KR100750626B1 - Styrene-form with excellent insulation and a manufacturing method thereof - Google Patents
Styrene-form with excellent insulation and a manufacturing method thereof Download PDFInfo
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- KR100750626B1 KR100750626B1 KR1020060138549A KR20060138549A KR100750626B1 KR 100750626 B1 KR100750626 B1 KR 100750626B1 KR 1020060138549 A KR1020060138549 A KR 1020060138549A KR 20060138549 A KR20060138549 A KR 20060138549A KR 100750626 B1 KR100750626 B1 KR 100750626B1
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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Abstract
Description
본 발명은 단열성이 우수한 압출 스티렌 폼 제조방법에 관한 것으로, 더욱 상세하게는 주원료인 폴리스티렌수지에 흑연분말, 난연제, 조핵제를 압출기에 투입하고, 용융한 다음, 발포제를 투입하여 압출하는 방법으로 단열성이 우수한 압출 스티렌 폼을 제조하고자 하는 것이다.The present invention relates to a method for producing an extruded styrene foam having excellent thermal insulation, and more particularly, to a polystyrene resin as a main raw material, graphite powder, a flame retardant, and a nucleating agent are added to an extruder, melted, and then extruded by adding a blowing agent. It is to make this excellent extruded styrene foam.
단열용으로 사용된 발포된 폴리스티렌 발포체 보드의 밀도는 일반적으로 약 30 g/ℓ인데, 그 이유는 팽창된 폴리스티렌 발포체의 열전도도가 상기 밀도에서 최소 값을 갖기 때문이다.The density of foamed polystyrene foam boards used for thermal insulation is generally about 30 g / l, since the thermal conductivity of the expanded polystyrene foam has a minimum value at this density.
단열용으로 사용된 발포된 폴리스티렌 발포체 보드의 밀도는 일반적으로 약 30 g/ℓ인데, 그 이유는 팽창된 폴리스티렌 발포체의 열전도도가 상기 밀도에서 최소 값을 갖기 때문이다. The density of foamed polystyrene foam boards used for thermal insulation is generally about 30 g / l, since the thermal conductivity of the expanded polystyrene foam has a minimum value at this density.
재료 및 공간을 절약하기 위하여, 보다 낮은 밀도, 특히 15 g/ℓ 미만을 갖는 발포체 보드를 단열을 위해 사용하는 것이 바람직하다. 상기 발포체의 제조는 기술적으로는 문제점이 없다. In order to save material and space, it is preferable to use foam boards having a lower density, in particular less than 15 g / l, for thermal insulation. The production of such foams is technically free of problems.
그러나, 상기 낮은 밀도를 갖는 발포체 보드는 단열 성능을 급격하게 감소시켜 열전도도 등급 035 (DIN 18 164, 1부)의 필요조건을 만족시키지 않는다. However, the low density foam boards dramatically reduce the thermal insulation performance and do not meet the requirements of thermal conductivity class 035 (DIN 18 164, 1 part).
발포체의 열전도도는 카본 블랙, 금속 산화물, 금속 분말 또는 안료와 같은 무열 재료의 혼입에 의해 감소될 수 있음은 공지되어 있다. It is known that the thermal conductivity of the foam can be reduced by the incorporation of heatless materials such as carbon black, metal oxides, metal powders or pigments.
따라서, 유럽 특허 공개 공보 제372 343호에는 카본 블랙 1 내지 25 중량%를 함유하는 폴리스티렌 발포체가 기재되어 있다. 카본 블랙의 입도는 10 내지 100 ㎚이다. Thus, EP 372 343 describes polystyrene foams containing 1 to 25% by weight carbon black. The particle size of the carbon black is 10 to 100 nm.
기재된 폴리스티렌 발포체는 주로 압출법에 의해 제조되고, 바람직하게 밀도는 32-40g/ℓ이다. 또한, 폴리스티렌 중 카본 블랙 농축물을 발포제와 함께 폴리스티렌 용융물로 혼합하고 상기 혼합물을 압출하고 결정화하여 발포제를 함유하는 미립자상 폴리스티렌을 제조하는 방법이 기재되어 있으며 이는 제조방법이 매우 복잡하다. The polystyrene foams described are mainly produced by extrusion method, preferably the density is 32-40 g / l. Also described is a process for mixing carbon black concentrate in polystyrene with a blowing agent into a polystyrene melt and extruding and crystallizing the mixture to produce particulate polystyrene containing blowing agent which is very complicated.
국제 특허 공개 공보 제94/13721호에는 카본 블랙의 입도가 150㎚ 초과인 유사 발포체가 기재되어 있다. International Publication No. 94/13721 describes similar foams with a particle size of carbon black greater than 150 nm.
