KR20220018433A - Flame retardant plastic based on adenosine triphosphate and polylactic acid - Google Patents
Flame retardant plastic based on adenosine triphosphate and polylactic acid Download PDFInfo
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- KR20220018433A KR20220018433A KR1020210101871A KR20210101871A KR20220018433A KR 20220018433 A KR20220018433 A KR 20220018433A KR 1020210101871 A KR1020210101871 A KR 1020210101871A KR 20210101871 A KR20210101871 A KR 20210101871A KR 20220018433 A KR20220018433 A KR 20220018433A
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- adenosine triphosphate
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- ZKHQWZAMYRWXGA-KQYNXXCUSA-J ATP(4-) Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O)[C@@H](O)[C@H]1O ZKHQWZAMYRWXGA-KQYNXXCUSA-J 0.000 title claims abstract description 89
- ZKHQWZAMYRWXGA-UHFFFAOYSA-N Adenosine triphosphate Natural products C1=NC=2C(N)=NC=NC=2N1C1OC(COP(O)(=O)OP(O)(=O)OP(O)(O)=O)C(O)C1O ZKHQWZAMYRWXGA-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 64
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 63
- 239000003063 flame retardant Substances 0.000 title claims abstract description 61
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229920003023 plastic Polymers 0.000 title claims abstract description 19
- 239000004033 plastic Substances 0.000 title claims abstract description 19
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 43
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 43
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 43
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 27
- 229910052698 phosphorus Inorganic materials 0.000 claims description 27
- 239000011574 phosphorus Substances 0.000 claims description 27
- MWFNQNPDUTULBC-UHFFFAOYSA-N phosphono dihydrogen phosphate;piperazine Chemical compound C1CNCCN1.OP(O)(=O)OP(O)(O)=O MWFNQNPDUTULBC-UHFFFAOYSA-N 0.000 claims description 26
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 21
- 235000011180 diphosphates Nutrition 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 10
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- 230000000694 effects Effects 0.000 abstract description 7
- 150000002894 organic compounds Chemical class 0.000 abstract description 4
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- 229920003002 synthetic resin Polymers 0.000 description 11
- 229930024421 Adenine Natural products 0.000 description 8
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- HMFHBZSHGGEWLO-SOOFDHNKSA-N D-ribofuranose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H]1O HMFHBZSHGGEWLO-SOOFDHNKSA-N 0.000 description 8
- PYMYPHUHKUWMLA-LMVFSUKVSA-N Ribose Natural products OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 description 8
- 229960000643 adenine Drugs 0.000 description 8
- HMFHBZSHGGEWLO-UHFFFAOYSA-N alpha-D-Furanose-Ribose Natural products OCC1OC(O)C(O)C1O HMFHBZSHGGEWLO-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910052736 halogen Inorganic materials 0.000 description 5
- 150000002367 halogens Chemical class 0.000 description 5
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 4
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- 125000002264 triphosphate group Chemical group [H]OP(=O)(O[H])OP(=O)(O[H])OP(=O)(O[H])O* 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- LHCPRYRLDOSKHK-UHFFFAOYSA-N 7-deaza-8-aza-adenine Chemical compound NC1=NC=NC2=C1C=NN2 LHCPRYRLDOSKHK-UHFFFAOYSA-N 0.000 description 1
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/529—Esters containing heterocyclic rings not representing cyclic esters of phosphoric or phosphorous acids
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/126—Polymer particles coated by polymer, e.g. core shell structures
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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Abstract
Description
본 발명은 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱에 관한 것이다. 본 발명에 따르면, 생명 활동을 위해 에너지를 공급하는 유기 화합물인 아데노신 삼인산(adenosine triphosphate; ATP)을 생분해성 고분자화합물 중 가장 많이 생산되고 있는 수지인 폴리젖산(polylactic acid)에 적용시켜 새로운 난연성 플라스틱을 제공할 수 있다.The present invention relates to flame-retardant plastics based on adenosine triphosphate and polylactic acid. According to the present invention, a new flame retardant plastic is produced by applying adenosine triphosphate (ATP), an organic compound that supplies energy for life activities, to polylactic acid, which is the most produced resin among biodegradable high molecular compounds. can provide
본 발명에서는 모델 고분자 수지로 높은 수요로 인해 생산량이 가장 많은 폴리젖산 수지를 선정하였다. 폴리젖산 수지는 옥수수와 사탕수수 등의 식물로 만드는 생분해성 수지로써, 가수분해의 산물로 젖산을 방출하기 때문에 무독한 특성을 가짐. 강성 및 인장강도가 높고 인체에 무해하고 바이오매스로부터 얻을 수 있으며 가공성이 우수하다는 장점 등으로 인하여 약물전달, 인공피부, 인공삽입장치등의 의료분야 혹은 젖병, 티백 등의 식품용으로도 주로 사용된다. In the present invention, as a model polymer resin, polylactic acid resin with the highest production volume was selected due to high demand. Polylactic acid resin is a biodegradable resin made from plants such as corn and sugar cane, and has non-toxic properties because it releases lactic acid as a product of hydrolysis. Due to the advantages of high rigidity and tensile strength, harmless to the human body, obtained from biomass, and excellent processability, it is mainly used for drug delivery, artificial skin, medical fields such as artificial insertion devices, or food such as baby bottles and tea bags. .
