KR100865176B1 - Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same - Google Patents

Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same Download PDF

Info

Publication number
KR100865176B1
KR100865176B1 KR1020070028302A KR20070028302A KR100865176B1 KR 100865176 B1 KR100865176 B1 KR 100865176B1 KR 1020070028302 A KR1020070028302 A KR 1020070028302A KR 20070028302 A KR20070028302 A KR 20070028302A KR 100865176 B1 KR100865176 B1 KR 100865176B1
Authority
KR
South Korea
Prior art keywords
flame retardant
magnesium
weight
bentonite
titanium
Prior art date
Application number
KR1020070028302A
Other languages
Korean (ko)
Other versions
KR20080086294A (en
Inventor
임영진
Original Assignee
리머스(주)
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 리머스(주) filed Critical 리머스(주)
Priority to KR1020070028302A priority Critical patent/KR100865176B1/en
Publication of KR20080086294A publication Critical patent/KR20080086294A/en
Application granted granted Critical
Publication of KR100865176B1 publication Critical patent/KR100865176B1/en

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/06Organic materials
    • C09K21/10Organic materials containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/06Organic materials
    • C09K21/12Organic materials containing phosphorus
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H5/00Special paper or cardboard not otherwise provided for
    • D21H5/0082Wall papers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B27WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
    • B27KPROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
    • B27K2240/00Purpose of the treatment
    • B27K2240/30Fireproofing
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2503/00Domestic or personal
    • D10B2503/04Floor or wall coverings; Carpets
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S57/00Textiles: spinning, twisting, and twining
    • Y10S57/904Flame retardant

Abstract

본 발명은 수용성 난연제 조성물, 그 제조방법, 및 그 제조방법에 의해 제조된 난연제 조성물을 이용한 난연 처리 방법에 관한 것이다.The present invention relates to a water-soluble flame retardant composition, a method for producing the same, and a method for treating flame retardant using the flame retardant composition produced by the method.

본 발명은 인산티탄마그네슘 수용액, 벤토나이트, 콩기름, 베이킹파우더, 유화제, 올레인산, 디메틸아민을 포함한 염기, 및 인산마그네슘암모늄 수용액으로 이루어지는 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물을 제공한다.The present invention provides a titanium magnesium phosphate-bentonite flame retardant composition comprising an aqueous magnesium magnesium phosphate solution, bentonite, soybean oil, a baking powder, an emulsifier, a base including oleic acid, dimethylamine, and an aqueous magnesium ammonium phosphate solution.

본 발명은 인산티탄마그네슘 수용액과 벤토나이트의 혼합물에 인산마그네슘암모늄 수용액을 혼합하여 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물을 제조하는 방법과 상기 제조방법에 의하여 제조된 난연제 조성물을 건축자재 또는 마감재에 도포, 건조하는 난연 처리 방법을 제공한다.The present invention is a method of preparing a titanium magnesium ammonium phosphate-bentonite-based flame retardant composition by mixing a magnesium ammonium phosphate solution in a mixture of aqueous magnesium titanium phosphate solution and bentonite, and applying the flame retardant composition prepared by the above method to a building material or finish, It provides a flame retardant treatment method for drying.

본 발명에 따른 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물은 인과 질소, 그리고 수산화마그네슘, 티탄, 벤토나이트, 베이킹파우더 등에 의한 난연성 상승효과와 단일약품으로 여러 종류의 건축재에 난연처리를 할 수 있어 경제적이고, 내열, 내수, 저독성, 내화기능이 우수하고, 환경공해를 유발하지 않는 친환경적인 난연제로서 그 성능이 뛰어나며, 인체에 무해하다.The titanium magnesium ammonium phosphate-bentonite-based flame retardant composition according to the present invention is economical because it can be flame-retardant treatment of various kinds of building materials as a single chemical and a synergistic effect of phosphorus and nitrogen, magnesium hydroxide, titanium, bentonite, baking powder, etc. It is excellent in heat resistance, water resistance, low toxicity, fire resistance, eco-friendly flame retardant that does not cause environmental pollution, and its performance is excellent and harmless to human body.

수용성, 난연제, 인산티탄마그네슘, 인산마그네슘암모늄, 벤토나이트, retardant, flameproof Water Soluble, Flame Retardant, Magnesium Titanium Phosphate, Magnesium Phosphate, Bentonite, Retardant, Flameproof

Description

수용성 난연제 조성물, 그 제조방법, 및 그 제조방법에 의해 제조된 난연제 조성물을 이용한 난연 처리 방법{Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same}Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same}

도 1은 본 발명에 따른 인산티탄마그네슘암모늄-벤토나이트계 수용성 난연제 조성물의 제조방법을 나타내는 공정도이다.1 is a process chart showing a method for producing a titanium magnesium ammonium phosphate-bentonite-based water-soluble flame retardant composition according to the present invention.

도 2는 본 발명에 따른 난연제 조성물을 도포한 목재의 난연성 실험결과를 나타낸 사진이고, 도 3은 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 목재의 난연성 실험결과를 나타낸 사진이다.Figure 2 is a photograph showing the flame retardant test results of the wood coated with the flame retardant composition according to the present invention, Figure 3 is a photograph showing the flame retardant test results of the wood coated with the flame retardant composition is not added to the aqueous solution of magnesium ammonium phosphate.

도 4는 본 발명에 따른 난연제 조성물을 도포한 무늬목MDF의 난연성 실험결과를 나타낸 사진이고, 도 5는 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 무늬목MDF의 난연성 실험결과를 나타낸 사진이다.Figure 4 is a photograph showing the flame retardancy test results of the wood veneer MDF coated with a flame retardant composition according to the present invention, Figure 5 is a photograph showing the flame retardant test results of the wood veneer MDF coated with a flame retardant composition is not added to the aqueous solution of magnesium ammonium phosphate.

도 6은 본 발명에 따른 난연제 조성물을 도포한 무늬목우레탄코팅MDF의 난연성 실험결과를 나타낸 사진이고 도 7은 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 무늬목우레탄코팅MDF의 난연성 실험결과를 나타낸 사진이다.다.Figure 6 is a photograph showing the flame retardancy test results of the veneer urethane coating MDF coated with a flame retardant composition according to the present invention and Figure 7 shows the flame retardancy test results of the veneer urethane coating MDF coated with a flame retardant composition is not added to the aqueous solution of magnesium ammonium phosphate It is a photograph.

도 8은 본 발명에 따른 난연제 조성물을 도포한 PVC필름MDF의 난연성 실험결 과를 나타낸 사진이고, 도 9는 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 PVC필름MDF의 난연성 실험결과를 나타낸 사진이다.Figure 8 is a photograph showing the results of the flame retardancy test of the PVC film MDF coated with a flame retardant composition according to the present invention, Figure 9 is a flame retardancy test results of the PVC film MDF coated with a flame retardant composition is not added to the aqueous solution of magnesium ammonium phosphate It is a photograph.

본 발명은 수용성 난연제 조성물, 그 제조방법, 및 그 제조방법에 의해 제조되는 난연제 조성물을 이용한 난연 처리 방법에 관한 것으로서, 보다 상세하게는 인산티탄마그네슘 수용액, 벤토나이트, 콩기름, 베이킹파우더, 유화제, 올레인산, 디메틸아민을 포함한 염기, 및 인산마그네슘암모늄 수용액으로 이루어지는 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물, 그 제조하는 방법, 및 그 제조방법에 의해 제조된 난연제 조성물을 건축자재 또는 마감재에 도포, 건조하는 난연 처리 방법에 관한 것이다.The present invention relates to a water-soluble flame retardant composition, a method for producing the same, and a flame retardant treatment method using the flame retardant composition prepared by the method, and more particularly, an aqueous solution of titanium magnesium phosphate, bentonite, soybean oil, baking powder, emulsifier, oleic acid, Flame retardant treatment of applying and drying a titanium magnesium ammonium phosphate-bentonite flame retardant composition comprising a base containing dimethylamine and an aqueous solution of magnesium ammonium phosphate, a method for preparing the same, and a flame retardant composition prepared by the method for construction or finishing It is about a method.

