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KR100364899B1 - Dry Crusher for Cellulose Ether Production - Google Patents

Dry Crusher for Cellulose Ether Production Download PDF

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KR100364899B1
KR100364899B1 KR1019950020135A KR19950020135A KR100364899B1 KR 100364899 B1 KR100364899 B1 KR 100364899B1 KR 1019950020135 A KR1019950020135 A KR 1019950020135A KR 19950020135 A KR19950020135 A KR 19950020135A KR 100364899 B1 KR100364899 B1 KR 100364899B1
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cellulose ether
cellulose
raw material
air
particles
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KR970005396A (en
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이병주
이상구
노경록
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삼성정밀화학 주식회사
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/11High-speed drum mills
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00Disintegrating plant with or without drying of the material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C25/00Control arrangements specially adapted for crushing or disintegrating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B17/00Apparatus for esterification or etherification of cellulose
    • C08B17/06Apparatus for esterification or etherification of cellulose for making cellulose ethers

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

본 발명은 분쇄기 중앙에 원료공급기 (3)에서 유입된 공기와 원료를 회전시키기 위한 회전판(7)과 선별된 미립자를 분리하는 분리기 (1)와 큰입자를 제거하는 입자 제거관(4), 유도장치 (5) 및 라이너 (6)로 구성된 셀룰로오스에테르 제조용 건조분쇄기에 관한 것이다.The present invention is a rotary plate (7) for rotating the raw material and the air introduced from the raw material feeder (3) in the center of the mill, a separator (1) for separating the selected fine particles and particle removal tube (4) for removing large particles, induction It relates to a dry crusher for producing cellulose ethers composed of an apparatus (5) and a liner (6).

Description

셀룰로오스에테르 제조용 건조분쇄기Dry Crusher for Cellulose Ether Production

본 발명은 분쇄기 내부의 온도상승을 억제하여 셀룰로오스에테르 유도체의 변성을 막아주면서, 셀룰로오스에테르의 입자 크기를 작게 만드는 새로운 셀룰로오스에테르 제조용 건조분쇄기 및 그 사용방법에 관한 것이다.The present invention relates to a novel dry pulverizer for producing cellulose ether and a method of using the same, which reduces the temperature of the inside of the pulverizer and prevents modification of the cellulose ether derivative.

일반적으로, 셀룰로오스에테르는 건축업에서 모르타르, 자갈, 시멘트와 석고의 첨가제, 벽지의 접착제, 금형물질의 충전제, 합성수지의 첨가제 및 합성수지의 표면 처리제로 사용된다. 이때 사용되는 셀룰로오스에테르는 물에 녹일때 덩어리가 지지않고 물에 골고루 퍼져 신속하게 녹아야 한다. 이런 조건을 만족하기 위해서는 셀룰로오스에테르의 물에 대한 용해도가 커야 하는데 물에 대한 용해도는 입자의크기가 균일하게 분포되고 작을수록 좋다. 입자의 크기가 작으면 셀룰로오스에테르 입자의 표면적이 크기 때문에 물에 대한 용해도가 커지고, 벌크 밀도가 작아져서 포장시 부피가 작아지므로 유리하다.In general, cellulose ether is used in the construction industry as an additive of mortar, gravel, cement and gypsum, adhesive of wallpaper, filler of mold material, additive of synthetic resin and surface treatment agent of synthetic resin. At this time, the cellulose ether used should not dissolve in water and spread quickly in water evenly. In order to satisfy these conditions, the solubility of cellulose ether in water must be large, so that the solubility in water is more uniformly distributed and smaller in particle size. Small particle size is advantageous because the surface area of the cellulose ether particles is large, so that the solubility in water is increased, the bulk density is small, and the volume is small during packaging.

셀룰로오스에테르의 분쇄방법에 관해서는 여러문헌에 개시된 바 있으나, 이중 특허문헌에 개시된 사항을 살펴보면 다음과 같다.A method for pulverizing cellulose ether has been disclosed in various documents, but looking at the matter disclosed in the patent literature as follows.

미국 특허 제4,076,935호에 개시된 셀룰로오스의 분쇄방법은 물과 공기의 존재하에서 바이브레이션밀을 사용하여 셀룰로오스에테르를 분쇄하는 방법을 나타내고 있으나, 이는 분쇄된 셀룰로오스에테르가 약 2∼10중량%의 수분을 포함하게 되어 바람직한 방법은 아니었다.The grinding method of cellulose disclosed in U.S. Patent No. 4,076,935 shows a method of grinding cellulose ether using a vibration mill in the presence of water and air. It was not a preferred method.