유럽 특허 공개 공보 제620 246호에는 미립자상 무열 재료, 특히 카본 블랙과 또한 흑연을 함유하는 팽창된 폴리스티렌 발포체 성형물이 기재되어 있다. 성형물의 밀도는 20g/ℓ 미만이다. EP 620 246 describes expanded polystyrene foam moldings containing particulate heatless materials, in particular carbon black and also graphite. The density of the moldings is less than 20 g / l.
입자를 성형물에 혼입시키는 것은 바람직하게는 예비 발포화된 폴리스티렌 비드의 표면을 코팅하거나 또는 아직 발포화되지 않은 폴리스티렌 입자체에 매립시킴으로써 수행된다. 그러나 폴리스티렌 입자의 표면상에 입자를 분포시키는 것은 예비 발포화된 비드의 접착을 대단히 손상하여 저품질의 발포체를 유발하며, 또한 입자는 성형물의 표면에서 벗겨질 수 있다. 두 경우 모두에서 입자는 폴리스티렌 입자의 내부에 균일하게 분포되지 않는다.The incorporation of the particles into the molding is preferably carried out by coating the surface of the prefoamed polystyrene beads or by embedding them in a polystyrene particle body which has not yet been foamed. However, distributing the particles on the surface of the polystyrene particles greatly impairs the adhesion of the prefoamed beads, resulting in low quality foams, and the particles can also peel off from the surface of the moldings. In both cases the particles are not evenly distributed inside the polystyrene particles.
본 발명은 상기와 같은 문제점을 감안하여 이를 해소하고자 발명한 것으로서, 그 목적은 낮은 밀도 및 특히 낮은 열전도도를 갖는 발포된 폴리스티렌 발포체를 형성하고 양호한 가공 특성 및 양호한 물리적 특성을 갖도록 가공될 수 있는 흑연을 함유하는 단열성이 우수한 압출 스티렌 폼 및 그 제조방법을 제공함에 있다.The present invention has been invented to solve the above problems, and an object thereof is to form a foamed polystyrene foam having low density and especially low thermal conductivity and to be processed to have good processing properties and good physical properties. The present invention provides an extruded styrene foam having excellent heat insulation and a method of manufacturing the same.
상기 목적을 달성하기 위한 본 발명의 특징적인 기술적 구성은, 폴리스티렌수지 중량대비 흑연분말 0.1-5중량%, 난연제는 브롬계로 HBCD 1-5중량%, 조핵제 0.3-4중량%를 압출기에 투입하여 180-240℃에서 용융하고, 이에 발포제 3-15중량%를 투입하여 100-140℃에서 압출하는 것으로 이루어진다.Characteristic technical features of the present invention for achieving the above object, 0.1-5% by weight of graphite powder relative to the weight of polystyrene resin, flame retardant is added to the extruder by broth-based HBCD 1-5% by weight, nucleating agent 0.3-4% by weight It melts at 180-240 ° C, and 3-15% by weight of blowing agent is extruded at 100-140 ° C.
그리고, 상기 흑연분말은 천연흑연 또는 합성흑연(인조흑연)중 어느 하나이고, 상기 HBCD는 EPS(expanded polystyrene foam)나 XPS(extruded polystyrene foam)중 어느 하나이며, 상기 조핵제는 TALC, 탄산칼슘, 실리카 중 어느 하나이고, 상기 발포제는 H2O, 알콜, 가압화하여 액화상태가 된 HCFC류 (HCFC-22, HCFC-142b), 부탄, CO2, DME(CH3OCH3) 중 어느 하나이다.In addition, the graphite powder is any one of natural graphite or synthetic graphite (artificial graphite), the HBCD is any one of expanded polystyrene foam (EPS) or extruded polystyrene foam (XPS), the nucleating agent is TALC, calcium carbonate, Any one of silica, and the blowing agent is any one of H 2 O, alcohol, HCFCs (HCFC-22, HCFC-142b), butane, CO 2 , DME (CH 3 OCH 3 ) that has been liquefied by pressing.
상기와 같은 특징을 갖는 본 발명의 단열성이 우수한 압출 스티렌 폼 제조방 법을 구체적으로 설명하면 다음과 같다.Referring to the method of producing an extruded styrene foam with excellent thermal insulation of the present invention having the above characteristics as follows.
먼저 본 발명의 단열성이 우수한 압출 스티렌 폼을 제조하기 위하여 사용되는 각 성분의 사용함량 이유를 설명하면 다음과 같다.First, the reasons for the content of each component used to prepare the extruded styrene foam having excellent thermal insulation of the present invention will be described.
