KR0174134B1 - Manufacturing Method of Polyamide 6 by Reaction Extrusion Process - Google Patents
Manufacturing Method of Polyamide 6 by Reaction Extrusion Process Download PDFInfo
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- KR0174134B1 KR0174134B1 KR1019960027716A KR19960027716A KR0174134B1 KR 0174134 B1 KR0174134 B1 KR 0174134B1 KR 1019960027716 A KR1019960027716 A KR 1019960027716A KR 19960027716 A KR19960027716 A KR 19960027716A KR 0174134 B1 KR0174134 B1 KR 0174134B1
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- polyamide
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 19
- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000001125 extrusion Methods 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract description 18
- 239000003999 initiator Substances 0.000 claims abstract description 17
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 21
- 238000004898 kneading Methods 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010539 anionic addition polymerization reaction Methods 0.000 abstract description 4
- 230000000704 physical effect Effects 0.000 abstract description 4
- 229910052786 argon Inorganic materials 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 3
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 abstract 2
- DVPHDWQFZRBFND-DMHDVGBCSA-N 1-o-[2-[(3ar,5r,6s,6ar)-2,2-dimethyl-6-prop-2-enoyloxy-3a,5,6,6a-tetrahydrofuro[2,3-d][1,3]dioxol-5-yl]-2-[4-[(2s,3r)-1-butan-2-ylsulfanyl-2-(2-chlorophenyl)-4-oxoazetidin-3-yl]oxy-4-oxobutanoyl]oxyethyl] 4-o-[(2s,3r)-1-butan-2-ylsulfanyl-2-(2-chloropheny Chemical group C1([C@H]2[C@H](C(N2SC(C)CC)=O)OC(=O)CCC(=O)OC(COC(=O)CCC(=O)O[C@@H]2[C@@H](N(C2=O)SC(C)CC)C=2C(=CC=CC=2)Cl)[C@@H]2[C@@H]([C@H]3OC(C)(C)O[C@H]3O2)OC(=O)C=C)=CC=CC=C1Cl DVPHDWQFZRBFND-DMHDVGBCSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000007334 copolymerization reaction Methods 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- QISSLHPKTCLLDL-UHFFFAOYSA-N N-Acetylcaprolactam Chemical compound CC(=O)N1CCCCCC1=O QISSLHPKTCLLDL-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 229920006122 polyamide resin Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- SLXKOJJOQWFEFD-UHFFFAOYSA-N 6-aminohexanoic acid Chemical compound NCCCCCC(O)=O SLXKOJJOQWFEFD-UHFFFAOYSA-N 0.000 description 1
- 229920006051 Capron® Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229960002684 aminocaproic acid Drugs 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010538 cationic polymerization reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- -1 cyclic lactams Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 125000003717 m-cresyl group Chemical group [H]C1=C([H])C(O*)=C([H])C(=C1[H])C([H])([H])[H] 0.000 description 1
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-methyl-PhOH Natural products CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polyamides (AREA)
Abstract
본 발명은 반응압출 공정에 의한 폴리아마이드 6의 음이온 중합반응에 의한 연속중합 및 후공정에 관한 것으로, 그 기술구성은 6개의 탄소원자로 이루어진 중합가능한 락탐 단량체 2∼6몰에 0.05∼0.15몰의 개시제를 넣은 혼합물과 2∼6몰의 단량체에 0.05∼0.15몰의 보조개새제를 넣은 혼합물에 12∼32몰의 단량체를 혼련시킨 후, 이축압출기의 투입구에 질소 또는 아르곤 가스와 함께 투입하되, 이축압출기의 온도영역을 4부분으로 구분하고 중합온도 70∼290℃, 스크류 속도 50∼350rpm으로 하여 연속적으로 공중합하여 연속방사를 할 수 있는 것을 특징으로 하는 반응압출 공정에 의한 폴리아마이드 6의 제조방법으로서, 기계적 물성이 뛰어나고 연속방사가 가능한 폴리아마이드 6을 얻기 위한 신규한 발명이다.The present invention relates to a continuous polymerization and an after-polymerization process of anionic polymerization of polyamide 6 by a reaction extrusion process, and its technical configuration is 0.05 to 0.15 mole of initiator in 2 to 6 moles of polymerizable lactam monomer composed of six carbon atoms. 12 to 32 moles of monomer were kneaded in a mixture containing 2 to 6 moles of monomer and 0.05 to 0.15 moles of co-opening agent, and then introduced together with nitrogen or argon gas into the inlet of the twin screw extruder. A method for producing polyamide 6 by a reaction extrusion process, characterized in that the temperature range is divided into four parts and the polymerization temperature is 70 to 290 ° C. and the screw speed is 50 to 350 rpm to allow continuous copolymerization and continuous spinning. It is a novel invention for obtaining polyamide 6 having excellent physical properties and capable of continuous spinning.