영국 공개특허 제2,262,527호에서도 셀룰로오스에테르의 분쇄방법을 개시하고 있으나 이는 셀룰로오스에테르에 30∼80중량%의 수분을 함유하는 습식분쇄방법으로 별도의 건조공정을 요구하는 것으로 실용화되기 어려웠던 것이다.British Patent Publication No. 2,262,527 also discloses a method of pulverizing cellulose ether, which is difficult to be practically required to require a separate drying process by a wet grinding method containing 30 to 80% by weight of water in cellulose ether.

또한 셀룰로오스에테르의 분쇄에 사용되는 종래의 분쇄기로는 볼 밀(ball mill), 로터리 밀(rotary mill), 바이브레이션 밀(vibration mill)등이 사용되었으나 이런 분쇄기도 다음과 같은 문제점을 가지고 있다.In addition, a ball mill, a rotary mill, a vibration mill, and the like are used as conventional mills used for milling cellulose ethers, but such mills also have the following problems.

셀룰로오스에테르는 매우 부서지기 쉬운 물질이어서 연마하기 쉽지만 분진에 의한 폭발 위험성이 높아 매우 위험하므로 비활성 기체하에서 연마작업을 수행해야 하며 ; 폭발을 방지하기 위해 액체 질소 존재하에 연마를 수행해야 하므로, 원가 상승의 요인이 되고 ; 분쇄기의 효율이 낮아 연마작업을 여러번 실시해야 하므로 에너지의 소비자 많고, 연마 도중에 열이 발생하여 셀룰로오스에테르가 변성이 되고 전기적인 전하를 띠게 되어 폭발의 원인도 되며 ; 때로는 연마 도중에 발생하는 열을 줄이기 위해 외부에서 물을 공급하든지 아니면 습기를 포함하고 있는 셀룰로오스에테르를 사용해야 하는 것이었다.Cellulose ether is a very fragile material, which is easy to polish, but it is very dangerous because of the high risk of explosion by dust, so it must be polished under inert gas; Polishing must be carried out in the presence of liquid nitrogen to prevent explosion, which is a factor of cost increase; Low efficiency of the crusher requires a lot of polishing operations, so many consumers of energy, heat is generated during polishing, cellulose ether is denatured and an electric charge, causing explosion; Sometimes it was necessary to supply water from the outside or use cellulose ethers containing moisture to reduce the heat generated during grinding.

따라서 본 발명은 상기한 문제점을 해결하고 건조된 셀룰로오스에테르를 분쇄하기 위해 사용되는 개량된 에어 크러쉬 밀(Air Crush Mill)과 그 사용방법에 관한 것이다.The present invention therefore relates to an improved air crush mill (air crush mill) used to solve the above problems and to pulverize dried cellulose ether and a method of using the same.

일반적으로 에어 크러쉬 밀(ACM) 분쇄기는 셀룰로오스에테르의 분쇄에 부적합한 것으로 알려져 있으나, 본 발명에서는 셀룰로오스에테르의 분쇄를 위해 이를 개조 적용하였다. 액체 질소와 같은 냉매를 사용하지 않고 공기를 사용하여 셀룰로오스에테르의 온도 상승을 억제하고, ACM 분쇄기 자체에서 회전판의 속도에 의해 셀룰로오스에테르의 입자크기 별로 분리할 수 있다. 입자의 크기가 큰 셀룰로오스에테르가 분쇄기 내부에 존재하면 폭발의 위험성이 있는데 본 발명에서는 입자 크기가 큰 것을 분쇄기 밑으로 제거하여 폭발의 위험성을 제거하였다. 이때 얻어진 셀룰로오스에테르 입자크기는 적어도 전체중 60%가 100㎛ 이하 이고, 벌크 밀도는 0.33∼0.35g/ml 이다.In general, an air crush mill (ACM) grinder is known to be unsuitable for crushing cellulose ether, but in the present invention, it is adapted for crushing cellulose ether. The temperature of the cellulose ether can be suppressed by using air without using a refrigerant such as liquid nitrogen, and the particle size of the cellulose ether can be separated by the speed of the rotating plate in the ACM mill itself. There is a risk of explosion when the cellulose ether having a large particle size is present in the grinder. In the present invention, the particle having a large particle size is removed under the grinder to eliminate the risk of explosion. At least 60% of the cellulose ether particle size obtained at this time is 100 micrometers or less, and a bulk density is 0.33-0.35 g / ml.

