KR20030091853A - Flame retardant powder composition - Google Patents
Flame retardant powder composition Download PDFInfo
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- KR20030091853A KR20030091853A KR1020030067113A KR20030067113A KR20030091853A KR 20030091853 A KR20030091853 A KR 20030091853A KR 1020030067113 A KR1020030067113 A KR 1020030067113A KR 20030067113 A KR20030067113 A KR 20030067113A KR 20030091853 A KR20030091853 A KR 20030091853A
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/016—Flame-proofing or flame-retarding additives
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
본 발명은 난연제 분말의 조성물에 관한 것으로서, 무독성, 무해성등을 가진 환경친화형의 금속수산화물인 수산화마그네슘(Mg(OH)2), 수산화알루미늄(Al(OH)3)과 인산염인 암모늄 폴리포스페이트(NH4PO3)를 물(H2O)과 수화 반응시켜 만들어진 화합물에 히드록시아파타이트(hydroxyapatite,(Ca10(PO4)6(OH)2))를 첨가한 조성물로 모든 열가소성수지 및 합성고무에 충진제로서의 안정성이 높은 새로운 타입의 난연제이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a composition of a flame retardant powder, and is an ammonium polyphosphate that is a phosphate of magnesium hydroxide (Mg (OH) 2 ), aluminum hydroxide (Al (OH) 3 ), which is an environmentally friendly metal hydroxide having nontoxicity, and no harm. All thermoplastic resins and synthetic compounds containing hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 )) added to a compound prepared by hydration of (NH 4 PO 3 ) with water (H 2 O). It is a new type of flame retardant with high stability as a filler in rubber.
금속산화물인 수산화마그네슘(Mg(OH)2), 수산화알루미늄(Al(OH)3)과 인산염 암모늄 폴리포스페이트(ammonium polyphosphate)를 물(H2O)와 반응시킨 화합물에 히드록시아파타이트(hydroxyapatite)를 첨가한 조성물을 열가소성수지 및 각종 합성고무에 충진시켜 난연성을 부여한 난연제 분말의 조성물을 만드는데 그 목적이 있다.Metal oxide, hydroxide, a magnesium (Mg (OH) 2), aluminum hydroxide (Al (OH) 3) and phosphate ammonium polyphosphate (ammonium polyphosphate) of water (H 2 O) and hydroxyapatite in reacting compound (hydroxyapatite) The purpose is to make a composition of flame retardant powder imparting flame retardancy by filling the added composition with thermoplastic resin and various synthetic rubbers.
본 발명은 난연제 분말의 조성물에 관한 것으로서, 본 발명에 속하는 기술분야는, 기존의 난연제로 사용하고 있는 금속수산화물인 수산화마그네슘(Mg(OH)2) , 수산화알루미늄(Al(OH)3)에 암모늄 폴리포스페이트(ammonium polyphosphate)를 첨가하여 물( H2O)을 반응 촉매로 하여 반응 시켜 만든 화합물에 히드록시아파타이트(hydroxyapatite)를 첨가한 조성물로, 난연효과의 평가법의 하나인 산소지수(Ol)를 높인 것의 특징으로서 유해가스의 발생이 없고, 인체의 유해성 및 장치의 부식 등의 문제점이 없어 안전성이 높은 것과 연소시 불활성 기체를 생성하므로 난연효과가 뛰어나고 금속인산염을 생성하여 견고한 피막을 생성하여 산소지수(Ol)를 높이고, 화재시 단계적 2차 난연효과로 난연성이 향상되었으며, 특히 모든 열가소성수지 및 합성고무에 적용 할 수 있다는 차이점이 기존의 난연제와의 분명한 기술의 차이가 있다.The present invention relates to a composition of a flame retardant powder, and the technical field of the present invention relates to ammonium in magnesium hydroxide (Mg (OH) 2 ) and aluminum hydroxide (Al (OH) 3 ), which are metal hydroxides used as a conventional flame retardant. Hydroxyapatite is added to a compound made by adding polyphosphate and reacting with water (H 2 O) as a reaction catalyst. Oxygen index (Ol), which is one of evaluation methods of flame retardant effects, is added. It is characterized by the high quality, no generation of harmful gas, no harm to human body and no corrosion of equipment, high safety and inert gas during combustion, so it has excellent flame retardant effect and produces metal phosphate to create a solid film to produce oxygen index. Increased (Ol) and improved flame retardancy due to staged secondary flame retardant effect in fire, especially applicable to all thermoplastic resins and synthetic rubber The difference is there is a clear difference between the technology and the existing flame retardants.