그러나 취약한 기계적 특성 및 난연 특성으로 인해 매우 우수한 난연성이 요구되는 산업계 분야에서는 그 사용이 극히 제한되고 있다. 따라서, 이러한 젖산 소재의 난연성을 높이기 위해 할로겐 기반의 난연제를 사용할 수 있으나, 이는 폴리젖산의 친환경성 및 생체적합성을 없애기 때문에 산업적으로의 가치가 떨어진다. 이에 최근 생체 내에서 추출할 수 있는 식물 단백질, DNA 등 바이오 분자가 친환경 난연제로서의 대안으로서 개발 및 발굴되고 있으며, 본 발명은 바이오 분자인 아데노신 삼인산을 친환경 난연제로 사용하여, 친환경성 고분자인 폴리젖산 수지에 적용, 난연성을 지닌 친환경성 고분자 수지를 합성하고자 한다.However, its use is extremely limited in the industrial field requiring very good flame retardancy due to weak mechanical properties and flame retardant properties. Therefore, it is possible to use a halogen-based flame retardant to increase the flame retardancy of the lactic acid material, but since it eliminates the eco-friendliness and biocompatibility of polylactic acid, its industrial value is reduced. Accordingly, recently, biomolecules such as plant proteins and DNA that can be extracted in vivo are being developed and discovered as alternatives as eco-friendly flame retardants. To synthesize an eco-friendly polymer resin with flame retardancy.
본 발명은 아데노신 삼인산에 존재하는 3개의 인산기 (phosphate group), 리보스 (ribose sugar) 그리고 아데닌 (adenine) 염기 각각의 멀티 시너지 효과를 통해 폴리젖산 고분자 수지에 난연성을 부여하여, 친환경성 고분자 수지를 만드는 것을 목적으로 한다.The present invention provides flame retardancy to polylactic acid polymer resin through the multi synergistic effect of each of the three phosphate groups, ribose sugar, and adenine bases present in adenosine triphosphate, thereby making an eco-friendly polymer resin aim to
본 발명의 일 실시예에 따른 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱은, 폴리젖산; 인계 난연제; 및 아데노신 삼인산(ATP)을 포함한다.A flame retardant plastic based on adenosine triphosphate and polylactic acid according to an embodiment of the present invention, polylactic acid; phosphorus-based flame retardants; and adenosine triphosphate (ATP).
상기 인계 난연제는 폴리인산암모늄(Ammonium polyphosphate; APP) 또는 피로인산피페라진(Piperazine pyrophosphate; PPP) 중 어느 하나이다.The phosphorus-based flame retardant is either ammonium polyphosphate (APP) or piperazine pyrophosphate (PPP).
상기 인계 난연제가 폴리인산암모늄(APP)인 경우, 89.4 내지 91wt%의 폴리젖산; 7.5 내지 10wt%의 폴리인산암모늄; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함한다.When the phosphorus-based flame retardant is ammonium polyphosphate (APP), 89.4 to 91 wt% of polylactic acid; 7.5 to 10 wt% of ammonium polyphosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
상기 인계 난연제가 피로인산피페라진(PPP)인 경우, 97.4 내지 98.4wt%의 폴리젖산; 0.5 내지 2wt%의 피로인산피페라진; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함한다.When the phosphorus-based flame retardant is piperazine pyrophosphate (PPP), 97.4 to 98.4 wt% of polylactic acid; 0.5 to 2 wt% of piperazine pyrophosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
본 발명의 일 실시예에 따른 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱의 제조 방법은, 분말 형태의 폴리젖산; 폴리인산암모늄(APP) 또는 피로인산피페라진(PPP) 중 어느 하나; 및 아데노신 삼인산을 혼합하여 압출 공정을 통해 샘플을 준비하는 단계; 및 상기 샘플을 금형에 넣고 170℃ 온도 및 150MPa 압력에서 10분간 압축시키는 단계를 포함한다.A method for producing a flame-retardant plastic based on adenosine triphosphate and polylactic acid according to an embodiment of the present invention comprises: polylactic acid in powder form; Any one of ammonium polyphosphate (APP) or piperazine pyrophosphate (PPP); and preparing a sample through an extrusion process by mixing adenosine triphosphate; and putting the sample in a mold and compressing it for 10 minutes at a temperature of 170° C. and a pressure of 150 MPa.