본 발명에 사용한 개조된 ACM 분쇄기는 셀룰로오스에테르 유도체의 분쇄에 작용할 수 있다. 적용가능한 셀룰로오스에테르에는 알킬, 히드록시알킬, 알킬히드록시알킬과 카르복시알킬 셀룰로오스 등으로 단일 또는 혼합형의 메틸셀룰로오스, 메틸히드록시에틸셀룰로오스, 히드록시프로필메틸셀룰로오스, 에틸셀룰로오스, 에틸히드록시에틸셀룰로오스와 카르복시메틸셀룰로오스를 들수 있다.Modified ACM mills used in the present invention can act on the milling of cellulose ether derivatives. Applicable cellulose ethers include methyl cellulose, methyl hydroxyethyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, ethyl hydroxyethyl cellulose and carboxy, either single or mixed, such as alkyl, hydroxyalkyl, alkyl hydroxyalkyl and carboxyalkyl cellulose. Methyl cellulose can be mentioned.

이하 본 발명의 분쇄기의 구성을 첨부한 도면에 의거 상세히 설명하겠는바 다음과 같다.Hereinafter, the configuration of the grinder of the present invention will be described in detail with reference to the accompanying drawings.

본 발명의 분쇄기는 분쇄기 중앙에 원료공급기(3)에서 유입된 공기와 원료를 회전시키기 위한 회전판(7)과 선별된 미립자를 분리하는 분리기 (1)와 큰입자를 제거하는 입자 제거관(4), 유도장치 (5) 및 라이너 (6)로 구성된 것이다.The mill of the present invention is a rotary plate (7) for rotating the raw material and the air introduced from the raw material feeder (3) in the center of the mill, a separator (1) for separating the selected fine particles and a particle removal tube (4) for removing large particles , Induction device 5 and liner 6.

이하 본 발명의 분쇄기 사용방법은 다음과 같다.Hereinafter, the grinder usage method of the present invention is as follows.

원료공급기 (3)로 주입된 80℃의 원료(2)는 공기 주입기 (8)로 주입된 많은량의 공기에 의해 유동하면서 유도장치 (5)를 따라 분리기 (1)로 이동한다. 강력하게 회전하는 회전판(7)에 의해 입자가 작은 (120㎛ 이하) 셀룰로오스에테르는 배출하여 다음 공정으로 이송하고, 입자크기가 큰 셀룰로오스에테르는 입자 제거관(4)을 통해 밑으로 제거한다. 마모나 과열을 방지하기 위해 회전판과 몸체 사이에 라이너 (6)를 설치한 것이다.The raw material 2 at 80 ° C. injected into the raw material feeder 3 moves to the separator 1 along the induction device 5 while flowing by the large amount of air injected into the air injector 8. The cellulose ether having small particles (120 µm or less) is discharged and transferred to the next process by the strongly rotating rotary plate 7, and the cellulose ether having a large particle size is removed downward through the particle removal tube 4. The liner 6 is installed between the rotor and the body to prevent wear and overheating.

이때 분쇄기내에는 많은량의 공기를 주입하는바 이는 회전판과 분리기에서 발생하는 열을 억제하기 위한 것이며, 본 발명의 분쇄기를 통과한 건조셀룰로오스 입자는 적어도 60% 이상이 100㎛ 이하로 분쇄된다.In this case, a large amount of air is injected into the grinder to suppress heat generated from the rotating plate and the separator. At least 60% or more of the dried cellulose particles passing through the grinder of the present invention is pulverized to 100 µm or less.

제 1도는 본 발명의 셀룰로오스에테르 제조용 건조분쇄기의 구성도이다.1 is a block diagram of a dry grinding machine for producing cellulose ether of the present invention.

* 도면부호의 설명* Explanation of Reference Numbers

1 : 분리기 2 : 원료(80℃인 건조셀룰로오스에테르) 3 : 원료공급기 4 : 입자 제거관 5 : 유도장치 (Gulde ring) 6 : 라이너 (Liner) 7 : 회전판 8 : 공기주입구DESCRIPTION OF SYMBOLS 1 Separator 2 Raw material (dry cellulose ether of 80 degreeC) 3 Raw material feeder 4 Particle removal pipe 5 Gulde ring 6 Liner 7 Rotating plate 8 Air inlet

Claims (5)