산소지수(Ol)라는 것온 시험재료가 연소를 계속하기 직전에 요하는 최저 산소농도를 %로 나타내는 방법으로, 지수가 클수록 타기 어려운 것을 나타낸다. 즉 가연성 22%, 자기소염성 23-27%, 난연성 28-34%, 고난연성 35%이상, 산소지수와 인(P)함유량과의 관계의 일례는 다음과 같다.Oxygen index (Ol) A method of expressing the minimum oxygen concentration required by the test material before it continues to burn in%. The larger the index, the more difficult to burn. That is, an example of the relationship between 22% of flammability, 23-27% of self-inflammation, 28-34% of flame retardancy, 35% or more of high flame retardancy, and oxygen index and phosphorus (P) content is as follows.
Ol(P%) PET 30(6), PE 26(8), Ol(무첨가) PET 20.5(0), PE 18.5(0), 최근 환경문제에 대한 전세계적인 관심 및 우려가 난연 플라스틱에도 고조되고 있다. 특히 서구 유럽 및 미국, 일본 등 선진국을 중심으로 2차 세계대전에서 개발돼 지금까지 주로 사용되어 왔던 안티몬계와 활로겐계 난연 플라스틱에 대한 문제점이 대두되고 있다.Ol (P%) PET 30 (6), PE 26 (8), Ol (Non-Additive) PET 20.5 (0), PE 18.5 (0), Recently, global interest and concern about environmental problems are increasing in flame retardant plastics. . In particular, problems with the antimony-based and halogenated flame-retardant plastics developed in World War II, mainly in developed countries such as Western Europe, the United States, and Japan, have been used so far.
안티몬계 난연 플라스틱은 강력한 중금속의 특징으로 인한 환경문제, 할로겐계 난연 플라스틱(브롬, 염소함유)은 할로겐화 수소를 발생시켜 가공기기를 부식 시키고, 금형부식,수지분해, 착색 등의 원인을 제공, 내광변색성이 나쁘고, 화재발생시 다량의 할로RPS 화합물발생으로 인명 및 재산피해, 할로겐화 다이옥신 및 퓨란발생 등등의 문제점을 본 발명의 난연제는 해소하게 되었다.Antimony flame retardant plastics are environmental problems due to the characteristics of strong heavy metals, and halogen flame retardant plastics (bromine and chlorine) generate hydrogen halides to corrode the processing equipment and provide the cause of mold corrosion, resin decomposition, coloring, etc. The discoloration is poor, and the fire retardant of the present invention solves the problems of life and property damage, halogenated dioxins and furan generation due to the generation of a large amount of haloRPS compounds in the event of fire.
본 발명의 기술적 과제로서, 플라스틱의 난연화 방법으로서 분자구조 변경을 통한 내열성 플라스틱의 제조, 난연성분을 플라스틱 구조 내에 화학적으로 결합 (반응형 난연제), 난연제를 플라스틱 내에 물리적으로 첨가(첨가형 난연제), 기타 난연제 코팅 또는 페인팅을 하거나 제품 디자인 변경을 통한 내열성 향상 등의 방법이 있다.As a technical problem of the present invention, as a flame retardant method of plastic production of heat-resistant plastic by changing the molecular structure, chemically bonding the flame retardant component in the plastic structure (reactive flame retardant), physically adding the flame retardant in the plastic (additional flame retardant) Other methods include improving flame resistance by coating or painting flame retardants or changing product design.