천연물인 목재, MDF(또는 합판), 무늬목부착 MDF(또는 합판), PVC필름 MDF(또는 합판)등의 가연물질에 사용되고 있는 기존 난연제는 각각에 대한 단일 난연제로서 목재용, MDF(또는 합판) 무늬목용, MDF(또는 합판) 무늬목우레탄코팅용, MDF(또는 합판) PVC필름부착용 등으로 나뉘어 개별적인 난연제를 사용함으로써 경제적으로 부담이 클 뿐만 아니라, 난연제가 종류별로 난해하여 선택이 복잡한 점과, 연소시 발화를 늦추고 발연 및 유독가스량을 적게 발생하거나 억제하는 기능이 저하되는 등의 문제점이 있었다.Existing flame retardants used in combustible materials such as natural wood, MDF (or plywood), veneered MDF (or plywood), PVC film MDF (or plywood), and as a single flame retardant for each wood, MDF (or plywood) veneer And MDF (or plywood) veneer urethane coating, MDF (or plywood) PVC film, etc. It is economically burdened by using individual flame retardants. There was a problem of slowing the ignition and degrading the function of generating or suppressing the amount of fumes and toxic gases.

또한 최근 화학제품의 건축자재 보급이 빠르게 확산됨에 따라, 화재시 엄청난 유독가스와 연기발생을 일으키게 된다. 화학제품의 건축자재가 탈 때는 목재류가 탈때보다 10~25배 이상의 연기가 발생하고, 시안화수소, 염화수소, 포스겐, 일산화탄소, 이산화탄소 등의 유독가스가 발생하는 문제점이 있다.In addition, the recent rapid spread of building materials of chemical products, causing a tremendous amount of toxic gases and smoke during fire. When building materials of chemical products are burned, there is a problem that 10 to 25 times more smoke is generated than wood is burned, and toxic gases such as hydrogen cyanide, hydrogen chloride, phosgene, carbon monoxide, and carbon dioxide are generated.

연소시 건축마감재에 불이 붙으면 소재인 나무가 불쏘시게 역할을 하며 PVC시트가 타면서 유독가스와 연기를 방출하게 되어 인명의 사상이 늘어난다는 문제점을 내포하고 있다.If the building material is burned during combustion, the wood acts as a fire, and the PVC sheet burns, releasing toxic gas and smoke, which increases the lives of people.

이러한 문제점을 개선하기 위하여 저유독성가스, 저발연성, 내열성 등의 기능을 가진 난연제 제조와 난연화 처리 공법 연구가 필요하다.In order to improve these problems, it is necessary to manufacture a flame retardant having a function of low toxic gas, low smoke, heat resistance, and research on a flame retardant treatment method.

따라서 본 발명의 목적은 저유독성가스, 저발연성 및 내열성이 우수한 난연제 조성물, 그 제조방법, 및 그 제조방법에 의해 제조되는 난연제 조성물을 이용하여 건축자재 또는 마감재를 난연 처리 하는 방법을 제공하는 것이다.Accordingly, it is an object of the present invention to provide a flame retardant composition using a flame retardant composition excellent in low toxic gas, low smoke resistance and heat resistance, a method of manufacturing the same, and a flame retardant composition prepared by the method of the present invention.

본 발명의 상기 목적은 인산티탄마그네슘 수용액과 벤토나이트의 혼합물에 본 발명자에 의해 특허 출원된 인산마그네슘암모늄 수용액(대한민국 특허출원 제 2006-28243호)을 혼합하여 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물을 제조함으로써 달성할 수 있다.The object of the present invention is to prepare a titanium magnesium ammonium phosphate-bentonite flame retardant composition by mixing the aqueous magnesium ammonium phosphate (Korean Patent Application No. 2006-28243) patent application by the present inventor to a mixture of aqueous magnesium titanium phosphate solution and bentonite This can be achieved by.

본 발명은 수용성 난연제 조성물, 그 제조방법, 및 그 제조방법에 의해 제조되는 난연제 조성물을 이용한 난연 처리 방법에 관한 것이다.The present invention relates to a water-soluble flame retardant composition, a method for producing the same, and a method for treating flame retardant using the flame retardant composition produced by the method.

이하, 본 발명을 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail.

본 발명에 따른 난연제 조성물은 연소하기 쉬운 천연물인 목재, 무늬목이 부착된 MDF 또는 합판(이하, 무늬목MDF(합판)), 무늬목에 우레탄코팅을 하여 부착된 MDF 또는 합판(이하, 무늬목우레탄코팅MDF(합판)), 및 PVC 필름을 부착한 MDF 또는 합판(이하, PVC필름MDF(합판))류에 인산과 질소 그리고 금속화합물등의 난연성이 큰 화합물을 도포함으로써 발화를 늦춰주고, 연소확대를 막아 발연 및 유독가스의 발생을 억제하는데 그 특성이 있다.Flame retardant composition according to the present invention is a natural product that is easy to burn wood, veneer MDF or plywood (hereinafter, veneer MDF (plywood)), veneer MDF or plywood (hereinafter, veneer urethane coating MDF) Plywood)), and MDF or Plywood (hereinafter PVC film MDF) with PVC film attached, which are highly flame retardant such as phosphoric acid, nitrogen, and metal compounds, to slow the ignition and prevent the expansion of combustion. And it has the characteristics to suppress the generation of toxic gas.

위와 같은 특성은 상기 난연제 조성물을 인산티탄마그네슘 수용액 5~13 중량%, 벤토나이트 0.1~1.0 중량%, 콩기름 0.01~0.5 중량%, 베이킹파우더 0.01~0.5 중량%, 유화제 0.1~1.0 중량%, 올레인산 0.01~0.5 중량%, 디메틸아민을 포함한 염기 1~5 중량%, 및 인산마그네슘암모늄 수용액 85~93 중량%로 조성함으로써 달성할 수 있다.The above properties are the flame retardant composition of the titanium magnesium phosphate aqueous solution 5 ~ 13% by weight, bentonite 0.1 ~ 1.0% by weight, soybean oil 0.01 ~ 0.5% by weight, baking powder 0.01 ~ 0.5% by weight, emulsifier 0.1 ~ 1.0% by weight, oleic acid 0.01 ~ It can achieve by 0.5 weight%, 1-5 weight% of bases containing dimethylamine, and 85-93 weight% of aqueous solution of magnesium ammonium phosphate.

본 발명에 따른 난연제 조성물은 인과 질소성분에 무기계의 수산화마그네슘 및 티탄금속을 반응시켜 제조된 것이므로 수산화마그네슘 및 티탄금속의 상승작용으로 기존의 난연제보다 난연성이 훨씬 높다. 수산화마그네슘은 연소시 물을 발생시켜 수증기로 변화한다. 이렇게 변화된 수증기는 연소성 유독가스를 희석감소시킨다. 또한 연소물질인 목재나 건축내장재 등의 표면을 희석가스로 도포하여 산소의 접근을 방지하여 소화작용을 한다. 동시에 고체상 표면에서 흡열반응을 통하여 냉각 및 열분해 생성물의 생성을 감소시키는 효과가 높다. 티탄(Ti)은 물을 분해하여 수소와 티탄산을 생성하여 발수 역할을 하며 연소를 지연, 저지시키는 역할을 한다. 또한 티탄(Ti)은 커플링제로 난연물질의 부착을 도와 난연효과를 증대시킨다.The flame retardant composition according to the present invention is prepared by reacting inorganic magnesium and titanium metals with phosphorus and nitrogen components, so the flame retardancy is much higher than conventional flame retardants due to the synergy of magnesium hydroxide and titanium metals. Magnesium hydroxide turns into water vapor by producing water on combustion. This altered water vapor dilutes the combustible toxic gases. In addition, the surface of wood or building interior materials, which is a combustion material, is coated with diluent gas to prevent oxygen from accessing to extinguish. At the same time, the effect of reducing the production of cooling and pyrolysis products through the endothermic reaction on the solid phase surface is high. Titanium (Ti) decomposes water to produce hydrogen and titanic acid, which plays a water repellent role, and delays and prevents combustion. In addition, titanium (Ti) is a coupling agent to help the attachment of the flame retardant material to increase the flame retardant effect.

인산티탄마그네슘 수용액의 함량은 특별히 제한되지 않으나 5~13 중량%인 것이 바람직하다. 인산티탄마그네슘 수용액의 함량이 5 중량% 미만인 경우 티탄의 효과가 미비하고, 13 중량%를 초과하는 경우, 상대적으로 나머지 조성물의 함량이 상대적으로 줄어들어 난연성이 떨어지기 때문이다.The content of the aqueous solution of titanium magnesium phosphate is not particularly limited, but is preferably 5 to 13% by weight. If the content of the magnesium magnesium phosphate aqueous solution is less than 5% by weight, the effect of titanium is inadequate, and when the content of more than 13% by weight, the content of the remaining composition is relatively reduced and the flame retardancy is inferior.