분쇄기 중앙에 원료공급기 (3)에서 유입된 공기와 원료를 회전시키기 위한 회전판(7)과 선별된 미립자를 분리하는 분리기 (1)와 큰입자를 제거하는 입자 제거관(4), 유도장치 (5) 및 라이너 (6)로 구성된 셀룰로오스에테르 제조용 건조분쇄기In the center of the mill, a rotary plate (7) for rotating the air and raw material introduced from the raw material feeder (3), a separator (1) for separating the selected fine particles, a particle removal tube (4) for removing large particles, and an induction device (5). ) And liner (6) for drying cellulose ethers 제 1항에 있어서, 공기를 사용하여 셀룰로오스에테르의 온도 상승을 억제하고, 분쇄기 자체에서 회전판의 속도에 의해 셀룰로오스에테르의 입자크기 별로 분리함을 특징으로 하는 셀룰로오스에테르 제조용 건조분쇄기The method of claim 1, wherein the air is used to suppress the increase in the temperature of the cellulose ether, and the pulverizer itself for drying the cellulose ether, characterized in that separated by the particle size of the cellulose ether by the speed of the rotating plate. 원료공급기 (3)로 주입된 80℃의 원료(2)는 공기 주입기 (8)로 주입된 많은량의 공기에 의해 유동하면서 유도장치 (5)를 따라 분리기 (1)로 이동하고, 회전 회전판(7)에 의해 입자가 작은 (120㎛ 이하) 셀룰로오스에테르는 다음 공정으로 배출하고, 큰 입자의 셀룰로오스에테르는 입자 제거관(4)을 통해 밑으로 제거함을 특징으로 하는 셀룰로오스에테르 제조용 건조분쇄기의 사용방법The raw material 2 at 80 ° C. injected into the raw material feeder 3 is moved to the separator 1 along the induction device 5 while flowing by a large amount of air injected into the air injector 8, and rotating rotary plate ( 7) The method of using a dry pulverizer for manufacturing cellulose ethers, characterized in that the small particles (120㎛ or less) cellulose ether is discharged to the next step, and the large particles of cellulose ether are removed through the particle removal tube (4). 원료공급기(3)으로 주입된 원료(2)는 공기 주입기(8)로 주입된 많은 양의 공기에 의해 유동하면서 유도장치(5)를 따라 분리기(1)로 이동하고, 회전판(7)의 회전에 의해 셀룰로오스에테르를 분쇄시켜 적어도 60% 이상이 100㎛ 이하의 입경을 지닌 셀룰로오스에테르 입자로 제조함을 특징으로 하는 셀룰로오스에테르 제조용건조분쇄기의 사용방법The raw material 2 injected into the raw material feeder 3 moves by the large amount of air injected into the air injector 8 to the separator 1 along the induction device 5 and rotates the rotary plate 7. Method of using a dry mill for cellulose ether production, characterized in that the cellulose ether is pulverized by at least 60% to produce cellulose ether particles having a particle diameter of 100 ㎛ or less 제 3항에 있어서, 원료 셀룰로오스에테르는 알킬셀룰로오스, 히드록시알킬셀룰로오스, 알킬히드록알킬셀룰로오스 및 카르복시알킬셀룰로오스임을 특징으로 하는 셀룰로오스에테르 제조용 건조분쇄기의 사용방법4. The method according to claim 3, wherein the raw cellulose ether is alkyl cellulose, hydroxyalkyl cellulose, alkyl hydroxyalkyl cellulose and carboxyalkyl cellulose.
KR1019950020135A 1995-07-10 1995-07-10 Dry Crusher for Cellulose Ether Production Expired - Lifetime KR100364899B1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100654423B1 (en) 2004-10-19 2006-12-06 삼성정밀화학 주식회사 Method for pulverizing and drying cellulose ether and its derivatives, and pulverizing and drying apparatus used therein
KR100909305B1 (en) * 2001-10-26 2009-08-05 다우 글로벌 테크놀로지스 인크. Process and apparatus for combined milling and drying
KR102054859B1 (en) * 2019-09-17 2019-12-13 주식회사 그래핀 코어 Manufacturing apparatus for wasted polyethylene terephthalate microparticles, manufacturing method of paint composition using thereof, and paint composition manufactured by the method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100909305B1 (en) * 2001-10-26 2009-08-05 다우 글로벌 테크놀로지스 인크. Process and apparatus for combined milling and drying
KR100654423B1 (en) 2004-10-19 2006-12-06 삼성정밀화학 주식회사 Method for pulverizing and drying cellulose ether and its derivatives, and pulverizing and drying apparatus used therein
KR102054859B1 (en) * 2019-09-17 2019-12-13 주식회사 그래핀 코어 Manufacturing apparatus for wasted polyethylene terephthalate microparticles, manufacturing method of paint composition using thereof, and paint composition manufactured by the method

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