난연제의 분류로 보면 플라스틱의 난연화에 사용되는 난연제의 구분에는 크게 구성 성분에 의한 분류와 사용법에 의한 분류로 나눌수 있는데 구성 성분에 의한 분류로 보면 유기계와 무기계로 구분되며, 인계, 인, 할로겐계, 브롬화합물, 염소화합물, 금속수산화물계로 수산화알루미늄, 수산화마그네슘, 안티몬계,기타(molybden계, Zinc borate계등),이 있다.According to the classification of flame retardants, the classification of flame retardants used for flame retardation of plastics can be divided into classification by constituents and classification by usage.The classification by constituents is divided into organic and inorganic. , Bromine compounds, chlorine compounds, metal hydroxides include aluminum hydroxide, magnesium hydroxide, antimony, other (molybdenum, Zinc borate, etc.).
난연 플라스틱 기술 개요로서, 난연 플라스틱의 정의는 플라스틱은 대부분 탄소, 수소, 산소로 구성된 유기물질로 연소하기 쉬운 성질을 가지고 있다, 이러한 통상의 플라스틱은 다양한 형태로 사용되고 있는테 특히 전자제품, 건축의 내외장제 등 산업자재로서의 용도가 매우 많다. 이러한 산업자재의 경우에는 우수한 난연성을 요구 하는데 이러한 용도로 통상의 플라스틱에 난연제를 첨가 공중합 또는 폴리브렌딩(polyblending)해서 통상의 플라스틱보다 연소 속도를 늦추거나 자소성(self extinguishing)를 갖게 만든 플라스틱을 말한다.Flame retardant plastics As an overview of flame retardant plastics, the definition of flame retardant plastics is that plastics are mostly composed of organic substances composed of carbon, hydrogen and oxygen, and are easy to burn. Such conventional plastics are used in various forms, especially in electronics and architecture. There are many uses as industrial materials such as burial. In the case of these industrial materials, excellent flame retardancy is required. For this purpose, a plastic made by adding a flame retardant to a conventional plastic or copolymerizing or blending (polyblending) has a slower burning rate or has a self extinguishing effect than a conventional plastic. Say.
플라스틱의 난연화 과정에 있어서, 싸이클(cycle)과정 가연성물질---산소---열--- 과정의 가열---비열, 열전도도, 응용--- 응용 및 휘발잠열, 노화, 분혜--- 열에 불안정한 결합의 함유율, 분해잠열, 열의 공급속도, 분해거동, 기화, 확산--- 확산속도, 산소농도, 기화열, 착화--- 분해생성물의 분포, 양, 발화점, 인화점, 연소의 진행--- 연소열, 연소속도, 불 안정속도, 난연성이란 위의 각 단계와 같은 불의 발전과정을 저지하여 불의 확산을 막는 성질을 말함이고, 사용법에 의한 분류로 보면 첨가형과 반응형이 있는데 유기계, 무기계, 비닐기를 갖는 것, 카르복실기를 갖는 것, 수산기를 갖는 것, 에폭시기를 갖는 것이 있고, 반응형 난연제는 난연성분이 플라스틱에 화학적으로 결합돼 있어 외부조건과 관계없이 브로밍(blooming) 현상없이 난연성이 지속, 열경화성 플라스틱에 사용, 첨가형 난연제는 플라스틱에 물리적으로 분산돼 있으며,주로 열가소성 플라스틱에 이용 브로밍(blooming) 현상이 있음. 본 발명은 첨가형 난연제로서 장점은 제조방법이 용이하고, 난연성이 우수하고, 다양한 난연제의 사용이 가능하고, 2종 이상의 난연제의 혼합 사용이 가능(시너지 효과로 인하여 난연성의 극대), 열가소성 수지와 각종의 합성고무에 사용 할 수 있다. 본 발명의 수산화알루미늄(Al(OH)3)와 수산화마그네슘(Mg(OH)2)에 인산염 암모늄 폴리포스페이트(ammonium polyphosphate)를 첨가하여 물(H2O)를적정량 스프레이 분사하여 혼합하여 수화(水化)반응에 의한 열이 발생하여 화학적 반응을 충분히 준 다음 충분한 시간동안 숙성 하는 과정중 화학적 반응열에 의한 암모늄 개스(GAS)를 충분히 휘발 시킨후 히드록시아파타이트(hydroxyapatite)를 첨가하여 충분히 분산 혼합하여 완성시킨다.In the flame retardant process of plastics, cycle process combustible materials --- oxygen --- heat --- heating process --- specific heat, thermal conductivity, application --- application and latent heat of heat, aging, benefit- -Content of thermally unstable bonds, latent heat of decomposition, heat supply rate, decomposition behavior, vaporization, diffusion ---- Diffusion rate, oxygen concentration, heat of vaporization, ignition ---- Distribution, quantity, flash point, flash point, combustion progress --- Combustion heat, combustion rate, instability rate, and flame retardancy refer to the property of preventing the spread of fire by preventing the development of fire as in each of the above stages.In terms of usage, there are additive type and reactive type. , Having a vinyl group, having a carboxyl group, having a hydroxyl group, and having an epoxy group, the reactive flame retardant is a flame-retardant component is chemically bonded to the plastic, so that the flame retardancy is maintained without a blooming phenomenon regardless of external conditions Thermosetting Used in the plastic, the flame retardant is cheomgahyeong gotta physically dispersed in the plastic, principally that the use of roaming probe (blooming) phenomenon in thermoplastics. Advantageous Effects of the Invention The present invention is an additive flame retardant. The advantages are easy to manufacture, excellent flame retardancy, various flame retardants can be used, and mixed use of two or more flame retardants is possible (maximum flame retardancy due to synergy effect), thermoplastic resins and various It can be used for synthetic rubber. Ammonium polyphosphate is added to aluminum hydroxide (Al (OH) 3 ) and magnesium hydroxide (Mg (OH) 2 ) of the present invention to hydrate by mixing a suitable amount of spraying water (H 2 O). Heat generated by the reaction is sufficient to give a chemical reaction and then fully volatilized ammonium gas (GAS) by the heat of chemical reaction during the aging process for a sufficient time, and then hydroxyapatite is added to the dispersion and mixed sufficiently Let's do it.
본 발명의 구성에 있어서는,(1). 수산화마그네슘(Mg(OH)2)은 평균입자의 크기는 3-5㎛ , Mg(OH)2함량은 97- 98.7 wt%, 경도는 2-3, 비표면적(BET)는 10-12, (2). 수산화알루미륨(Al(OH)3)은 평균입자의 크기는 0.9-1㎛, Al(OH)3함량은 98-99.8 wt%, 비표면적(BET) 7-9 ,백색도 95이상 , PH(at 25℃) 9,5-10,5 , (3). 암모늄 폴리포스페이트(ammonium polyphosphate,(NH4PO3))는 인(燐)함량이 31-32 wt%, 질소(nitrogen) 14-15 wt%, PH 5.5-7.5, 평균입자의 크기는 0.2㎛, (4). 일반 수돗물 . (5). 히드록시아파타이트(hydroxyapatite, (Ca10(PO4)6(OH)2)),평균입자의 크기 5㎛, 백색도 95이상, PH 7.5, 비중 2,5, 본 발명의 각성분별 조성 성분 배합비는 다음과 같다.In the structure of this invention, (1). The magnesium hydroxide (Mg (OH) 2 ) has an average particle size of 3-5 μm, the Mg (OH) 2 content is 97-98.7 wt%, the hardness is 2-3, the specific surface area (BET) is 10-12, ( 2). Aluminium hydroxide (Al (OH) 3 ) has an average particle size of 0.9-1 μm, Al (OH) 3 content is 98-99.8 wt%, specific surface area (BET) 7-9, whiteness of 95 or more, PH (at 25 ° C.) 9,5-10,5, (3). Ammonium polyphosphate (NH 4 PO 3 ) contains 31-32 wt% phosphorus, 14-15 wt% nitrogen, pH 5.5-7.5, average particle size 0.2 μm, (4). General Tap Water. (5). Hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 )), average particle size 5㎛, whiteness of 95 or more, PH 7.5, specific gravity 2,5, the composition ratio of each component of the present invention is as follows Same as