폴리스티렌 수지(중합체)는 중량 분자량이 20 - 30만으로 압출용도에 쓰는 것을 주재료로 사용하였다. 압출조건에 따라 재활용한 스티로폼 폴리스티렌 중합체도 주재료 대비 0.1 - 50%에서 사용 할 수 있는데 open cell형성 등으로 인한 단열성 저하나 품질 불균일로 인한 공정불안 제기되지 않도록 한다.Polystyrene resin (polymer) was used as the main material for use in extrusion applications with a weight molecular weight of 20-300,000. Styrofoam polystyrene polymer recycled according to extrusion conditions can be used at 0.1-50% of the main material, so that process unstable due to poor thermal insulation or uneven quality due to open cell formation can be avoided.
흑연분말은 천연흑연 또는 합성흑연(인조흑연)중 어느 것을 사용해도 가능하며, 그 사용량을 0.1-5중량%로 하는 이유는, 0.1중량% 미만에서는 단열성 개선여부가 나타나지 않고, 5중량%를 초과하게 되면 cell을 open시키는 것을 포함 cell 구조에 영향을 미쳐 열전도율 하락보다는 열전도율을 상승시키기 때문에 흑연 사용량을 0.1-5중량%로 하였다.The graphite powder may be either natural graphite or synthetic graphite (artificial graphite). The reason for the amount of the graphite powder used is 0.1-5% by weight. When used, the amount of graphite used was 0.1-5% by weight because it affects the cell structure including opening the cell, thereby increasing the thermal conductivity rather than decreasing the thermal conductivity.
또한 흑연의 밀도는 20-40g/ℓ인데, 그 이유는 20g/ℓ이하에서는 저밀도로 제품형상을 유지하기 어렵고, 40g/ℓ이상에서는 고밀도로 제조원가 상승으로 비경제적이다.In addition, the graphite has a density of 20-40 g / l, which is difficult to maintain the product shape at a low density below 20 g / l, and is uneconomical due to a high manufacturing cost at a high density above 40 g / l.
상기 합성흑연 즉, 인조흑연이라 함은 석유정제후 남은 찌거기인 석유코크나 석탄에서 추출되는 코크(coke)등을 2,500℃이상에서 가열하면 정향배열 구조를 바꾸는 흑연 화(graphiteization)과정을 거친 것을 인조흑연(합성흑연)이라고 한다.The synthetic graphite, that is, artificial graphite, is a graphitization process that changes the structure of the clove array when the coke extracted from petroleum coke or the coke extracted from coal is heated at 2,500 ° C. or more. It is called graphite (synthetic graphite).
난연제는 브롬계로서 그 브롬계를 사용하는 이유는 발포 폴리스티렌 폼 보드는 브롬이 들어감으로 해서 불연성가스 생성소화 작용 등 난연 메카니즘으로 자기 소화성을 갖게 하기 위함이다. 상기 난연제는 분말형태로 투입하거나 투입 전 폴리스티렌수지와 혼합(마스터뱃치) 펠렛 형태로 사용하며, 그 사용량은1-5중량%인데 그 이유는, 1중량%미만은 KS M 3808 연소성기준을 맞출 수 없고, 5중량% 초과시는 고가 난연제 사용으로 비경제적이며 제품물성 강도, 열전도율을 저하시키기 때문에 1-5중량% 사용하였다.The flame retardant is bromine-based, and the reason for using the bromine-based foam is that the expanded polystyrene foam board is made of bromine so that it is self-extinguishing by flame retardant mechanisms such as incombustible gas generation and digestion. The flame retardant is used in the form of powder or in the form of mixed (master batch) pellets with polystyrene resin before use, and its amount is 1-5% by weight, because less than 1% by weight can meet the KS M 3808 combustibility standards. If it is more than 5% by weight, it is uneconomical with the use of expensive flame retardant, and 1-5% by weight is used because it lowers product strength and thermal conductivity.
상기와 같이 사용되는 난연제는 브롬계로 HBCD인데, 그 HBCD는 Hexabromocyclododecane으로 유기 할로겐계 난연재로 폴리스티렌을 기본으로 하는 EPS(expanded polystyrene foam)에나 XPS(extruded polystyrene foam)등에 주로 사용한다.The flame retardant used as described above is bromine-based HBCD, the HBCD is Hexabromocyclododecane is an organic halogen-based flame retardant material used in polystyrene-based EPS (expanded polystyrene foam) or XPS (extruded polystyrene foam).