Description
제1도는 본 발명에 사용되는 반응압축 공정도.1 is a reaction compression process chart used in the present invention.
제2도는 본 발명에 사용되는 2축 압출기의 정면도이다.2 is a front view of a twin screw extruder used in the present invention.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : 이축압출기 2 : 온도셋팅판넬1: twin screw extruder 2: temperature setting panel
3 : 단량체투입구 4 : 벤트3: monomer inlet 4: vent
5 : 스크류5: screw
본 발명은 반응압출공정에 의한 폴리아마이드 6의 제조방법에 관한 것으로, 특히 음이온 중합반응에 의한 연속중합 및 연속적인 후공정에 따른 반응 압출공정에 의한 폴리아마이드 6의 제조방법에 관한 것이다.The present invention relates to a method for producing polyamide 6 by a reaction extrusion process, and more particularly to a method for producing polyamide 6 by a reaction extrusion process according to a continuous polymerization and a continuous post process by an anionic polymerization.
종래에 알려진 폴리아마이드의 중합공정으로는 미국특허 제 2,071,253 호에 의해 처음으로 ε-카프로락탐의 중합에 성공을 보아 상품화 되었으나(상표명 ; Perlon), 이 펄론은 카프로락탐과 하이드로 클로라이드를 이용한 양이온 중합 메카니즘에 의해 중합되어지고 반응시간이 길며 중합체의 물성이 좋지 않았다.Conventionally known polyamide polymerization process has been commercialized by the first successful polymerization of ε-caprolactam by US Patent No. 2,071,253 (trade name; Perlon), but this perlon is a cationic polymerization mechanism using caprolactam and hydrochloride. It was polymerized by, the reaction time was long and the physical properties of the polymer were not good.
또한 미국특허 제 2,251,519 호에서는 리튬 금속 촉매와 나트륨 금속 촉매를 이용한 음이온 중합방법이 개시되고 있으나, 축합 반응과 음이온 중합에 의해 합성된 폴리아마이드 6는 ε-아미노카프론산으로 중합된 것과 같은 구조를 보이고 있으나, 반응 시간이 길고, 만족할 만한 물성를 얻을 수 없다.In addition, US Patent No. 2,251,519 discloses an anionic polymerization method using a lithium metal catalyst and a sodium metal catalyst, but polyamide 6 synthesized by condensation reaction and anionic polymerization shows the same structure as polymerized with ε-aminocaproic acid. However, the reaction time is long and satisfactory physical properties cannot be obtained.
또 다른 선행기술인, 미국특허 제 3,166,533 호는 고속반응 공정에 관한 것으로, ε-카프로락탐의 알칼리 중합에서 이미드에 영향을 줄수 있는 많은 종류의 부촉매에 의해 반응 속도를 몇 분 이내로 줄이는 내용을 나타내고 있다. 이로써 반응시간은 짧아졌지만 반응 뱃치별 물성 차이가 심하였다.Another prior art, US Pat. No. 3,166,533, relates to a high-speed reaction process, which shows that the reaction rate is reduced to less than a few minutes by many types of subcatalysts that can affect imides in alkali polymerization of ε-caprolactam. . As a result, the reaction time was shortened, but the physical properties of the reaction batches were severe.
본 발명에서는 1대의 이축압출기를 사용하여 카프로락탐의 중합 및 연속적인 방사를 가능케 하는 공정으로, 기존의 축합 반응에 의해 만들어진 같은 분자량의 폴리아마이드 수지보다 반응시간이 짧고, 기계적 물성이 좋은 폴리 아마이드 수지의 제조방법에 관한 것이다. 즉, 낮은 온도에서 연속적인 음이온 반응에 의한 폴리아마이드 6의 합성 공정으로, 단량체와 개시제, 보조개시제의 혼합물을 이축압출기의 투입구에 넣고 70∼290℃ 사이의 온도 범위에서의 합성 방법으로 짧은 시간에 반응이 완료되도록 하는 폴리아마이드 6의 제조방법에 관한 것이다.In the present invention, one biaxial extruder is used to polymerize and continuously spin caprolactam. The reaction time is shorter than that of the polyamide resin of the same molecular weight produced by the conventional condensation reaction, and the mechanical properties of the polyamide resin are good. It relates to a manufacturing method of. That is, in the process of synthesizing polyamide 6 by continuous anion reaction at low temperature, the mixture of monomer, initiator, and co-initiator is placed in the inlet of the twin screw extruder and in a short time by the synthesis method in the temperature range of 70 to 290 ° C. It relates to a process for preparing polyamide 6 to complete the reaction.