인계 난연제가 폴리인산암모늄(APP)인 경우, 89.4 내지 91wt%의 폴리젖산; 7.5 내지 10wt%의 폴리인산암모늄; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함한다.When the phosphorus-based flame retardant is ammonium polyphosphate (APP), 89.4 to 91 wt% of polylactic acid; 7.5 to 10 wt% of ammonium polyphosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
인계 난연제가 피로인산피페라진(PPP)인 경우, 97.4 내지 98.4wt%의 폴리젖산; 0.5 내지 2wt%의 피로인산피페라진; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함한다.When the phosphorus-based flame retardant is piperazine pyrophosphate (PPP), 97.4 to 98.4 wt% of polylactic acid; 0.5 to 2 wt% of piperazine pyrophosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
본 발명에서 사용한 고분자 수지인 폴리젖산은 옥수수, 사탕수수, 고구마류 식물의 전분 발효로 생성되는 L-젖산을 중합체로 합성한 폴리머로 친환경적이며 투명성이 높으나 내열성이 낮은 단점을 가는다. 이를 보완하기 위해 본 발명에서 적용한 아데노신 삼인산은 3개의 인산기와 질소 (nitrogen)이 포함된 아데닌이 양 끝단에 존재하고, 챠르역할을 할 수 있는 리보스가 중간에 위치한 구조를 지니고 있기에 소재 자체만으로 우수한 난연 시너지 효과를 유발할 수 있다. 또한, 상대적으로 낮은 온도 (160-200도)에서 phophoric acid를 방출하여 고분자 차폐막인, 챠르를 짧은 시간 내에서 형성할 수 있으며, 형성되는 챠르의 두께도 일반적으로 사용되는 인계 난연제보다 수십 배 이상 두꺼워 적은 양으로도 고분자 수지에 우수한 난연성을 부여할 수 있다. 그리고, 세포에서 다양한 생명 활동을 수행하기 위해 매일 생성되는 유기 화합물이기에 친환경적이며, 따라서 생물 유래 원료에서 추출한 재료로 합성된 폴리젖산과의 친환경적 목적에의 사용에 부합한다.Polylactic acid, a polymer resin used in the present invention, is a polymer synthesized from L-lactic acid produced by starch fermentation of corn, sugar cane, and sweet potato plants. It is eco-friendly and has high transparency but low heat resistance. To compensate for this, the adenosine triphosphate applied in the present invention has a structure in which three phosphate groups and adenine containing nitrogen exist at both ends, and ribose, which can act as a char, is located in the middle. may cause synergistic effects. In addition, by releasing phophoric acid at a relatively low temperature (160-200 degrees), a polymer shielding film, char, can be formed within a short time, and the thickness of the formed char is also several tens of times thicker than commonly used phosphorus-based flame retardants. Even with a small amount, excellent flame retardancy can be imparted to the polymer resin. And, since it is an organic compound produced every day to perform various life activities in cells, it is eco-friendly, and therefore it is suitable for use for eco-friendly purposes with polylactic acid synthesized from a material extracted from a biological material.
도 1은 본 발명의 일 실시예에 따른 비할로겐계 인계 난연제가 코팅된 고분자 수지 및 이의 난연 특성을 나타낸 것이다.
다양한 실시예들이 이제 도면을 참조하여 설명되며, 전체 도면에서 걸쳐 유사한 도면번호는 유사한 엘리먼트를 나타내기 위해서 사용된다. 설명을 위해 본 명세서에서, 다양한 설명들이 본 발명의 이해를 제공하기 위해서 제시된다. 그러나 이러한 실시예들은 이러한 특정 설명 없이도 실행될 수 있음이 명백하다. 다른 예들에서, 공지된 구조 및 장치들은 실시예들의 설명을 용이하게 하기 위해서 블록 다이아그램 형태로 제시된다. 1 shows a polymer resin coated with a non-halogen-based phosphorus-based flame retardant according to an embodiment of the present invention and its flame retardant properties.
Various embodiments are now described with reference to the drawings, wherein like reference numerals are used to refer to like elements throughout. In this specification for purposes of explanation, various descriptions are presented to provide an understanding of the present invention. However, it will be apparent that these embodiments may be practiced without these specific descriptions. In other instances, well-known structures and devices are presented in block diagram form in order to facilitate describing the embodiments.
이하, 첨부한 도면을 참조하여 본 발명의 실시예에 대해 상세히 설명한다. 본 발명은 다양한 변경을 가할 수 있고 여러 가지 형태를 가질 수 있는 바, 특정 실시예들을 도면에 예시하고 본문에 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 개시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술 범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. 각 도면을 설명하면서 유사한 참조부호를 유사한 구성요소에 대해 사용하였다. Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. Since the present invention can have various changes and can have various forms, specific embodiments are illustrated in the drawings and described in detail in the text. However, this is not intended to limit the present invention to the specific disclosed form, it should be understood to include all modifications, equivalents and substitutes included in the spirit and scope of the present invention. In describing each figure, like reference numerals have been used for like elements.
본 출원에서 사용한 용어는 단지 특정한 실시 예를 설명하기 위해 사용된 것으로서 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다. 본 출원에서, "포함하다" 또는 "가지다" 등의 용어는 명세서 상에 기재된 특징, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.The terms used in the present application are only used to describe specific embodiments and are not intended to limit the present invention. The singular expression includes the plural expression unless the context clearly dictates otherwise. In the present application, terms such as “comprise” or “have” are intended to designate that a feature, step, operation, component, part, or combination thereof described in the specification is present, and includes one or more other features or steps. , it should be understood that it does not preclude the possibility of the existence or addition of an operation, a component, a part, or a combination thereof.
도 1은 본 발명의 일 실시예에 따른 비할로겐계 인계 난연제가 코팅된 고분자 수지 및 이의 난연 특성을 나타낸 것이다.1 shows a polymer resin coated with a non-halogenated phosphorus-based flame retardant and its flame retardant properties according to an embodiment of the present invention.
도 1을 참조하면, 본 발명의 일 실시예에 따른 비할로겐계 인계 난연제는 아데노신 삼인산(ATP)을 포함한다.Referring to FIG. 1 , the non-halogen-based phosphorus-based flame retardant according to an embodiment of the present invention includes adenosine triphosphate (ATP).