첨가제인 벤토나이트는 연소시 다공성 스폰지처럼 팽창하게 되어, 연소시 불이 붙는 것을 막고 다공성스폰지 형태의 공간에 유독가스를 끌어당겨 견고하게 가두는 역할을 한다.Bentonite, an additive, expands like a porous sponge during combustion, and prevents fire from burning and draws toxic gas into the porous sponge-type space and tightly confines it.

베이킹파우더는 식품용 합성팽창제로서 가스발생량이 70mL/g 이상이며, 연소시 열을 받으면 난연제가 도포된 표면을 발포시켜 연소를 저지하는 역할을 한다. 콩기름은 목재, 무늬목MDF(합판), 무늬목우레탄코팅MDF(합판), 또는 PVC필름MDF(합판) 등의 코팅성 및 내수성을 증대시키고, 유화제(예: sodium lauryl sulfate)는 위한 콩기름 첨가시 분산을 원활하게 하고 난연성 조성물을 난연처리 대상기질에 도포할 때, 보다 잘 침투하여 부착될 수 있도록 한다. 또한 올레인산(Oleic acid)은 수용성 난연제 조성물을 건축자재에 도포시 건조를 촉진시킨다.Baking powder is a synthetic expansion agent for foods, the gas generation amount is 70mL / g or more, and when the heat is received during combustion, it serves to block the combustion by foaming the surface coated with the flame retardant. Soybean oil increases the coating and water resistance of wood, veneer MDF (plywood), veneer urethane coated MDF (plywood), or PVC film MDF (plywood), and the dispersion of soybean oil for emulsifiers (e.g. sodium lauryl sulfate). When the flame retardant composition is applied to the substrate to be flame retarded, it can be better penetrated and attached. In addition, oleic acid promotes drying when the water-soluble flame retardant composition is applied to building materials.

본 발명에서 벤토나이트는 0.1~1.0 중량%, 콩기름은 0.01~0.5 중량%, 베이킹파우더는 0.01~0.5 중량%, 유화제는 0.1~1.0 중량%, 올레인산은 0.01~0.5 중량%인 것이 바람직하다. 상기의 중량% 범위 밖에서는 각 조성물의 시너지 효과가 떨어진다.Bentonite in the present invention is 0.1 to 1.0% by weight, soybean oil is 0.01 to 0.5% by weight, baking powder is 0.01 to 0.5% by weight, emulsifier is 0.1 to 1.0% by weight, oleic acid is preferably 0.01 to 0.5% by weight. Outside the above weight percent range, the synergistic effect of each composition is poor.

디메틸아민은 본 발명에 따른 난연제 조성물의 제조시 미반응된 찌꺼기를 용해시키고, 난연제 조성물을 투명하게 하는 역할을 한다. 디메틸아민의 함량은 1~5 중량%인 것이 바람직하다. 디메틸아민의 함량이 1~5 중량%인 경우 난연제 조성물의 pH가 5~6으로 유지되기 때문이다.Dimethylamine dissolves unreacted debris in the manufacture of the flame retardant composition according to the invention and serves to make the flame retardant composition transparent. The content of dimethylamine is preferably 1 to 5% by weight. If the content of dimethylamine is 1 to 5% by weight because the pH of the flame retardant composition is maintained at 5-6.

본 발명에 따른 난연화 도포제 조성물을 구성하는 인산마그네슘암모늄 수용액은 난연성을 강화시키고, 도포성을 향상시키는 역할을 한다. 본 발명에 따른 난연제 조성물은 암모늄이온과 같은 질소성분을 함유하고 있어, 폴리인산의 열적 중축합을 촉진시키고 고분자 폴리인산을 생성시켜 숯 형성에 도움을 주는데, 이는 탄소가 산화되어 유독가스인 일산화탄소 및 이산화탄소가 생성되는 것을 억제한다. 그리고 인산, 질소의 상승효과는 저독성과 고성능 난연제가 되며, 화재시 연기에 대한 안정성이 크다. 또한 탈수작용에 의한 탄소피막의 형성때문에 산소를 막아 연소를 방지하는 효과도 크다.The magnesium ammonium phosphate aqueous solution constituting the flame retardant coating agent composition according to the present invention serves to enhance the flame retardancy and improve the coating property. The flame retardant composition according to the present invention contains nitrogen components such as ammonium ions, and promotes thermal polycondensation of polyphosphoric acid and helps to form charcoal by generating high molecular polyphosphoric acid, which is oxidized to carbon monoxide and carbon monoxide. Suppresses the production of carbon dioxide. In addition, the synergistic effect of phosphoric acid and nitrogen becomes a low toxicity and high performance flame retardant, and has a great safety against smoke in a fire. In addition, due to the formation of a carbon film by the dehydration action it is also effective to prevent the combustion by preventing oxygen.

인산마그네슘암모늄 수용액의 함량은 85~93 중량%인 것이 바람직하다. 인산마그네슘암모늄 수용액의 함량이 85 중량% 미만인 경우 난연성이 떨어지고, 93 중량%를 초과하는 경우에는 나머지 조성물의 효과가 거의 발현되지 않기 때문이다.The content of aqueous magnesium ammonium phosphate solution is preferably 85 to 93% by weight. If the content of the aqueous magnesium ammonium phosphate solution is less than 85% by weight, the flame retardancy is lowered, and when the content of more than 93% by weight, the effect of the remaining composition is hardly expressed.

본 발명에 따른 난연제 제조방법은 도 1과 같이Flame retardant manufacturing method according to the invention as shown in FIG.

a) 인산 수용액에 상기 인산 중량 대비 26~32 중량%의 티탄을 첨가하고 교반, 가열시켜 인산티탄{Ti2(PO4)3} 수용액을 제조하는 단계;a) adding 26 to 32% by weight of titanium to the aqueous solution of phosphoric acid, stirring and heating to prepare an aqueous solution of titanium phosphate {Ti 2 (PO 4 ) 3 };

b) 상기 인산티탄 수용액에 벤토나이트 및 수산화마그네슘을 첨가하고 교반, 가열하여 인산티탄마그네슘 수용액과 벤토나이트의 혼합물을 제조하는 단계;b) adding bentonite and magnesium hydroxide to the aqueous solution of titanium phosphate, stirring and heating to prepare a mixture of aqueous solution of titanium magnesium phosphate and bentonite;

c) 상기 인산티탄마그네슘 수용액과 벤토나이트의 혼합물에 콩기름, 베이킹파우더, 유화제, 및 올레인산을 첨가하는 단계;c) adding soybean oil, a baking powder, an emulsifier, and oleic acid to the mixture of aqueous magnesium magnesium phosphate solution and bentonite;

d) 디메틸아민을 포함한 염기를 이용하여 상기 c) 단계 후의 인산티탄마그네슘 수용액과 벤토나이트의 혼합물의 pH를 5~6으로 조정하는 단계;d) adjusting the pH of the mixture of aqueous magnesium magnesium phosphate solution and bentonite after step c) to 5-6 using a base containing dimethylamine;

e) 상기 d) 단계 후의 인산티탄마그네슘 수용액과 벤토나이트의 혼합물에 인산마그네슘암모늄 수용액을 첨가하고 혼합시키는 단계; 및e) adding and mixing an aqueous magnesium ammonium phosphate solution to the mixture of aqueous magnesium magnesium phosphate solution and bentonite after step d); And

f) 상기 e) 단계 후의 혼합물을 여과하여 미용해된 찌꺼기를 걸러주는 단계;를 포함한다.f) filtering the mixture after step e) to filter out undissolved debris.

본 발명에 따른 난연제 조성물의 제조방법에서, 상기 a) 단계의 인산티 탄{Ti2(PO4)3} 수용액은 인산 농도가 15~25 중량%인 것이 바람직하다. 인산 농도가 15 중량% 미만인 경우 난연제 조성물의 고형분 함량이 적어 효과적인 난연 처리를 위하여 너무 많은 도포 또는 분무의 회수를 필요로 한다.In the method for preparing a flame retardant composition according to the present invention, the titanium phosphate {Ti 2 (PO 4 ) 3 } aqueous solution of step a) preferably has a phosphoric acid concentration of 15 to 25% by weight. If the phosphoric acid concentration is less than 15% by weight, the solid content of the flame retardant composition is low, requiring too much application or recovery of the spray for effective flame retardant treatment.

