여 90% 초산을 첨가하여 중화시키고 다시 반응물을 80% 메탄올 200ml로 3회 반복 세정한 후 무수 메탄올 200ml로 세정한 다음 생성물을 60℃ 오븐(dry oven)에서 건조하므로서 본 발명이 완성된다.10 g of the wood crushed in the first process or the deignified wood in the second process is placed in 250 ml of 80% isopropylaloohol, stirred sufficiently, and then 50 ml of 30% aqueous NaOH solution is added over 30 minutes at room temperature, and again. After stirring for 60 minutes, 5.5 g of monochloroacetioacid was added over 30 minutes, and the reaction was allowed to stand for 3 hours in a 55 ° C bath. After cooling, the reaction was filtered by suction with a glass filter and then stirred in 200 ml of 80% methanol. After dispersing, neutralize by adding 90% acetic acid to remove excess alkali, and then the reaction was washed three times with 200 ml of 80% methanol, washed with 200 ml of anhydrous methanol, and the product was dried in a 60 ° C. oven. Thus, the present invention is completed.

폭쇄시의 온도와 압력조건은 목재의 종류에 따라 다르나 예를 들면 아래의 표(1)과 같다.Temperature and pressure conditions at the time of explosion vary depending on the type of wood, but are shown in Table (1) below.

[표 1]TABLE 1

이와 같이 본 발명은 폐목재를 폭쇄처리하여 공지의 방법으로 CMC를 제조하므로 상당한 공정을 거쳐 얻을 수 있는 면 또는 펄프로 제조하는 종래의 제조방법에 비하여 제조공정이 간단하고 재료비가 적게 들며 폐자원을 활용할 수 있는 등의 효과가 있는 것이다.As described above, the present invention manufactures CMC by a well-known method by treating waste wood with a known method, so that the manufacturing process is simpler and the material cost is lower than that of conventional manufacturing method of cotton or pulp that can be obtained through a considerable process. It can be used to effect.

Claims (2)

목재 또는 폐목재를 일정크기로 잘라서 된 목재칩을 폭쇄기에 넣어 폭쇄압력 25kg∼30kg/cm2, 폭쇄온도 220∼250℃, 폭쇄시간 3∼9분의 조건으로 폭쇄하고 폭쇄된 목재칩을 아염소산나트륨용액과 교반하여 탈리그닌화하고 탈리그닌화한 목재칩을 통상의 CMC제조방법과 같이 이소프로필알코올에 넣고 충분히 교반한 후 NaOH수용액을 첨가하여 다시 교반하고 모노클로로초산을 첨가한 다음 반응물을 일정시간 방치하여 냉각되게 하고 냉각된 반응물을 여과기로 여과한 다음 메탄올에 넣고 교반하여 재분산시킨 후 초산을 첨가하여 중화시키고 다시 반응물을 메탄올로 3회 반복 세정한 후 생성된 생성물을 건조용 오븐으로 건조하여 제조하는 폭쇄처리한 목재로 카르복시메칠셀룰로오스(CMC)를 제조하는 방법.Oh the wood or wood waste into the groups pokswae the wood chips by cutting into a predetermined size pokswae pressure 25kg~30kg / cm 2, temperature of 220~250 pokswae ℃, pokswae time 3-9 minutes the wood chips and pokswae pokswae under the conditions of acid Stirring with sodium solution and then deignignized and deignignized wood chips into isopropyl alcohol as in the conventional CMC preparation method, stirred well, and stirred again with the addition of aqueous NaOH solution, followed by addition of monochloroacetic acid. The mixture was left to cool for a while, and the cooled reactant was filtered through a filter, stirred and redispersed in methanol, neutralized by addition of acetic acid, and the reaction was repeatedly washed three times with methanol, and the resulting product was dried in a drying oven. Method for producing carboxymethyl cellulose (CMC) from the fired wood to be prepared by. 제1항에 있어서, 폭쇄처리된 목재칩을 1∼2% 아염소산나트륨용액과 함께 용기에 넣고 실온에서 약 2시간 동안 교반하여 탈리그닌화함을 특징으로 하는 폭쇄처리한 목재로 카르복시메칠셀룰로오스(CMC)를 제조하는 방법.The method of claim 1, wherein the crushed wood chips are placed in a container with 1-2% sodium chlorite solution and stirred for about 2 hours at room temperature to deligignize carboxymethylcellulose (CMC). ) Method of making).
KR1019920022757A 1992-11-28 1992-11-28 Method of preparation of carboxymethylcellulose with steam-explosion wood KR960005426B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113582756A (en) * 2021-08-03 2021-11-02 中诚国联(河南)生物科技有限公司 Pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113582756A (en) * 2021-08-03 2021-11-02 中诚国联(河南)生物科技有限公司 Pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and application thereof

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