이하, 본 발명을 구체적으로 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명에서 사용되는 단량체는 6개의 탄소원자로 이루어진 환상락탐인 카프로락탐 플레이크를 사용하고, 개시제는 나트륨, 보조개시제는 노르말 아세틸 카프로락탐(N-Acetyl caprolactam)을 사용한다. 또한 물성비교를 위해 사용한 상업용 폴리아마이드는 앨라이드 시그날사(Allied Signal Co.)의 캐프론 8200을 사용하였다.The monomer used in the present invention uses caprolactam flakes, which are cyclic lactams consisting of six carbon atoms, sodium is used as an initiator, and N-Acetyl caprolactam is used as an auxiliary initiator. In addition, the commercial polyamide used for the comparison of properties was used Capron 8200 of Allied Signal Co. (Allied Signal Co.).
본 발명은 2∼6몰의 단량체에 0.05∼0.15몰의 개시제를 넣은 혼합물과 2∼6몰의 단량체에 0.05∼0.15몰의 보조개시제를 넣은 혼합물에 12∼32몰의 단량체를 혼련한 후 이축압출기의 투입구에 질소 또는 아르곤가스와 함께 투입하여 폴리아마이드 6을 제조한다. 만약, 단량체, 개시제 및 보조개시제가 상기 범위 미만일 경우는 폴리아마이드 6의 합성이 이루어지지 않으며 초과시는 폴리아마이드의 점도가 높아 압출가공이 좋지 않다. 이때의 이축압출기는 다음과 같이 4부분으로 구분하고 스크류의 속도는 50∼350ppm으로 한다. 만약 스크류의 속도가 50rpm 미만이면 이축압출기내의 체류시간이 길어 중합체의 열분해가 발생할 수 있고 350rpm을 초과시에는 압출기내의 체류시간이 짧아 원하는 분자량의 중합체를 얻을 수가 없다. 또 압출기 각 부위의 온도 범위는 다음과 같다. 분말 상태의 단량체, 개시제, 보조개시제를 성공적으로 투입하기 위해 투입구의 온도는 70 ∼260℃ 사이로 유지되어야 하는에, 이는 단량체의 녹는 온도와 끓는 온도가 각각 80℃와 265℃이기 때문이다. 또한 폴리아마이드 6의 결정이 녹는 온도가 215℃이므로 압출기 배랄(barrel)의 후반 부위와 다이(die)의 온도는 215℃를 넘어야만 압출이 가능하다. 또한 프로리아마이드 6의 분해 온도가 290℃이므로 후반부의 온도는 290℃를 넘으면 안된다.The present invention is a twin screw extruder after kneading 12 to 32 moles of monomer in a mixture of 0.05 to 0.15 mole of initiator in 2 to 6 moles of monomer and 0.05 to 0.15 mole of co-initiator in 2 to 6 moles of monomer. Injecting with nitrogen or argon gas into the inlet of the polyamide 6 is prepared. If the monomer, the initiator and the co-initiator is less than the above range, the synthesis of polyamide 6 is not performed, and when it exceeds, the viscosity of the polyamide is high and extrusion processing is not good. At this time, the twin screw extruder is divided into four parts as follows and the speed of screw is 50 ~ 350ppm. If the speed of the screw is less than 50 rpm, the residence time in the twin screw extruder may be long, and thermal decomposition of the polymer may occur. If the screw speed exceeds 350 rpm, the residence time in the extruder is short, so that a polymer having a desired molecular weight cannot be obtained. In addition, the temperature range of each part of an extruder is as follows. The temperature of the inlet must be maintained between 70 and 260 ° C. in order to successfully add powder monomers, initiators and co-initiators, since the melting and boiling temperatures of the monomers are 80 ° C. and 265 ° C., respectively. In addition, since the crystallization temperature of the polyamide 6 is 215 ° C, the temperature of the latter part of the extruder barrel and the die may be extruded only when it exceeds 215 ° C. In addition, since the decomposition temperature of proriamide 6 is 290 degreeC, the temperature of the latter part must not exceed 290 degreeC.
이러한 조건에 의해 아래와 같은 온도범위를 설정한다.Under these conditions, set the following temperature ranges.
따라서 위에 예시한 조건에 의거하여 다음과 같은 온도조건을 설정한다.Therefore, the following temperature conditions are set based on the conditions exemplified above.
또한 체류시간을 조절하기 위해 다음의 3가지의 압출기의 스크류 조합을 사용하여 반응물의 평균 체류시간을 짧게는 1분에서 길게는 6분 정도까지 조절한다.In addition, the average residence time of the reactants is controlled from as short as 1 minute to as long as 6 minutes using a combination of the following three extruders to control the residence time.