본 발명에 따른 난연제 조성물의 제조방법에서, 상기 a) 단계의 교반 및 가열은 70~90℃의 온도에서 2~4시간 동안 교반, 가열시키는 것이 바람직하다.In the method for preparing a flame retardant composition according to the present invention, the stirring and heating of the step a) is preferably performed by stirring and heating for 2 to 4 hours at a temperature of 70 ~ 90 ℃.

본 발명에 따른 난연제 조성물의 제조방법에서, 상기 b) 단계의 벤토나이트 첨가량 및 수산화마그네슘 첨가량은 상기 a) 단계의 인산티탄 수용액 중량 대비 2~4 중량% 및 0.1~0.5 중량%인 것을 특징으로 하고, 상기 c) 단계의 콩기름, 베이킹파우더, 유화제, 및 올레인산의 첨가량은 상기 a) 단계의 인산티탄 수용액 중량 대비 1~2 중량%, 0.4~1.2 중량%, 2~3 중량%, 및 0.4~0.8 중량%인 것을 특징으로 한다.In the method for preparing a flame retardant composition according to the present invention, the amount of bentonite and magnesium hydroxide added in step b) is 2 to 4% by weight and 0.1 to 0.5% by weight based on the weight of the titanium phosphate aqueous solution in step a). The amount of the soybean oil, the baking powder, the emulsifier, and the oleic acid added in step c) may be 1 to 2% by weight, 0.4 to 1.2% by weight, 2 to 3% by weight, and 0.4 to 0.8% by weight based on the titanium phosphate aqueous solution in step a). It is characterized by being%.

본 발명에 따른 난연제 조성물의 제조방법에서, 상기 e) 단계의 인산티탄마그네슘 수용액과 벤토나이트의 혼합물의 양은 상기 인산마그네슘암모늄 수용액의 중량 대비 10~15 중량%인 것이 바람직하다.In the method for preparing a flame retardant composition according to the present invention, the amount of the mixture of the magnesium magnesium phosphate solution and bentonite in step e) is preferably 10 to 15% by weight based on the weight of the aqueous magnesium ammonium phosphate solution.

본 발명에 따른 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물의 제조방법에서, 상기 d)단계의 인산마그네슘암모늄 수용액은 본 출원인에 의해 특허출원된 발명으로서 대한민국 특허 출원 제 2006-0028243호에 개시되어 있다.In the method for preparing titanium magnesium ammonium phosphate-bentonite-based flame retardant composition according to the present invention, the aqueous solution of magnesium ammonium phosphate in step d) is disclosed in Korean Patent Application No. 2006-0028243 as an invention patented by the present applicant.

상기 인산마그네슘암모늄 수용액의 제조방법은 a') 인산 및 수산화암모늄을 수용액상에서 1 : 0.2~0.7 몰비로 혼합하는 단계; 및 b') 인산에 대하여 0.1~0.5 몰비의 수산화마그네슘을 첨가하여 교반하여 인산마그네슘암모늄을 함유한 고형분 5 내지 30 중량%의 수용액을 제조하는 단계를 포함한다.The manufacturing method of the aqueous solution of magnesium ammonium phosphate a ') mixing the phosphoric acid and ammonium hydroxide in an aqueous solution of 1: 0.2 ~ 0.7 molar ratio; And b ') adding 0.1 to 0.5 molar ratio of magnesium hydroxide to phosphoric acid and stirring to prepare an aqueous solution of 5 to 30% by weight of solid content containing ammonium magnesium phosphate.

또한 상기 인산마그네슘암모늄 수용액의 제조방법은 상기 b') 단계 후 비이온성 계면활성제, 멜라민 수지, 또는 아크릴산 에스테르계 수지 및 이들의 혼합물을 첨가하는 단계를 더 포함할 수 있다.In addition, the method of preparing the magnesium ammonium phosphate aqueous solution may further include adding a nonionic surfactant, a melamine resin, or an acrylic ester resin and a mixture thereof after step b ′).

또한, 본 발명에 따른 난연제 조성물의 제조방법은 a) 인산 수용액에 상기 인산 중량 대비 26~32 중량%의 티탄을 첨가하고 교반, 가열시켜 인산티탄{Ti2(PO4)3} 수용액을 제조하는 단계; b) 상기 인산티탄 수용액에 벤토나이트, 수산화마그네슘, 콩기름, 베이킹파우더, 유화제, 올레인산, 인산마그네슘암모늄용액을 첨가하고, 교반, 가열시킨 후 디메틸아민을 포함한 염기를 이용하여 혼합물의 pH를 5~6으로 조정하는 단계; 및 c) 상기 b) 단계 후의 혼합물을 여과하여 미용해된 찌꺼기를 걸러주는 단계; 로 구성되는 것을 포함한다.In addition, the method for preparing a flame retardant composition according to the present invention comprises a) adding 26 to 32% by weight of titanium to the aqueous solution of phosphoric acid and stirring and heating to prepare a titanium phosphate {Ti 2 (PO 4 ) 3 } aqueous solution. step; b) Bentonite, magnesium hydroxide, soybean oil, baking powder, emulsifier, oleic acid, magnesium ammonium phosphate solution are added to the aqueous titanium phosphate solution, stirred and heated, and then the pH of the mixture is adjusted to 5-6 with a base containing dimethylamine. Adjusting; And c) filtering the mixture after step b) to filter out undissolved debris; It includes what consists of.

본 발명의 또 다른 목적을 달성하기 위하여, 본 발명은 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물을 건축자재 또는 마감재에 도포하는 단계 및 상기 도포된 난연제 조성물을 건조하는 단계;를 포함하는 난연 처리 방법을 제공한다.In order to achieve another object of the present invention, the present invention is a flame retardant treatment method comprising the step of applying a titanium magnesium ammonium phosphate-bentonite-based flame retardant composition to a building material or finish and drying the applied flame retardant composition to provide.

상기 건축자재는 목재, 무늬목MDF(합판), 무늬목우레탄코팅MDF(합판), 또는 PVC필름MDF(합판) 등의 목재류이고, 상기 마감재는 종이벽지 또는 실크벽지 등의 벽지류를 포함한다. 이들 자재의 난연 처리는 본 발명에 따른 수용성 난연제 조성물을 분무기, 롤러, 또는 붓 등을 사용하여 도포시키는 방법에 의하며, 도포 회수는 2회 이상 해주어야 한다. 분무기를 사용할 경우는 약액이 건조된 후 2~3차례 반복하여 분무하여야 한다.The building material is wood, such as wood, veneer MDF (plywood), veneer urethane coating MDF (plywood), or PVC film MDF (plywood), and the finishing material includes wallpaper such as paper wallpaper or silk wallpaper. The flame retardant treatment of these materials is by the method of applying the water-soluble flame retardant composition according to the present invention using a sprayer, a roller, a brush, or the like, and the number of times of application should be applied two or more times. If a nebulizer is used, it should be sprayed two to three times after the chemical is dried.

이렇게 난연제 조성물을 도포한 후 상온에서 3~4일 동안 완전건조시킨다. 건조실에서 건조시킬 경우는 60℃에서 1일 ~ 2일간 건조시킨다.After applying the flame retardant composition is dried completely for 3 to 4 days at room temperature. In the case of drying in a drying room, it is dried for 1 day to 2 days at 60 ℃.

본 발명에 따른 난연제 조성물을 사용할 경우 난연성, 내수성, 내열성 및 내마모성이 우수한 장점이 있다. 또한 단일 약품 한가지로 목재, 무늬목MDF(합판), 무늬목우레탄코팅MDF(합판), 또는 PVC필름MDF 등의 목재류 및 종이벽지 또는 실크벽지 등의 벽지류에 적용이 가능하다. 본 발명에 따른 난연제 조성물을 종이벽지 및 실크벽지에 적용한 실험결과를 도 9와 도 10에 나타내었다.When using the flame retardant composition according to the present invention has the advantage of excellent flame retardancy, water resistance, heat resistance and wear resistance. In addition, it is applicable to wood, such as wood, veneer MDF (plywood), veneer urethane coating MDF (plywood), or PVC film MDF and wallpaper such as paper wallpaper or silk wallpaper. Experimental results of applying the flame retardant composition according to the present invention to paper wallpaper and silk wallpaper are shown in FIGS. 9 and 10.

이하 실시예를 통하여 본 발명을 더 구체적으로 설명하나, 하기 실시예는 본 발명의 예시에 불과한 것으로서, 본 발명의 특허청구범위가 이에 따라 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the following Examples are merely illustrative of the present invention, and the claims of the present invention are not limited thereto.