실시예 1Example 1
1. 수산화마그네슘(Mg(OH)2)--- 25 wt%1.Magnesium hydroxide (Mg (OH) 2 ) --- 25 wt%
2. 수산화알루미늄(Al(OH)3)--- 25 wt%2.Aluminum hydroxide (Al (OH) 3 ) --- 25 wt%
3. 암모늄 폴리포스페이트(NH4PO3)--- 25 wt%3. Ammonium polyphosphate (NH 4 PO 3 ) --- 25 wt%
4. 일반 수돗물(H2O) --- 3 wt%4. Normal tap water (H 2 O) --- 3 wt%
5. 히드록시아파타이트(Ca10(PO4)6(OH)2)5. Hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 )
위의 실시예 1의 1. 수산화마그네슘(Mg(OH)2) 25 wt%, 2. 수산화알루미늄(Al(OH)3) 25 wt%, 3. 암모늄 폴리포스페이트(NH4PO3) 25wt%를 교반기에 넣고서 충분히 분산 하면서 교반중에 실시예 1의 1. 2. 3.전체 중량비에 4. 수돗물을 스프레이 분사 방법으로 3 wt% 첨가하면서 교반 하여 반응시킨다. 충분한 반응과 고루 분산이 이루어지면 실시예 1의 5. 히드록시아파타이트(Ca10(PO4)6(OH)2)을 25 wt% 교반기에 첨가하여 충분히 분산이 되도록 교반하여 최소 1일 정도 숙성하여 완성한 것에 그 특징이 있는 난연제 분말의 조성물.1. Example 1 of magnesium hydroxide (Mg (OH) 2 ) 25 wt%, 2. 25 wt% of aluminum hydroxide (Al (OH) 3 ), 3. 25 wt% of ammonium polyphosphate (NH 4 PO 3 ) The mixture was stirred in a stirrer while being sufficiently dispersed, while reacting by stirring while adding 1. wt. After sufficient reaction and even dispersion, 5. hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ) of Example 1 was added to a 25 wt% stirrer and stirred to be sufficiently dispersed, and aged for at least 1 day. The composition of the flame retardant powder which has the characteristics to the finished thing.
본 발명의 난연제 분말은 기존의 난연제 분말의 문제점을 해소하고, 환경친화적인 난연 플라스틱의 첨가물로서 열가소성 수지 및 각종의 합성고무등에 첨가하기가 용이하고, 작업성이 좋은 장점을 갖고 있다.The flame retardant powder of the present invention solves the problems of the existing flame retardant powder, has an advantage of being easy to add to thermoplastic resins and various synthetic rubbers as an environmentally friendly flame retardant plastic, and has good workability.
건축 단열제로 사용하는 2엑형 발포 우레탄 주제와 경화제 전체 중량비에 약 23% 난연제 분말을 첨가하여 난연 실험 결과 산소지수(Ol) 35로서 양호한 난연 효과를 나타내었다. 작업 방법은 건축 단열재 2엑형 우레탄 주제에 경화제와 전체 중량비에 약 23%의 난연제 분말을 주제에 첨가하여 충분히 교반하고 현장에서 실제 발포 작업시에 경화제를 첨가하여 발포 시켜서 시편을 사용하였다.Flame retardant experiments showed good flame retardant effect as oxygen index (Ol) 35 by adding about 23% flame retardant powder to the total weight ratio of two-pack foam urethane used as building insulation. The working method used the specimen by adding the hardener to the main body of the building insulation 2 extruded urethane and adding about 23% of the flame retardant powder to the main body and stirring the foam.
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KR100863282B1 (en) * | 2006-09-14 | 2008-10-15 | 동국대학교 산학협력단 | Synthetic method for metal hydroxide phosphate |
CN114426702A (en) * | 2022-01-19 | 2022-05-03 | 江西广源化工有限责任公司 | Composite inorganic flame retardant and preparation method thereof |
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KR100863282B1 (en) * | 2006-09-14 | 2008-10-15 | 동국대학교 산학협력단 | Synthetic method for metal hydroxide phosphate |
CN114426702A (en) * | 2022-01-19 | 2022-05-03 | 江西广源化工有限责任公司 | Composite inorganic flame retardant and preparation method thereof |
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