아데노신 삼인산(ATP)은 흥분, 근육 수축 및 화학 합성의 신경 전도를 포함하여 살아있는 유기체의 다양한 생화학적 과정에 에너지를 제공하는 중요한 생체 분자이다.Adenosine triphosphate (ATP) is an important biomolecule that provides energy for a variety of biochemical processes in living organisms, including nerve conduction of excitation, muscle contraction, and chemical synthesis.
아데노신 삼인산(ATP)는 도 1에 도시된 바와 같이, 삼인산기(three phosphate groups), 리보오스(Ribose) 및 아데닌(Adenine) 염기로 구성되어 있으며, 분자 자체에 난연 소재에서 필수적인 3대 구성 요소인 인(P), 질소(N) 및 탄소(C)를 포함하고 있어서 우수한 난연성을 나타낼 수 있다.As shown in Figure 1, adenosine triphosphate (ATP) is composed of three phosphate groups, ribose and adenine bases, and the molecule itself contains phosphorus, which is one of the three essential components in flame-retardant materials. (P), nitrogen (N) and carbon (C) can be included to exhibit excellent flame retardancy.
일 실시예에서, 상기 비할로겐계 인계 난연제는 연소 시에 유리 파편 형태의 차르(char)를 형성하여 여러 고분자 수지의 난연성을 향상시킬 수 있다.In one embodiment, the non-halogen-based phosphorus flame retardant may improve the flame retardancy of various polymer resins by forming char in the form of glass fragments during combustion.
또한, 본 발명의 비할로겐계 인계 난연제는 연소 시에 초기 부피 대비 최소 10 배 이상, 바람직하게는 70 내지 80배의 부피 팽창이 일어나기에, 적은 양으로도 여러 고분자 수지에 우수한 난연성을 부여할 수 있다.In addition, since the non-halogen phosphorus flame retardant of the present invention expands at least 10 times or more, preferably 70 to 80 times, compared to the initial volume during combustion, excellent flame retardancy can be imparted to various polymer resins even with a small amount. have.
이는 아데노신 삼인산(ATP)에 함유된 삼인산기, 아데닌 염기 및 리보오스가 멀티 시너지 효과를 발휘하기 때문이다.This is because the triphosphate group, adenine base, and ribose contained in adenosine triphosphate (ATP) exert a multi-synergistic effect.
구체적으로, 삼인산기는 산 공급원(acid source)으로 작용하며, 상대적으로 낮은 온도(약 160 내지 200℃)에서 방출되어 유리 파편 형태의 차르(char) 형성을 촉진할 수 있다.Specifically, the triphosphate group acts as an acid source, and may be released at a relatively low temperature (about 160 to 200° C.) to promote the formation of char in the form of glass fragments.
리보오스는 차르 공급원(char source)으로 작용하며, 연소 시에 유리 파편 형태의 차르(char)를 형성할 수 있다.Ribose acts as a char source and can form char in the form of glass fragments upon combustion.
아데닌은 질소를 함유하는 염기로, 발포제(blowing agent)로 작용하여 연소 시에 암모니아 등의 불연성 가스를 방출하게 된다.Adenine is a nitrogen-containing base, which acts as a blowing agent and releases non-combustible gases such as ammonia during combustion.
따라서, 본 발명의 아데노신 삼인산(ATP) 함유 난연제는 다른 첨가제의 존재 없이도, 삼인산기, 리보오스 및 아데닌 염기 각각의 멀티 시너지 효과를 통해 우수한 난연 특성을 나타낼 수 있으며, 여러 고분자 수지에 적용하여 고분자 수지의 난연성을 향상시킬 수 있다.Therefore, the adenosine triphosphate (ATP)-containing flame retardant of the present invention can exhibit excellent flame retardant properties through the multi-synergistic effect of each triphosphate group, ribose and adenine base without the presence of other additives, It is possible to improve the flame retardancy.
뿐만 아니라, 본 발명의 난연제에 함유된 아데노신 삼인산(ATP)은 세포에서 다양한 생명 활동을 수행하기 위해 매일 생성되는 유기 화합물이기에 무독성으로서 식품용기, 의료용기 등에 친환경 난연제로 적용 가능한 장점이 있다.In addition, adenosine triphosphate (ATP) contained in the flame retardant of the present invention is an organic compound that is generated every day to perform various life activities in cells, so it is non-toxic and can be applied as an eco-friendly flame retardant for food containers, medical containers, etc. There is an advantage.
본 발명에서 사용한 고분자 수지인 폴리젖산은 옥수수, 사탕수수, 고구마류 식물의 전분 발효로 생성되는 L-젖산을 중합체로 합성한 폴리머로 친환경적이며 투명성이 높으나 내열성이 낮은 단점을 가는다. 이를 보완하기 위해 본 발명에서 적용한 아데노신 삼인산은 3개의 인산기와 질소 (nitrogen)이 포함된 아데닌이 양 끝단에 존재하고, 챠르역할을 할 수 있는 리보스가 중간에 위치한 구조를 지니고 있기에 소재 자체만으로 우수한 난연 시너지 효과를 유발할 수 있다. 또한, 상대적으로 낮은 온도 (160-200도)에서 phophoric acid를 방출하여 고분자 차폐막인, 챠르를 짧은 시간 내에서 형성할 수 있으며, 형성되는 챠르의 두께도 일반적으로 사용되는 인계 난연제보다 수십 배 이상 두꺼워 적은 양으로도 고분자 수지에 우수한 난연성을 부여할 수 있다.Polylactic acid, a polymer resin used in the present invention, is a polymer synthesized from L-lactic acid produced by starch fermentation of corn, sugar cane, and sweet potato plants. It is eco-friendly and has high transparency but low heat resistance. To compensate for this, the adenosine triphosphate applied in the present invention has a structure in which three phosphate groups and adenine containing nitrogen exist at both ends, and ribose, which can act as a char, is located in the middle. may cause synergistic effects. In addition, by releasing phophoric acid at a relatively low temperature (160-200 degrees), a polymer shielding film, char, can be formed within a short time, and the thickness of the formed char is also several tens of times thicker than commonly used phosphorus-based flame retardants. Even with a small amount, excellent flame retardancy can be imparted to the polymer resin.