스크류 조합 1은 포지티브(positive)하게 우선회 스크류만의 조합으로 전단력이 매우 작고 평균 체류 시간이 1분 정도의 조합이며, 스크류 조합 2는 평균 체류 시간을 높이고, 전단력을 높여 주기 위해 두부분에 니딩 디스크 블록(kneading disc block)을 도입하고, 나머지는 라이트 핸디드한 스크류 조합이며, 스크류 조합 3은 세부분의 니딩디스크 블록과 하나의 좌선회의 스크류 및 나머지는 우선회 스크류의 조합으로 전단력 및 체류시간의 극대화를 꾀하도록 하였다.Screw combination 1 is a combination of positively-priority screw only with very small shear force and an average residence time of about 1 minute. Screw combination 2 has a kneading disc in two parts to increase the average residence time and increase the shear force. A kneading disc block is introduced, the remainder is a light handed screw combination, and screw combination 3 is a combination of the kneading disc block with one part and one left-turning screw and the remainder is a combination of the priority screw to It was intended to maximize.
또한 다이 구멍의 크기 및 숫자를 변경해서 압출되어 나오는 중합체를 와인더(winder)를 사용하여 방사한다. 반응전도를 알기 위한 전환율은 중합된 100g의 폴리아마이드 6을 끓은 물에 세정한 후, 물속에 남은 미반응 단량체를 회수하여 무게를 재어 결정하였다. 분자량은 GPC(Gel Permeation Chromatography)로 측정하였는데 이때 온도는 100℃, 용매는 m-크레졸을 사용하고, 표준 시료는 수평균 분자량이 20,000인 폴리아마이드로 하여 비교 수평균 분자량을 측정한다. 기계적 성질은 ASTM에 의거하여 측정한다.The extruded polymer is spun using a winder to change the size and number of die holes. The conversion rate to determine the reaction conductivity was determined by washing 100 g of polyamide 6 polymerized in boiled water and recovering the unreacted monomers remaining in the water. Molecular weight was measured by gel permeation chromatography (GPC), where temperature is 100 ° C., solvent is m-cresol, and standard sample is polyamide having a number average molecular weight of 20,000. Mechanical properties are measured according to ASTM.
본 발명을 실시예에 의거하여 설명하면 아래와 같다. 다만 본 발명은 아래 실시예에 한정된 것만은 아니다.The present invention will be described below based on examples. However, the present invention is not limited to the following examples.
[실시예 1]Example 1
미국 엘라이드 시스날사의 카프로락탐 플레이크 2몰을 단량체로 사용하고 개시제로 0.05몰의 나트륨, 보조개시제로 0.05몰의 노르말 아세틸 카프로락탐을 혼합한 혼합액에 12몰의 카프로락탐 플레이크의 단량체를 혼합한 혼합반응물을 이축 압출기(돌일 베르너 엔드 플라이더러(Werner ＆ Pfleiderer)사 제품으로 길이의 비가 42이고 6개의 가열구역을 가진 Z나-25 모델)의 투입구에 아르곤 가스와 함께 투입하였다. 이때 이축압출기 스크류 속도는 50rpm, 반응시간 6분간으로 하여 반응시킨 후 압출되어 나오는 중합체를 펠렛타이져(Pelletiger)로 펠렛(Pellet)으로 만들어서 기계적 물성을 측정한 결과를 표에 나타내었다.A mixture of 12 moles of caprolactam flake monomer is mixed with a mixture of 2 moles of caprolactam flakes manufactured by Elysine Cisnal USA as a monomer, 0.05 moles of sodium as an initiator, and 0.05 moles of normal acetyl caprolactam as an auxiliary initiator. The reaction was fed with argon gas into the inlet of a twin screw extruder (Z or-25 model with six heating zones, 42 in length, manufactured by Werner & Pfleiderer). At this time, the screw speed of the twin screw extruder was 50 rpm, and the reaction time was 6 minutes. After the reaction, the extruded polymer was pelletized with pelletizer (Pelletiger) to measure the mechanical properties.
[실시예 2∼5][Examples 2 to 5]
[비교예 1∼4][Comparative Examples 1 to 4]
단량체, 개시제, 보조개시제, 스크류 속도를 표와 같이 변경한 것 이외에는 실시예1에서 행한 것과 동일하게 실시하였다.It carried out similarly to having performed in Example 1 except having changed the monomer, the initiator, the co-initiator, and the screw speed as Table.
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| RU2471816C1 (en) * | 2012-01-10 | 2013-01-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Ивановский государственный химико-технологический университет" | Method of producing polyamide-6 |
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