실시예 1 : 수용성 난연제 조성물의 제조 Example 1 Preparation of Water-Soluble Flame Retardant Composition

21 중량%의 인산수용액 50.3g과 티탄금속 2~3mm 조각 3g을 교반기가 장착된 가열 반응기에 투입한 후 80℃에서 3시간 용해시켰다. 이때 pH는 1.0 정도가 되며, 진한 가지색의 인산티탄{Ti2(PO4)3} 수용액이 제조되었다.50.3 g of 21 wt% aqueous solution of phosphoric acid and 3 g of 2-3 mm pieces of titanium metal were added to a heating reactor equipped with a stirrer and dissolved at 80 ° C. for 3 hours. At this time, the pH was about 1.0, and a dark brown titanium phosphate {Ti 2 (PO 4 ) 3 } aqueous solution was prepared.

다음 단계로 상기 용액 100cc(149.76g)에 벤토나이트(Bentonite) 4.73g과 수산화마그네슘 0.38g을 첨가하여 30분간 가열하여, 인산티탄마그네슘 수용액과 벤토나이트의 혼합물을 제조하였다.In a next step, 4.73 g of bentonite and 0.38 g of magnesium hydroxide were added to 100 cc (149.76 g) of the solution, followed by heating for 30 minutes to prepare a mixture of aqueous titanium magnesium phosphate solution and bentonite.

상기 수용액에 콩기름 3cc(1.77g), 베이킹파우더 1cc(1.17g), 유화제(sodium lauryl sulfate) 3cc(4.03g), 및 올레인산(oleic acid) 1cc(0.99g)을 첨가하고 교반하여 혼합물 수용액을 제조하였다.Soybean oil 3cc (1.77g), baking powder 1cc (1.17g), emulsifier (sodium lauryl sulfate) 3cc (4.03g), and oleic acid 1cc (0.99g) was added and stirred to prepare a mixture aqueous solution It was.

상기 혼합물 수용액은 pH가 1.0 정도로 강산이었으며, 디메틸아민(dimethyl amine) 50cc(44g)을 첨가하여 pH를 5~6 정도로 조정하였다.The mixture solution was a strong acid pH of about 1.0, the pH was adjusted to about 5 ~ 6 by the addition of 50cc (44g) of dimethyl amine (dimethyl amine).

다음 단계로 상기 제조된 혼합물 수용액 10cc(14.27g)와 인산마그네슘암모늄(대한민국 특허출원번호 10-2006-28243) 수용액 100cc(115.55g)를 혼합하여 수용성 난연제 조성물을 제조하였다.Next, a water-soluble flame retardant composition was prepared by mixing 10 cc (14.27 g) of the aqueous solution of the mixture prepared above and 100 cc (115.55 g) of aqueous solution of magnesium ammonium phosphate (Korean Patent Application No. 10-2006-28243).

비교예 1 : 인산마그네슘암모늄 수용액이 첨가되지 않은 난연제 조성물의 제조 Comparative Example 1 Preparation of Flame Retardant Composition Without Magnesium Ammonium Phosphate Aqueous Solution

실시예 1에서 인산마그네슘암모늄 수용액을 첨가하지 않았고, 나머지 조건은 실시예 1과 동일하게 하여 난연제 조성물을 제조하였다.An aqueous magnesium ammonium phosphate solution was not added in Example 1, and the remaining conditions were the same as in Example 1 to prepare a flame retardant composition.

비교예 2 : 콩기름 등이 첨가되지 않은 난연제 조성물의 제조 Comparative Example 2: Preparation of Flame Retardant Composition Without Soybean Oil

실시예 1에서 콩기름, 베이킹파우더, 유화제, 및 올레인산을 첨가하지 않았고, 나머지 조건은 실시예 1과 동일하게 하여 난연제 조성물을 제조하였다.Soybean oil, baking powder, emulsifier, and oleic acid were not added in Example 1, and the remaining conditions were the same as in Example 1 to prepare a flame retardant composition.

콩기름, 베이킹파우더, 유화제, 및 올레인산이 미첨가된 난연제 조성물을 가지고 목재, 무늬목MDF, 무늬목우레탄코팅MDF, PVC필름MDF의 표면을 도포하는 경우 도포된 표면이 장시간 건조되지 않고 끈적끈적한 성분이 잔류하게 되는 현상이 발생하였다. 콩기름, 베이킹파우더, 유화제, 및 올레인산이 미첨가되는 경우 난연제 조성물의 내수성, 부착성, 및 건조성이 결여되어 인산이 끈적끈적한 상태로 존재하기 때문이라고 사료된다.When applying the surface of wood, veneer MDF, veneer urethane coating MDF, PVC film MDF with soybean oil, baking powder, emulsifier, and oleic acid-free flame retardant composition, the coated surface does not dry for a long time and sticky components remain. Has occurred. If soybean oil, baking powder, emulsifier, and oleic acid are not added, it is considered that phosphoric acid is in sticky state due to lack of water resistance, adhesion, and dryness of the flame retardant composition.

실험예 : 수용성 난연제 조성물의 난연성 평가 실험 Experimental Example: Flame retardancy evaluation experiment of the water-soluble flame retardant composition

실시예 1 및 비교예 2에서 제조한 난연제 조성물을 가지고 "한국소방검정공사"에서 제공하는 "합판 목재용 난연제의 형식승인 및 검정기술기준"에 따라서 난연성 실험을 실시하였다. 난연제 조성물 수용액을 목재, 무늬목MDF, 무늬목우레탄코팅MDF, PVC필름MDF, 종이벽지, 및 실크벽지에 분무기를 이용하여 각각 3회에 걸쳐 분무하여 드라이오븐에 각 도포 회마다 60℃에서 1시간씩 건조하였다.With the flame retardant composition prepared in Example 1 and Comparative Example 2, a flame retardancy test was carried out according to the "type approval and certification standard of the flame retardant for plywood wood" provided by "Korea Fire Protection Corporation." Spray the flame-retardant composition aqueous solution three times each using wood, veneer MDF, veneer urethane coating MDF, PVC film MDF, paper wallpaper, and silk wallpaper with a sprayer and dry them in a dry oven for 1 hour at 60 ℃ for each application. It was.

시료의 크기는 가로 29cm, 세로 19cm로 절단된 시편을 45℃온도의 마이크로 버너법에 근거한 실험장치인 연소시험기(극동방염사, 한국)에 넣고 실험하였다.The specimens were placed in a combustion tester (Far Eastern Bangsa, Korea), which was a test apparatus based on a micro-burner method at a temperature of 45 ° C.

난연성능기준은 잔염시간 10초이내, 잔신시간 30초이내, 탄화면적 50cm2 이 내, 탄화길이 20cm이내이어야 한다. 잔염시간은 버너의 불꽃을 제거한 때부터 불꽃을 올리며 연소하는 상태가 그칠 때까지의 시간이며, 잔신시간은 버너의 불꽃을 제거한 때부터 불꽃을 올리지 아니하고 연소하는 상태가 그칠 때까지의 시간을 의미한다.Flame retardant performance criteria should be within 10 seconds of residual flame time, within 30 seconds of residual time, within 50cm 2 of carbon screen area and within 20cm of carbonization length. Afterflame time means the time from burning of the burner to the state of burning up the flame, and the remaining time means the time from burning of the burner to the state of burning without raising the flame. .

실험예 1 : 목재의 난연성 실험 Experimental Example 1: Flame retardancy test of wood

목재의 난연성 실험결과는 표 1과 도 2 및 도 3에 나타내었다. 본 발명에 따른 난연제 조성물을 도포한 목재의 경우 잔염시간과 잔신시간이 0초이었으며, 탄화길이는 7cm, 탄화면적은 26.97cm2 로 아주 양호하였다. 반면, 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 목재의 경우 탄화길이는 17㎝로 10㎝의 차이가 났으며, 탄화면적도 52㎠로 2배가량의 차이가 났다.The flame retardancy test results of wood are shown in Table 1 and FIGS. 2 and 3. In the wood coated with the flame retardant composition according to the present invention, the residual flame time and residual time were 0 seconds, and the carbonization length was 7 cm and the carbon screen area was 26.97 cm 2 . On the other hand, in the case of wood coated with the flame retardant composition without the addition of aqueous solution of magnesium ammonium phosphate, the carbonization length was 17 cm to 10 cm, and the surface area was 52 cm 2, which was about 2 times the difference.