본 발명에서는 폴리젖산에 기존의 상용화 난연제인 폴리인산암모늄 (ammonium polyphosphate) 혹은 피로인산피페라진 (piperazine pyrophosphate)을 소량 첨가함과 동시에 상기 바이오 분자인 아데노신 삼인산을 도입하여 기존의 상용화된 난연 PLA에 비해 월등히 적은 양의 난연제만으로도 V-0 등급을 가지는 난연성 폴리젖산을 합성하였다.In the present invention, a small amount of ammonium polyphosphate or piperazine pyrophosphate, which is a conventional commercially available flame retardant, is added to polylactic acid, and at the same time, adenosine triphosphate, which is the biomolecule, is introduced. Flame-retardant polylactic acid having a grade of V-0 was synthesized with only a very small amount of flame retardant.
본 발명의 일 실시예에 따른 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱은, 폴리젖산; 인계 난연제; 및 아데노신 삼인산(ATP)을 포함한다.A flame retardant plastic based on adenosine triphosphate and polylactic acid according to an embodiment of the present invention, polylactic acid; phosphorus-based flame retardants; and adenosine triphosphate (ATP).
폴리젖산은 옥수수, 사탕수수 등의 생물 유래 원료에서 제조되는 폴리머로서 투명성이 높고 강성 및 인장 강도가 높은 특성으로 인해 차세대 고분자 재료로 평가되고 있다. 그러나 내열성이 낮아 성형 시의 결정화 속도가 낮기 때문에 내열성 향상을 위한 별도의 첨가제를 필요로 한다. 본 발명에서는 내열성 및 난연성을 부여하기 위하여 아데노신 삼인산 (adenosine triphosphate)를 첨가하고자 하며, 아데노신 삼인산을 구성하고 있는 작용기들은 3개의 phosphate group (acid source 역할), ribose sugar (char source 역할) 그리고 adenine (blowing agents 역할)으로 구성되어 있으며, 분자 자체에 난연소재에서 필수적인 3대 구성 요소인 (P), 질소 (N), 탄소 (C)를 포함하고 있어서 이상적인 난연제라고 할 수 있다. Polylactic acid is a polymer produced from biological raw materials such as corn and sugar cane, and is being evaluated as a next-generation polymer material due to its high transparency and high rigidity and tensile strength. However, since the heat resistance is low and the crystallization rate during molding is low, a separate additive for improving the heat resistance is required. In the present invention, adenosine triphosphate is added to impart heat resistance and flame retardancy, and the functional groups constituting adenosine triphosphate are three phosphate groups (acid source role), ribose sugar (char source role), and adenine (blowing). agents), and the molecule itself contains (P), nitrogen (N), and carbon (C), the three essential components of flame retardant materials, making it an ideal flame retardant.
인계 난연제는 폴리인산암모늄(Ammonium polyphosphate; APP) 또는 피로인산피페라진(Piperazine pyrophosphate; PPP) 중 어느 하나가 이용될 수 있다.As the phosphorus-based flame retardant, any one of ammonium polyphosphate (APP) or piperazine pyrophosphate (PPP) may be used.
인계 난연제가 폴리인산암모늄(APP)인 경우, 본 발명의 실시예에 따른 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱은 89.4 내지 91wt%의 폴리젖산; 7.5 내지 10wt%의 폴리인산암모늄; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는 것이 바람직하다.When the phosphorus-based flame retardant is ammonium polyphosphate (APP), the flame-retardant plastic based on adenosine triphosphate and polylactic acid according to an embodiment of the present invention contains 89.4 to 91 wt% of polylactic acid; 7.5 to 10 wt% of ammonium polyphosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
인계 난연제가 피로인산피페라진(PPP)인 경우, 본 발명의 실시예에 따른 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱은 97.4 내지 98.4wt%의 폴리젖산; 0.5 내지 2wt%의 피로인산피페라진; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는 것이 바람직하다.When the phosphorus-based flame retardant is piperazine pyrophosphate (PPP), the flame-retardant plastic based on adenosine triphosphate and polylactic acid according to an embodiment of the present invention contains 97.4 to 98.4 wt% of polylactic acid; 0.5 to 2 wt% of piperazine pyrophosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
인계 난연제의 종류에 따른 폴리젖산, 인계 난연제 및 아데노신 삼인산의 적정 함량은 아래 표 1 내지 표 3에서 확인할 수 있다.The appropriate content of polylactic acid, phosphorus-based flame retardant, and adenosine triphosphate according to the type of phosphorus-based flame retardant can be confirmed in Tables 1 to 3 below.