조핵제는 압출법 발포성 폴리스티렌 중합체 제조시 단열성을 보완하기 위해 사용됨과 동시에 발포 Cell 크기를 작게 하거나 균일하게 만들어 주기 위해 사용되는 것으로 그 사용량은 0.3-4.0% 투입함이 바람직하다.The nucleating agent is used to supplement the thermal insulation during the manufacture of the extruded expandable polystyrene polymer and at the same time, it is used to make the expanded cell size small or uniform. The amount of the nucleating agent is preferably 0.3-4.0%.
발포제는 폴리스티렌수지의 충분히 발포를 유도하기 위하여 사용되는 것으로 그 사용량은 3-15중량%인데 그 이유는, 3중량%이하에서는 폴리스티렌수지를 충분히 발포 할 수 없으므로 제품의 밀도를 상승시킬 수 있으며, 15중량%를 초과하면 발포제 손실이 발생하여 비경제적이며 평평한 판상을 얻기 어렵다. 따라서 발포제는 3-15중량% 사용함이 바람직하다.The blowing agent is used to induce sufficient foaming of the polystyrene resin. The amount of the blowing agent is 3-15% by weight because the polystyrene resin cannot be sufficiently foamed below 3% by weight, thereby increasing the density of the product. Exceeding the weight% causes blowing agent loss, making it difficult to obtain an uneconomical and flat plate. Therefore, it is preferable to use 3-15% by weight of the blowing agent.
상기 발포제는 H2O, 알콜, 가압화여 액화상태가 된 HCFC류 (HCFC-22, HCFC-142b), 부탄, CO2, DME(CH3OCH3) 중 어느 하나이고, 상기 HCFC류 즉 HCFC-22(클로로 디플루오르 메탄(Monochloro difluoro methane)), HCFC-142b(클로로디플루오르 에탄(Monochloro difluoro ethane))이다.The blowing agent is any one of H 2 O, alcohol, HCFCs (HCFC-22, HCFC-142b), butane, CO 2, and DME (CH 3 OCH 3 ) which have been liquefied under pressure. 22 (Monochloro difluoro methane), HCFC-142b (Monochloro difluoro ethane).
이하 본 발명의 실시예를 들어 상세히 설명하면 다음과 같다.Hereinafter, an embodiment of the present invention will be described in detail.
(실시예1)Example 1
폴리스티렌 수지(LG화학 24HRE) 100kg를 첨가제로 난연제3kg, 조핵제1kg를 혼합 투입하고 220℃에 녹이고 발포제 HCFC22,142b를 8kg 투입 120℃로 냉각 압출 발포폴리스티렌 중합체를 만들었다. 밀도는 30g/ℓ이였다. 열전도율 시험방법 평균온도 20± 5℃에 KS L 9016으로 열전도율은 0.0253W/mk이였다. 그리고 흑연입자를 0.3% 투입했을 때에 0.0235W/mk을 얻었다.100 kg of polystyrene resin (LG Chemistry 24HRE) was added as an additive to flame retardant 3 kg, 1 kg of nucleating agent was mixed and dissolved at 220 ° C., and 8 kg of blowing agent HCFC22,142b was added to 120 ° C. to produce a cold extrusion expanded polystyrene polymer. The density was 30 g / l. Thermal conductivity test method KS L 9016 at the average temperature of 20 ± 5 ℃, the thermal conductivity was 0.0253W / mk. And 0.0235 W / mk was obtained when 0.3% of graphite particles were added.
(실시예2)Example 2
상기예에 같은 조건으로 흑연입자를 0.9% 투입시에는 0.0218w/mk을 얻었다.When the graphite particles were added 0.9% under the same conditions as in the above example, 0.0218w / mk was obtained.
(실시예3)Example 3
상기예에 같은 조건에서 반복적으로 0.9% 투입시 0.0225w/mk을 얻었다.0.0225w / mk was obtained when 0.9% was added repeatedly under the same conditions in the above examples.
(실시예4)Example 4
폴리스티렌 수지(LG화학 24HRE) 100kg를 첨가제로 난연제3kg, 조핵제2kg를 혼합 투입하고 220℃에 녹이고 발포제 HCFC22,142b를 9kg 투입 120℃로 냉각 압출 발포폴리스티렌 중합체를 만들었다. 밀도는 30g/ℓ이였다. 열전도율은 0.0236W/mk이였다. 그리고 흑연입자를 0.9% 투입했을 때에 0.0212W/mk을 얻었다.100 kg of polystyrene resin (LG Chemistry 24HRE) was added as an additive to flame retardant 3 kg and nucleating agent 2 kg, and the mixture was dissolved at 220 ° C., and 9 kg of blowing agent HCFC22,142b was added to 120 ° C. to produce a cold-extruded polystyrene polymer. The density was 30 g / l. The thermal conductivity was 0.0236 W / mk. And 0.0212 W / mk was obtained when 0.9% of graphite particles were added.