구분division 기준치Reference value 실시예 1Example 1 비교예 1Comparative Example 1 잔염시간Afterglow time 10초이내Within 10 seconds 00 00 잔신시간Remaining time 30초 이내Within 30 seconds 00 00 탄화길이Carbonization length 20cm 이내Within 20cm 7cm7 cm 17cm17 cm 탄화면적Ammunition 50cm2 이내Within 50cm 2 26.97cm2 26.97 cm 2 52cm2 52 cm 2

실험예 2 : 무늬목MDF의 난연성 실험Experimental Example 2: Flame retardancy test of veneer MDF

무늬목MDF의 난연성 실험결과는 표 2와 도 4 및 도 5에 나타내었다. 본 발명에 따른 난연성 조성물을 도포한 무늬목MDF의 경우 잔염시간과 잔신시간이 0초이었으며, 탄화길이는 9.2cm, 탄화면적은 33.5cm2 로 아주 양호하였다. 반면, 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 무늬목MDF의 경우 탄화길이는 18㎝로 2배가량의 차이가 났으며, 탄화면적도 54㎠로 1.6배가량의 차이가 났다.The flame retardant test results of veneer MDF are shown in Table 2 and FIGS. 4 and 5. In the case of veneer MDF coated with the flame retardant composition according to the present invention, the residual flame time and residual time were 0 seconds, and the carbonization length was 9.2 cm and the carbon screen area was 33.5 cm 2 . On the other hand, in the case of the veneer MDF coated with the flame retardant composition without the addition of aqueous solution of magnesium ammonium phosphate, the carbonization length was 18 cm, which was about 2 times the difference, and the carbon screen area was 54 cm 2, which was 1.6 times the difference.

구분division 기준치Reference value 실시예 1Example 1 비교예 1Comparative Example 1 잔염시간Afterglow time 10초이내Within 10 seconds 00 00 잔신시간Remaining time 30초 이내Within 30 seconds 00 00 탄화길이Carbonization length 20cm 이내Within 20cm 9.2cm9.2 cm 18cm18 cm 탄화면적Ammunition 50cm2 이내Within 50cm 2 33.5cm2 33.5cm 2 54cm2 54 cm 2

실험예 3 : 무늬목우레탄코팅MDF의 난연성 실험Experimental Example 3: Flame retardancy test of veneer urethane coated MDF

무늬목우레탄코팅MDF의 난연성 실험결과는 표 3과 도 6 및 도 7에 나타내었다. 본 발명에 따른 난연성 조성물을 도포한 무늬목우레탄코팅MDF의 경우 잔염시간과 잔신시간이 0초이었으며, 탄화길이는 8.9cm, 탄화면적은 30.16cm2 로 아주 양호하였다. 반면, 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 무늬목우레탄코팅MDF의 경우 탄화길이는 22㎝로 2.4배가량의 차이가 났으며, 탄화면적도 60.2㎠로 2배가량의 차이가 났다.The flame retardant test results of the veneer urethane coated MDF are shown in Table 3 and FIGS. 6 and 7. In the case of the pattern wood urethane coated MDF coated with the flame-retardant composition according to the present invention, the residual flame time and residual time were 0 seconds, and the carbonization length was 8.9 cm and the screen area was 30.16 cm 2 . On the other hand, in the case of patterned urethane coated MDF coated with a flame retardant composition without the addition of aqueous solution of magnesium ammonium phosphate, the carbonization length was 22 cm to 2.4 times, and the carbon screen area was 60.2 cm 2 to about 2 times.

구분division 기준치Reference value 실시예 1Example 1 비교예 1Comparative Example 1 잔염시간Afterglow time 10초이내Within 10 seconds 00 00 잔신시간Remaining time 30초 이내Within 30 seconds 00 00 탄화길이Carbonization length 20cm 이내Within 20cm 8.9cm8.9 cm 22cm22 cm 탄화면적Ammunition 50cm2 이내Within 50cm 2 30.16cm2 30.16 cm 2 60.2cm2 60.2 cm 2

실험예 4 : PVC필름MDF의 난연성 실험Experimental Example 4: Flame retardancy test of PVC film MDF

PVC필름MDF의 난연성 실험결과는 표 4와 도 8 및 도 9에 나타내었다. 본 발명에 따른 난연성 조성물을 도포한 무늬목우레탄코팅MDF의 경우 잔염시간과 잔신시간이 0초이었으며, 탄화길이는 7.2cm, 탄화면적은 26.46cm2 로 아주 양호하였다. 반면, 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 PVC필름MDF의 경우 탄화길이는 22㎝로 3배가량의 차이가 났으며, 탄화면적도 51.3㎠로 2배가량의 차이가 났다.Flame retardant test results of the PVC film MDF are shown in Table 4 and FIG. 8 and FIG. 9. In the case of the pattern wood urethane coated MDF coated with the flame retardant composition according to the present invention, the residual flame time and residual time were 0 seconds, and the carbonization length was 7.2 cm and the carbon screen area was 26.46 cm 2 . On the other hand, in the case of PVC film MDF coated with the flame retardant composition without the addition of aqueous solution of magnesium ammonium phosphate, the carbonization length was 22 cm, which was about 3 times different, and the carbon screen area was 51.3 cm 2, which was about 2 times the difference.

구분division 기준치Reference value 실시예 1Example 1 비교예 1Comparative Example 1 잔염시간Afterglow time 10초이내Within 10 seconds 00 00 잔신시간Remaining time 30초 이내Within 30 seconds 00 00 탄화길이Carbonization length 20cm 이내Within 20cm 7.2cm7.2 cm 22cm22 cm 탄화면적Ammunition 50cm2 이내Within 50cm 2 26.46cm2 26.46 cm 2 51.3cm2 51.3 cm 2

실험예 5 : 종이벽지의 난연성 실험Experimental Example 5: Flame retardancy test of paper wallpaper

종이벽지의 난연성 실험결과는 표 5에 나타내었다. 본 발명에 따른 난연성 조성물을 도포한 종이벽지의 경우 잔염시간과 잔신시간이 0초이었으며, 탄화길이는 6.4cm, 탄화면적은 20.4cm2 로 아주 양호하였다. 반면, 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 종이벽지의 경우 탄화길이는 28㎝로 4.3배가량의 차이가 났으며, 탄화면적도 52㎠로 2.5배가량의 차이가 났다.The flame retardant test results of paper wallpaper are shown in Table 5. In the case of paper wallpaper coated with the flame-retardant composition according to the present invention, the residual flame time and residual time were 0 seconds, and the carbonization length was 6.4 cm and the carbon screen area was 20.4 cm 2 . On the other hand, in the case of paper wallpaper coated with the flame retardant composition without the addition of aqueous solution of magnesium ammonium phosphate, the carbonization length was 28 cm, which was about 4.3 times, and the carbon screen area was 52 cm 2, which was 2.5 times the difference.

구분division 기준치Reference value 실시예 1Example 1 비교예 1Comparative Example 1 잔염시간Afterglow time 10초이내Within 10 seconds 00 00 잔신시간Remaining time 30초 이내Within 30 seconds 00 00 탄화길이Carbonization length 20cm 이내Within 20cm 6.4cm6.4 cm 28cm28 cm 탄화면적Ammunition 50cm2 이내Within 50cm 2 20.4cm2 20.4 cm 2 52cm2 52 cm 2

실험예 6 : 실크벽지의 난연성 실험Experimental Example 6: Flame retardancy test of silk wallpaper

실크벽지의 난연성 실험결과는 표 6에 나타내었다. 본 발명에 따른 난연성 조성물을 도포한 실크벽지의 경우 잔염시간과 잔신시간이 0초이었으며, 탄화길이는 6.5cm, 탄화면적은 28cm2 로 아주 양호하였다. 반면, 인산마그네슘암모늄 수용액을 첨가하지 않은 난연제 조성물을 도포한 실크벽지의 경우 탄화길이는 21㎝로 3배가량의 차이가 났으며, 탄화면적도 38㎠로 1.3배가량의 차이가 났다.The flame retardancy test results of silk wallpaper are shown in Table 6. In the case of the silk wallpaper coated with the flame-retardant composition according to the present invention, the residual flame time and residual time were 0 seconds, and the carbonization length was 6.5 cm and the carbon screen area was 28 cm 2 . On the other hand, in the case of the silk wallpaper coated with the flame retardant composition without the addition of aqueous solution of magnesium ammonium phosphate, the carbonization length was 21 cm, which was about 3 times different, and the surface area was 38 cm 2, which was 1.3 times the difference.