표 1의 경우 생분해성 플라스틱 소재로 많이 사용되어왔던 PLA의 난연평가를 진행한 결과로서, 난연성 평가를 위해 수직 배치 시험을 진행하여 UL-94 시험법에 따라 등급을 분류하였다. 가연성이 있어 PLA 단독으로는 등급을 매길 수 없는 것에 반해서 난연제가 첨가된 폴리프로필렌의 경우 그 함량에 따라 등급이 달라짐을 확인하였다. Piperazine pyrophosphate (PPP), ammonium polyphosphate (APP), adenosine triphosphate (ATP)의 적정 비율에 따라 가장 높은 등급의 V-0를 얻을 수 있었으며, ATP 함량이 평가 등급의 결과에 큰 영향을 줌을 확인하였다.In the case of Table 1, as a result of the flame retardancy evaluation of PLA, which has been widely used as a biodegradable plastic material, a vertical placement test was performed for flame retardancy evaluation and grades were classified according to the UL-94 test method. While PLA alone cannot be graded due to its flammability, it was confirmed that polypropylene with flame retardant added was graded according to its content. The highest grade of V-0 could be obtained according to the appropriate ratio of piperazine pyrophosphate (PPP), ammonium polyphosphate (APP), and adenosine triphosphate (ATP), and it was confirmed that the ATP content had a significant effect on the results of the evaluation grade.
ratingNo
rating
표 2는 APP와 ATP를 이용한 경우의 결과를 다시 나타낸 것으로써, APP를 7.5%로 고정했을 때, ATP를 1.5% 이상 첨가했을 때 V-0등급의 PLA를 얻을 수 있었다. 그 이하 비율의 ATP 함량을 첨가했을 때는 V-0등급의 난연성을 얻을 수 없었다. APP를 10%로 고정했을 때에도, ATP를 0.6% 이상 첨가해야만 V-0등급의 PLA를 얻을 수 있었다. 최소한의 ATP 양으로 V-0 등급을 도출하는 것이 목적이므로, PLA의 일부 비율을 ATP로 대체하는 것으로 V-0등급을 기록할 수 있었다.Table 2 again shows the results when using APP and ATP, and when APP was fixed at 7.5%, when more than 1.5% of ATP was added, PLA of V-0 grade was obtained. When the ATP content was added in a ratio lower than that, it was not possible to obtain flame retardancy of V-0 grade. Even when APP was fixed at 10%, it was possible to obtain V-0 grade PLA only by adding more than 0.6% of ATP. Since the goal is to derive a V-0 grade with the minimum amount of ATP, it was possible to record a V-0 grade by replacing some proportion of PLA with ATP.
표 3은 PPP와 ATP를 이용한 경우의 결과를 다시 나타낸 것으로써, PPP를 2%로 고정했을 때, ATP를 0.6% 이상 첨가했을 때 V-0등급의 PLA를 얻을 수 있었다. 그 이하 비율의 ATP 함량을 첨가했을 때는 V-0등급의 난연성을 얻을 수 없었다. PPP를 1%로 고정했을 때에도, ATP를 0.6% 이상 첨가해야만 V-0등급의 PLA를 얻을 수 있었다. 이를 통해 부풀어오르는 char가 충분히 형성되기 위해서는 최소 0.6% 이상의 ATP가 첨가되어야 한다는 것을 도출하였으며, 이를 통해 PPP의 비율을 최대한으로 줄이고자 하였다. 그러나 PPP의 비율이 0.5%일때는 ATP가 최소 1.5% 이상 첨가되어야 V-0등급을 얻을 수 있었으며, 따라서 PPP가 1, ATP가 0.6일때가 최대한의 PLA 비율을 가지면서 V-0등급을 가지는 조건임을 확인하였다.Table 3 shows the results when using PPP and ATP again, and when PPP was fixed at 2%, and when ATP was added to 0.6% or more, PLA of V-0 grade was obtained. When the ATP content was added in a ratio lower than that, it was not possible to obtain flame retardancy of V-0 grade. Even when PPP was fixed at 1%, it was possible to obtain V-0 grade PLA only by adding more than 0.6% of ATP. Through this, it was deduced that at least 0.6% of ATP should be added in order to sufficiently form swollen char, and through this, the ratio of PPP was reduced to the maximum. However, when the ratio of PPP is 0.5%, at least 1.5% of ATP can be added to obtain V-0 grade. Therefore, when PPP is 1 and ATP is 0.6, the condition to have V-0 grade while having the maximum PLA ratio It was confirmed that
본 발명의 일 실시예에 따른 아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱의 제조 방법은, 분말 형태의 폴리젖산; 폴리인산암모늄(APP) 또는 피로인산피페라진(PPP) 중 어느 하나; 및 아데노신 삼인산을 혼합하여 압출 공정을 통해 샘플을 준비하는 단계; 및 상기 샘플을 금형에 넣고 170℃ 온도 및 150MPa 압력에서 10분간 압축시키는 단계를 포함한다.A method for producing a flame-retardant plastic based on adenosine triphosphate and polylactic acid according to an embodiment of the present invention comprises: polylactic acid in powder form; Any one of ammonium polyphosphate (APP) or piperazine pyrophosphate (PPP); and preparing a sample through an extrusion process by mixing adenosine triphosphate; and putting the sample in a mold and compressing it for 10 minutes at a temperature of 170° C. and a pressure of 150 MPa.