(실시예5)Example 5
폴리스티렌 수지(LG화학 24HRE) 100kg를 첨가제로 난연제3kg, 조핵제1kg를 혼합 투입하고, 220℃에 녹이고 발포제 HCFC22,142b를 8kg 투입 120℃로 냉각 압출 발포폴리스티렌 중합체를 만들었다. 밀도는 30g/ℓ이였다. 열전도율은 0.0241W/mk이였다. 그리고 흑연입자를 2.4% 투입했을 때에 0.0204W/mk을 얻었다.100 kg of polystyrene resin (LG Chemistry 24HRE) was added as an additive to flame retardant 3 kg and 1 kg of nucleating agent, and the mixture was dissolved in 220 ° C., and 8 kg of blowing agent HCFC22,142b was added to 120 ° C. to produce a cold-extruded polystyrene polymer. The density was 30 g / l. The thermal conductivity was 0.0241 W / mk. And when 2.4% of graphite particles were added, 0.0204 W / mk was obtained.
상술한 바와 같은 본 발명은 폴리스티렌수지 중량대비 흑연분말 0.1-5중량%, 난연제는 브롬계로 HBCD 1-5중량%, 조핵제 0.3-4중량%를 압출기에 투입하여 180-240℃에서 용융하고, 이에 발포제 3-15중량%를 투입하여 100-140℃에서 압출함으로서, 낮은 밀도 및 낮은 열전도도를 갖는 폴리스티렌 발포체를 형성하고, 양호한 가공 특성 및 양호한 물리적 특성을 갖는 단열성이 우수한 압출 스티렌 폼 제조방법 제공할 수 있는 효과가 있다.The present invention as described above is 0.1-5% by weight graphite powder relative to the weight of the polystyrene resin, flame retardant is bromine-based, 1-5% by weight of HBCD, 0.3-4% by weight of the nucleating agent is melted at 180-240 ℃, 3-15% by weight of the blowing agent is extruded at 100-140 ° C. to form a polystyrene foam having a low density and low thermal conductivity, thereby providing an extruded styrene foam manufacturing method having excellent heat insulating properties having good processing properties and good physical properties. It can work.
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CN104151674A (en) * | 2014-08-25 | 2014-11-19 | 倪海霞 | Flame-retardant ceiling and preparation method thereof |
KR101484615B1 (en) | 2013-05-09 | 2015-01-21 | 주식회사 벽산 | Method for manufacturing styrene-form with excellent insulation and non-deformation |
KR20160038163A (en) * | 2014-09-29 | 2016-04-07 | 주식회사 벽산 | styrene-form using blowing agent compromising carbon dioxide with excellent insulation and a manufacturing method thoereof |
KR101689675B1 (en) * | 2015-10-20 | 2016-12-27 | 남정욱 | Fire retardant polystyrene materials using foam fire retardant rating |
KR101928336B1 (en) | 2015-11-11 | 2018-12-12 | 명일폼주식회사 | Composition for polystyrene foam and a manufacturing method for extruded polystyrene form using the same |
KR101977818B1 (en) | 2018-05-11 | 2019-05-13 | 제일화학주식회사 | Flame retardant master batch composition for extruded polystyrene foam and extruded polystyrene foam using the same |
KR20220040612A (en) | 2020-09-24 | 2022-03-31 | 고하연 | Fire retardant polystyrene foam and making process thereof |
KR20220141178A (en) | 2021-04-12 | 2022-10-19 | 김선희 | Method for preparing flame retardant expanded polystyrene panel and the blind therefrom |
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KR20140085248A (en) * | 2012-12-27 | 2014-07-07 | 제일모직주식회사 | Expandable resin composition, method for preparing the same and foam using the same |
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KR101484615B1 (en) | 2013-05-09 | 2015-01-21 | 주식회사 벽산 | Method for manufacturing styrene-form with excellent insulation and non-deformation |
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KR101977818B1 (en) | 2018-05-11 | 2019-05-13 | 제일화학주식회사 | Flame retardant master batch composition for extruded polystyrene foam and extruded polystyrene foam using the same |
KR20220040612A (en) | 2020-09-24 | 2022-03-31 | 고하연 | Fire retardant polystyrene foam and making process thereof |
KR20220141178A (en) | 2021-04-12 | 2022-10-19 | 김선희 | Method for preparing flame retardant expanded polystyrene panel and the blind therefrom |
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