구분division 기준치Reference value 실시예 1Example 1 비교예 1Comparative Example 1 잔염시간Afterglow time 10초이내Within 10 seconds 00 00 잔신시간Remaining time 30초 이내Within 30 seconds 00 00 탄화길이Carbonization length 20cm 이내Within 20cm 6.4cm6.4 cm 28cm28 cm 탄화면적Ammunition 50cm2 이내Within 50cm 2 20.4cm2 20.4 cm 2 52cm2 52 cm 2

상술한 바와 같이, 본 발명에 따른 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물은 난연성, 내수성, 내열성 및 내마모성이 우수한 장점이 있다.As described above, the titanium magnesium ammonium phosphate-bentonite-based flame retardant composition according to the present invention has an advantage of excellent flame retardancy, water resistance, heat resistance, and wear resistance.

또한, 단일 약품 한가지로, 즉 단일 난연제 조성물을 이용하여 목재, 무늬목MDF, 무늬목우레탄코팅MDF, 또는 PVC필름MDF 등의 여러종류의 건축자재를 난연 처리함으로써, 연기 및 유독가스의 발생을 감소시키고 연소확산을 막아 인명과 재산의 피해를 줄일 수 있다.In addition, one flame retardant treatment of various types of building materials, such as wood, veneer MDF, veneer urethane coated MDF, or PVC film MDF, using a single flame retardant composition, reduces the occurrence of smoke and toxic gases and burns. It can prevent the spread and reduce the damage of life and property.

또한, 국내 난연제 업계의 대외 의존도가 심각하여 90%가량을 해외로부터 수 입하고 있는 실정을 감안하여 볼때, 본 발명에 따른 난연제 조성물은 수입대체효과가 클 것으로 기대된다.In addition, in view of the fact that the domestic flame retardant industry is heavily dependent on the foreign countries imported about 90% from abroad, the flame retardant composition according to the present invention is expected to have a large import substitution effect.

Claims (11)

인산티탄마그네슘 수용액 5~13 중량%, 벤토나이트 0.1~1.0 중량%, 콩기름 0.01~0.5 중량%, 베이킹파우더 0.01~0.5 중량%, 유화제 0.1~1.0 중량%, 올레인산 0.01~0.5 중량%, 디메틸아민을 포함한 염기 1~5 중량%, 및 인산마그네슘암모늄 수용액 85~93 중량%로 이루어지는 것을 특징으로 하는 난연제 조성물.Titanium Magnesium Phosphate Solution 5 ~ 13% by weight, Bentonite 0.1 ~ 1.0% by weight, Soybean oil 0.01 ~ 0.5% by weight, Baking powder 0.01 ~ 0.5% by weight, Emulsifier 0.1 ~ 1.0% by weight, Oleic acid 0.01 ~ 0.5% by weight, including dimethylamine A flame retardant composition comprising 1 to 5% by weight of a base, and 85 to 93% by weight of an aqueous solution of magnesium ammonium phosphate. a) 인산 수용액에 상기 인산 중량 대비 26~32 중량%의 티탄을 첨가하고 교반, 가열시켜 인산티탄{Ti2(PO4)3} 수용액을 제조하는 단계;a) adding 26 to 32% by weight of titanium to the aqueous solution of phosphoric acid, stirring and heating to prepare an aqueous solution of titanium phosphate {Ti 2 (PO 4 ) 3 }; b) 상기 인산티탄 수용액에 벤토나이트 및 수산화마그네슘을 첨가하고 교반, 가열하여 인산티탄마그네슘 수용액과 벤토나이트의 혼합물을 제조하는 단계;b) adding bentonite and magnesium hydroxide to the aqueous solution of titanium phosphate, stirring and heating to prepare a mixture of aqueous solution of titanium magnesium phosphate and bentonite; c) 상기 인산티탄마그네슘 수용액과 벤토나이트의 혼합물에 콩기름, 베이킹파우더, 유화제, 및 올레인산을 첨가하는 단계;c) adding soybean oil, a baking powder, an emulsifier, and oleic acid to the mixture of aqueous magnesium magnesium phosphate solution and bentonite; d) 디메틸아민을 포함한 염기를 이용하여 상기 c) 단계 후의 인산티탄마그네슘 수용액과 벤토나이트의 혼합물의 pH를 5~6으로 조정하는 단계;d) adjusting the pH of the mixture of aqueous magnesium magnesium phosphate solution and bentonite after step c) to 5-6 using a base containing dimethylamine; e) 상기 d) 단계 후의 인산티탄마그네슘 수용액과 벤토나이트의 혼합물에 인산마그네슘암모늄 수용액을 첨가하고 혼합시키는 단계; 및e) adding and mixing an aqueous magnesium ammonium phosphate solution to the mixture of aqueous magnesium magnesium phosphate solution and bentonite after step d); And f) 상기 e) 단계 후의 혼합물을 여과하여 미용해된 찌꺼기를 걸러주는 단 계;를 포함하는 것을 특징으로 하는 인산티탄마그네슘암모늄 -벤토나이트계 난연제 조성물의 제조방법.f) filtering the mixture after step e) to filter out undissolved debris; titanium magnesium ammonium phosphate-bentonite-based flame retardant composition, comprising: a. 제 2항에 있어서,The method of claim 2, 상기 a) 단계의 인산티탄{Ti2(PO4)3} 수용액은 인산 농도가 15~25 중량%인 것을 특징으로 하는 난연제 조성물의 제조방법.The titanium phosphate {Ti 2 (PO 4 ) 3 } aqueous solution of step a) is a method of producing a flame retardant composition, characterized in that the phosphoric acid concentration is 15 to 25% by weight. 제 3항에 있어서, 상기 a) 단계의 교반 및 가열은 70~90℃에서 2~4시간 동안 교반, 가열시키는 것을 특징으로 하는 난연제 조성물의 제조방법.The method of claim 3, wherein the stirring and heating of step a) are performed by stirring and heating at 70 to 90 ° C. for 2 to 4 hours. 제 4항에 있어서,The method of claim 4, wherein 상기 b) 단계의 벤토나이트 첨가량 및 수산화마그네슘 첨가량은 상기 a) 단계의 인산티탄 수용액 중량 대비 2~4 중량% 및 0.1~0.5 중량%인 것을 특징으로 하는 난연제 조성물의 제조방법.The amount of bentonite added and the amount of magnesium hydroxide added in the step b) are 2 to 4% by weight and 0.1 to 0.5% by weight based on the weight of the titanium phosphate aqueous solution of step a). 제 4항에 있어서,The method of claim 4, wherein 상기 c) 단계의 콩기름, 베이킹파우더, 유화제, 및 올레인산의 첨가량은 상기 a) 단계의 인산티탄 수용액 중량 대비 1~2 중량%, 0.4~1.2 중량%, 2~3 중량%, 및 0.4~0.8 중량%인 것을 특징으로 하는 난연제 조성물의 제조방법.The amount of the soybean oil, the baking powder, the emulsifier, and the oleic acid added in step c) may be 1 to 2% by weight, 0.4 to 1.2% by weight, 2 to 3% by weight, and 0.4 to 0.8% by weight based on the titanium phosphate aqueous solution in step a). Method for producing a flame retardant composition, characterized in that%. 제 2항 내지 제 6항 중 어느 한 항에 있어서,The method according to any one of claims 2 to 6, 상기 e) 단계의 인산티탄마그네슘 수용액과 벤토나이트의 혼합물의 양은 상기 인산마그네슘암모늄 수용액의 중량 대비 10~15 중량%인 것을 특징으로 하는 난연제 조성물의 제조방법.The amount of the mixture of the magnesium magnesium phosphate solution and bentonite in step e) is 10 to 15% by weight based on the weight of the aqueous magnesium ammonium phosphate solution. a) 인산 수용액에 상기 인산 중량 대비 26~32 중량%의 티탄을 첨가하고 교반, 가열시켜 인산티탄{Ti2(PO4)3} 수용액을 제조하는 단계;a) adding 26 to 32% by weight of titanium to the aqueous solution of phosphoric acid, stirring and heating to prepare an aqueous solution of titanium phosphate {Ti 2 (PO 4 ) 3 }; b) 상기 인산티탄 수용액에 벤토나이트, 수산화마그네슘, 콩기름, 베이킹파우더, 유화제, 올레인산, 인산마그네슘암모늄용액을 첨가하고, 교반, 가열시킨 후 디메틸아민을 포함한 염기를 이용하여 혼합물의 pH를 5~6으로 조정하는 단계; 및b) Bentonite, magnesium hydroxide, soybean oil, baking powder, emulsifier, oleic acid, magnesium ammonium phosphate solution are added to the aqueous titanium phosphate solution, stirred and heated, and then the pH of the mixture is adjusted to 5-6 using a base containing dimethylamine. Adjusting; And c) 상기 b) 단계 후의 혼합물을 여과하여 미용해된 찌꺼기를 걸러주는 단계;를 포함하는 것을 특징으로 하는 인산티탄마그네슘암모늄 -벤토나이트계 난연제 조성물의 제조방법.c) filtering the mixture after step b) to filter out undissolved debris; titanium magnesium ammonium phosphate-bentonite-based flame retardant composition comprising a. 제 7항의 제조방법에 의해 제조되는 인산티탄마그네슘암모늄-벤토나이트계 난연제 조성물을 건축자재 또는 마감재에 도포하는 단계 및 상기 도포된 난연제 조성물을 건조하는 단계;를 포함하는 난연 처리 방법.A flame retardant treatment method comprising: applying a titanium magnesium ammonium phosphate-bentonite-based flame retardant composition prepared by the method of claim 7 to a building material or a finishing material, and drying the applied flame retardant composition. 제 9항에 있어서,The method of claim 9, 상기 건축자재는 목재, 무늬목MDF(합판), 무늬목우레탄코팅MDF(합판), 또는 PVC필름MDF(합판)인 것을 특징으로 하는 난연 처리 방법.The building material is wood, veneer MDF (plywood), veneer urethane coating MDF (plywood), PVC film MDF (plywood) characterized in that the flame retardant treatment method. 제 9항에 있어서,The method of claim 9, 상기 마감재는 종이벽지 및 실크벽지를 포함하는 벽지류인 것을 특징으로 하는 난연 처리 방법.The finishing material is a flame retardant treatment method, characterized in that the wallpaper including paper wallpaper and silk wallpaper.
KR1020070028302A 2007-03-22 2007-03-22 Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same KR100865176B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020070028302A KR100865176B1 (en) 2007-03-22 2007-03-22 Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020070028302A KR100865176B1 (en) 2007-03-22 2007-03-22 Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same