인계 난연제가 폴리인산암모늄(APP)인 경우, 89.4 내지 91wt%의 폴리젖산; 7.5 내지 10wt%의 폴리인산암모늄; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는 것이 바람직하다.When the phosphorus-based flame retardant is ammonium polyphosphate (APP), 89.4 to 91 wt% of polylactic acid; 7.5 to 10 wt% of ammonium polyphosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
인계 난연제가 피로인산피페라진(PPP)인 경우, 97.4 내지 98.4wt%의 폴리젖산; 0.5 내지 2wt%의 피로인산피페라진; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는 것이 바람직하다.When the phosphorus-based flame retardant is piperazine pyrophosphate (PPP), 97.4 to 98.4 wt% of polylactic acid; 0.5 to 2 wt% of piperazine pyrophosphate; and 0.6 to 1.5 wt% of adenosine triphosphate.
이하에서는 구체적인 실시예와 함께 본 발명의 내용을 추가적으로 설명하도록 하겠다.Hereinafter, the content of the present invention will be further described along with specific examples.
분말 형태의 폴리젖산에 다양한 중량%의 폴리인산암모늄 혹은 피로인산피페라진을 소량 첨가함과 동시에 다양한 중량%의 아데노신 삼인산을 첨가하여 섞어 압출 공정을 통해 펠렛 샘플을 준비하였다. (압출조건: 150-170도 / 100 rpm).A small amount of ammonium polyphosphate or piperazine pyrophosphate of various weight % was added to polylactic acid in powder form, and at the same time various weight % of adenosine triphosphate was added and mixed to prepare a pellet sample through an extrusion process. (Extrusion conditions: 150-170 degrees / 100 rpm).
2T 두께의 스테인레스강 소재의 UL-94 시편 금형에 준비된 샘플을 넣음. 폴리젖산은 일반적으로 섭씨 170도~200도의 범위에서 녹는점을 가지기 때문에 첨가된 다른 재료들을 고려, 섭씨 170도에서 핫 프레스 장비를 이용하여 150 MPa 압력에서 10분간 압축시켜 시편을 제작하였다.Put the prepared sample into a UL-94 specimen mold made of stainless steel with a thickness of 2T. Polylactic acid generally has a melting point in the range of 170°C to 200°C, so taking into account other added materials, a specimen was prepared by compressing it for 10 minutes at 150 MPa pressure using a hot press equipment at 170°C.
완성된 폴리젖산 시편의 난연 테스트를 진행하였으며, 객관적인 데이터의 확보를 위해서 UL-94 규격에 따른 Vertical burning 시험을 진행하였다.A flame-retardant test was performed on the finished polylactic acid specimen, and a vertical burning test according to the UL-94 standard was performed to secure objective data.
아데노신 삼인산이 적용된 폴리젖산의 난연성 증대 확인Confirmation of increased flame retardancy of polylactic acid applied with adenosine triphosphate
비교군으로써 ATP를 첨가하지 않은 폴리젖산 시편을 100중량% 설정하였으며 피로인산피페라진을 첨가한 시편의 경우, 피로인산피페라진을 각각 0.5중량%, 1중량%, 2중량%로 설정하였다(표 1 참조). 해당 비교군 시편들의 경우 V-2 혹은 V-1의 난연성을 가졌다. 0.5중량%의 피로인산피페라진이 첨가된 시편의 경우 아데노신 삼인산이 1.5~2.0중량%의 범위에서 첨가될 경우 V-0등급의 난연성이 확보되었다. 1중량%의 피로인산피페라진이 첨가된 시편의 경우 아데노신 삼인산이 0.5~0.7중량%의 범위에서 첨가될 경우 V-0등급의 난연성이 확보되었다. 2중량%의 피로인산피페라진이 첨가된 시편의 경우 아데노신 삼인산이 0.5~0.7중량%의 범위에서 첨가될 경우 V-0등급의 난연성이 확보되었다. 폴리인산암모늄을 첨가한 시편의 경우, 폴리인산 암모늄을 각각 7.5중량%, 10중량% 첨가하였다. 해당 비교군 시편들의 경우 V-2 혹은 V-1의 난연성을 가짐을 확인하였다. 7.5중량%의 폴리인산암모늄이 첨가된 시편의 경우 아데노신 삼인산이 1.5~2중량%의 범위에서 첨가될 경우 V-0등급의 난연성이 확보되었다. 10중량%의 폴리인산암모늄이 첨가된 시편의 경우 아데노신 삼인산이 0.5~0.7중량%의 범위에서 첨가될 경우 V-0등급의 난연성이 확보되었다. 적은 양의 아데노신 삼인산 첨가만으로도 챠르의 형성 및 불연소성 가스의 생성을 극대화할 수 있기 때문에 비교군에 비해 더 좋은 난연성을 갖는다.As a comparative group, 100% by weight of the polylactic acid specimen without ATP was set, and in the case of the specimen containing piperazine pyrophosphate, 0.5% by weight, 1% by weight, and 2% by weight of piperazine pyrophosphate, respectively (Table see 1). In the case of the comparative specimens, they had a flame retardancy of V-2 or V-1. In the case of the specimen to which 0.5% by weight of piperazine pyrophosphate was added, when adenosine triphosphate was added in the range of 1.5 to 2.0% by weight, V-0 grade flame retardancy was secured. In the case of the specimen to which 1 wt% of piperazine pyrophosphate was added, when adenosine triphosphate was added in the range of 0.5 to 0.7 wt%, flame retardancy of V-0 grade was secured. In the case of the specimen to which 2% by weight of piperazine pyrophosphate was added, when adenosine triphosphate was added in the range of 0.5 to 0.7% by weight, V-0 grade flame retardancy was secured. In the case of the specimen to which ammonium polyphosphate was added, 7.5 wt% and 10 wt% of ammonium polyphosphate were added, respectively. In the case of the comparative specimens, it was confirmed that they had a flame retardancy of V-2 or V-1. In the case of the specimen to which 7.5% by weight of ammonium polyphosphate was added, when adenosine triphosphate was added in the range of 1.5 to 2% by weight, V-0 grade flame retardancy was secured. In the case of the specimen to which 10% by weight of ammonium polyphosphate was added, when adenosine triphosphate was added in the range of 0.5 to 0.7% by weight, V-0 grade flame retardancy was secured. Since it is possible to maximize the formation of char and the generation of incombustible gas only by adding a small amount of adenosine triphosphate, it has better flame retardancy compared to the comparative group.