Publications (2)

Publication Number Publication Date
KR20080086294A KR20080086294A (en) 2008-09-25
KR100865176B1 true KR100865176B1 (en) 2008-10-24

Family

ID=40025687

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020070028302A KR100865176B1 (en) 2007-03-22 2007-03-22 Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same

Country Status (1)

Country Link
KR (1) KR100865176B1 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20160098101A (en) 2016-04-07 2016-08-18 (주)신영목재 Method of controlling infiltration pressure of water-soluble fire-retardant liquid in wood impregnation
KR20160098021A (en) 2015-12-11 2016-08-18 (주)신영목재 Method for controlling infiltration pressure of water-soluble fire-retardant liquid in wood impregnation
KR20160098100A (en) 2016-03-30 2016-08-18 (주)신영목재 Method for controlling infiltration pressure of water-soluble fire-retardant liquid in wood impregnation
KR20200070669A (en) 2018-12-10 2020-06-18 럭키목재 주식회사 Water soluble flame retardant composition for wood and Flame retardant wood

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990021573A (en) * 1997-08-30 1999-03-25 성재갑 Non-halogen flame retardant styrene resin composition
JP2002322374A (en) 2001-04-27 2002-11-08 Kanegafuchi Chem Ind Co Ltd Foamable fire-retardant composition excellent in fire resistance
JP2004010407A (en) 2002-06-05 2004-01-15 Jfe Engineering Kk Method of producing ammonium magnesium phosphate monohydrate
JP2004075811A (en) 2002-08-14 2004-03-11 Furukawa Electric Co Ltd:The Acidproof flame-retardant resin composition and insulated electric wire
KR20050090833A (en) * 2004-03-10 2005-09-14 김두환 Incombustible coating material for styrofoom and the method thereof
KR20050118113A (en) * 2005-04-28 2005-12-15 한우섭 The flameproof composition of adiabatic material and its manufacturing method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990021573A (en) * 1997-08-30 1999-03-25 성재갑 Non-halogen flame retardant styrene resin composition
JP2002322374A (en) 2001-04-27 2002-11-08 Kanegafuchi Chem Ind Co Ltd Foamable fire-retardant composition excellent in fire resistance
JP2004010407A (en) 2002-06-05 2004-01-15 Jfe Engineering Kk Method of producing ammonium magnesium phosphate monohydrate
JP2004075811A (en) 2002-08-14 2004-03-11 Furukawa Electric Co Ltd:The Acidproof flame-retardant resin composition and insulated electric wire
KR20050090833A (en) * 2004-03-10 2005-09-14 김두환 Incombustible coating material for styrofoom and the method thereof
KR20050118113A (en) * 2005-04-28 2005-12-15 한우섭 The flameproof composition of adiabatic material and its manufacturing method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20160098021A (en) 2015-12-11 2016-08-18 (주)신영목재 Method for controlling infiltration pressure of water-soluble fire-retardant liquid in wood impregnation
KR20160098100A (en) 2016-03-30 2016-08-18 (주)신영목재 Method for controlling infiltration pressure of water-soluble fire-retardant liquid in wood impregnation
KR20160098101A (en) 2016-04-07 2016-08-18 (주)신영목재 Method of controlling infiltration pressure of water-soluble fire-retardant liquid in wood impregnation
KR20200070669A (en) 2018-12-10 2020-06-18 럭키목재 주식회사 Water soluble flame retardant composition for wood and Flame retardant wood

Also Published As

Publication number Publication date
KR20080086294A (en) 2008-09-25

Similar Documents

Publication Publication Date Title
KR101192453B1 (en) Flame retardant composition soluble in water
CN101880408B (en) Flame retardant and preparation method thereof
KR100865176B1 (en) Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same
CN104774509A (en) Fireproof paint
DK149819B (en) EFFECTIVE, FIRE-RESISTANT COATING MASS CONTAINING AMMONIUM POLYPHOSPHATE
KR100893948B1 (en) Flame retardant composition soluble in water, method for preparing the same, and flameproof process using the same
CN111607219B (en) Low-smoke thermoplastic polyurethane elastomer composite material and preparation method thereof
RU2204547C2 (en) Intumescent coke-forming fire retardant, method of preparation thereof, method of fire-protective treatment of combustible substance, and a method for extinguishing heat source
KR101834824B1 (en) A method for preparing water-soluble fire-retardant liquid
KR100751566B1 (en) Preparing method of flame retardant composition comprising ammonium magnesium phosphate and flameproof process using the same
JP2005161588A (en) Flame retardant woody material and its manufacturing method
KR20050052333A (en) Composition for action of resist-fire and fire-extinguishing
CN114232350A (en) Phosphorus-nitrogen synergistic aqueous flame-retardant coating composition containing tubular kaolin, preparation method and prepared flame-retardant fabric
US3915931A (en) Organic polymer flame retardants based on sulfamide
EP1476510B1 (en) Fireproofing agent
KR20080000550A (en) Aqueous flame-retarding materials composition and its production methods
JP3320553B2 (en) Powder extinguishing agent
JPS6241033B2 (en)
JP2003020596A (en) Flame retardant and method for imparting flame- retardancy to textile product
CN111364282B (en) Halogen-free inorganic flame-retardant material and preparation method and application thereof
Strekalova et al. Cellulose materials with reduced fire hazard
KR102254316B1 (en) Water soluble flame retardant composition for wood and Flame retardant wood
JP2006082227A (en) Manufacturing method of flame-retardant and non-combustible wood for imparting digestion capacity to wood itself by impregnating wood with injection agent applying no load to environment in realizing flame-retardance and non-combustibility of wood
Arinze et al. Reducing the flammability of Gmelina arborea wood using flame retardants
KR20010110512A (en) Fire retardant

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E701 Decision to grant or registration of patent right
GRNT Written decision to grant
FPAY Annual fee payment

Payment date: 20121017

Year of fee payment: 5

FPAY Annual fee payment

Payment date: 20131231

Year of fee payment: 6

FPAY Annual fee payment

Payment date: 20141017

Year of fee payment: 7

FPAY Annual fee payment

Payment date: 20151016

Year of fee payment: 8

FPAY Annual fee payment

Payment date: 20161007

Year of fee payment: 9

FPAY Annual fee payment

Payment date: 20171017

Year of fee payment: 10

FPAY Annual fee payment

Payment date: 20181018

Year of fee payment: 11

FPAY Annual fee payment

Payment date: 20191015

Year of fee payment: 12