상기에서는 본 발명의 바람직한 실시예를 참조하여 설명하였지만, 해당 기술분야의 숙련된 당업자는 하기의 특허 청구 범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있음을 이해할 수 있을 것이다.Although the above has been described with reference to the preferred embodiments of the present invention, those skilled in the art can variously modify and change the present invention without departing from the spirit and scope of the present invention as set forth in the following claims. You will understand that you can.
Claims (8)
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱.
polylactic acid; phosphorus-based flame retardants; and adenosine triphosphate (ATP);
Flame-retardant plastics based on adenosine triphosphate and polylactic acid.
상기 인계 난연제는 폴리인산암모늄(Ammonium polyphosphate; APP) 또는 피로인산피페라진(Piperazine pyrophosphate; PPP) 중 어느 하나인,
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱.
The method of claim 1,
The phosphorus-based flame retardant is any one of ammonium polyphosphate (Ammonium polyphosphate; APP) or piperazine pyrophosphate (PPP),
Flame-retardant plastics based on adenosine triphosphate and polylactic acid.
상기 인계 난연제가 폴리인산암모늄(APP)인 경우,
89.4 내지 91wt%의 폴리젖산; 7.5 내지 10wt%의 폴리인산암모늄; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는,
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱.
3. The method of claim 2,
When the phosphorus-based flame retardant is ammonium polyphosphate (APP),
89.4 to 91 wt % polylactic acid; 7.5 to 10 wt% of ammonium polyphosphate; and 0.6 to 1.5 wt% of adenosine triphosphate,
Flame-retardant plastics based on adenosine triphosphate and polylactic acid.
상기 인계 난연제가 피로인산피페라진(PPP)인 경우,
97.4 내지 98.4wt%의 폴리젖산; 0.5 내지 2wt%의 피로인산피페라진; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는,
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱.
3. The method of claim 2,
When the phosphorus-based flame retardant is piperazine pyrophosphate (PPP),
97.4 to 98.4 wt % of polylactic acid; 0.5 to 2 wt% of piperazine pyrophosphate; and 0.6 to 1.5 wt% of adenosine triphosphate,
Flame-retardant plastics based on adenosine triphosphate and polylactic acid.
상기 샘플을 금형에 넣고 170℃ 온도 및 150MPa 압력에서 10분간 압축시키는 단계를 포함하는,
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱의 제조 방법.
polylactic acid in powder form; Any one of ammonium polyphosphate (APP) or piperazine pyrophosphate (PPP); and preparing a sample through an extrusion process by mixing adenosine triphosphate; and
Putting the sample into a mold and compressing it for 10 minutes at a temperature of 170° C. and a pressure of 150 MPa,
Method for producing flame-retardant plastics based on adenosine triphosphate and polylactic acid.
인계 난연제가 폴리인산암모늄(APP)인 경우,
89.4 내지 91wt%의 폴리젖산; 7.5 내지 10wt%의 폴리인산암모늄; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는,
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱의 제조 방법.
6. The method of claim 5,
When the phosphorus-based flame retardant is ammonium polyphosphate (APP),
89.4 to 91 wt % polylactic acid; 7.5 to 10 wt% of ammonium polyphosphate; and 0.6 to 1.5 wt% of adenosine triphosphate,
Method for producing flame-retardant plastics based on adenosine triphosphate and polylactic acid.
인계 난연제가 피로인산피페라진(PPP)인 경우,
97.4 내지 98.4wt%의 폴리젖산; 0.5 내지 2wt%의 피로인산피페라진; 및 0.6 내지 1.5wt%의 아데노신 삼인산을 포함하는,
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱의 제조 방법.
6. The method of claim 5,
When the phosphorus-based flame retardant is piperazine pyrophosphate (PPP),
97.4 to 98.4 wt % of polylactic acid; 0.5 to 2 wt% of piperazine pyrophosphate; and 0.6 to 1.5 wt% of adenosine triphosphate,
Method for producing flame-retardant plastics based on adenosine triphosphate and polylactic acid.
아데노신 삼인산 및 폴리젖산에 기반한 난연성 플라스틱.Prepared by the method of any one of claims 5 to 7,
Flame-retardant plastics based on adenosine triphosphate and polylactic acid.
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