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KR20210158504A - FRP flame retardant additive - Google Patents

FRP flame retardant additive Download PDF

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Publication number
KR20210158504A
KR20210158504A KR1020200076892A KR20200076892A KR20210158504A KR 20210158504 A KR20210158504 A KR 20210158504A KR 1020200076892 A KR1020200076892 A KR 1020200076892A KR 20200076892 A KR20200076892 A KR 20200076892A KR 20210158504 A KR20210158504 A KR 20210158504A
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South Korea
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water glass
weight
resin
vinyl ester
curing
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KR1020200076892A
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Korean (ko)
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공석태
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공석태
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Priority to KR1020200076892A priority Critical patent/KR20210158504A/en
Priority to PCT/KR2021/007889 priority patent/WO2021261912A1/en
Publication of KR20210158504A publication Critical patent/KR20210158504A/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/40—Glass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L31/00—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 acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers
    • C08L31/02—Homopolymers or copolymers of esters of monocarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/06—Unsaturated polyesters

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Macromonomer-Based Addition Polymer (AREA)

Abstract

Composite materials are generally called FRP and are manufactured by combining fibers and resins, and fibers are generally made of glass, but various materials such as carbon are used as needed. If a resin is acid or corrosion resistant, a vinyl ester resin is used, and in general, inexpensive unsaturated ester resins are used, but vinyl ester resins and unsaturated ester resins burn easily, and toxic gas is generated when burning, and there is a problem in that people drink poisonous gas and suffocate in a short time by the gas, rather than being burned to death in the case of a fire. The resin for making FRP is a thermosetting resin, which is generally used as a two-component type, and is used by mixing 0.3 to 1% of a curing agent with the vinyl ester resin and an unsaturated ester resin, and adding an accelerator or a retarder as necessary. After the curing agent is added, UV light or heat is applied to induce a curing reaction, so that a novel polymer is formed by reacting 30 to 70% of water in the water glass component with vinyl ester or unsaturated polyester.

Description

FRP 난연첨가제{FRP flame retardant additive}FRP flame retardant additive

비닐에스테르,불포화 폴리에스터,난연제,물유리,규산나트륨(Na2SiO3)Vinyl ester, unsaturated polyester, flame retardant, water glass, sodium silicate (Na2SiO3)

복합소재를 일반적으로 FRP라 부르며 섬유와 수지를 결합해 제작하며 섬유는 일반적으로 유리로 된것을 사용하나 필요에 따라 카본등 다양한 소재를 이용한다Composite materials are generally called FRP and are manufactured by combining fibers and resins. Fibers are generally made of glass, but various materials such as carbon are used as needed.

수지는 내산,내식 일 경우 비닐에스테르 수지를 사용하며 일반적으로는 저가의 불포화 에스테르 수지를 사용하는데 비닐에스테르 수지와 불포화 에스테르 수지는 불에 잘타며 불에 탈때 유독성 개스가 발생되어 화재시 사람이 불에 타죽는것이 아니라 유독성가스를 마시고 가스에 의해 짧은시간에 질식사하는 문제가 있다In case of acid and corrosion resistance, vinyl ester resin is used. In general, low-cost unsaturated ester resin is used. Vinyl ester resin and unsaturated ester resin are easily flammable, and toxic gas is generated when burning. There is a problem of suffocation in a short time by drinking poisonous gas rather than burning to death.

비닐에스테르 수지와 불포화 에스테르 수지는 불에 잘타며 불에 탈때 유독성 개스가 발생되어 화재시 사람이 불에 타죽는것이 아니라 유독성가스를 마시고 가스에 의해 짧은시간에 질식사하는 문제가 있으나 기존 비닐에스테르 수지와 불포화 에스테르 수지를 난연화시켜야 되는데 기존 인계난연제,할로겐족 난연제는 가격이 비싸 적용시 가격이 고가가 되어 산업현장에서 적용하기 어려운데 물유리는 가격이싼데 물성분을 포함하고 있다 보니 기존 상온경화제(MEKPO) 상황에서는 물유리를 첨가하는 시도할 생각조차 할수 없었다.Vinyl ester resin and unsaturated ester resin burn easily, and toxic gas is generated when burned. Unsaturated ester resins need to be flame-retardant, but existing phosphorus-based flame retardants and halogen-based flame retardants are expensive and difficult to apply in industrial fields because they are expensive. In Esau couldn't even think of adding a glass of water.

본인이 얼음을 몰드로 삼아 불포화 폴리에스테르에 TPO를 혼합후 UV빛을 조사하여 경화시킨 실험 경험이 있어 불포화 폴리에스테르에 물유리를 혼합후 UV빛을 조사하면 경화가 가능할것이라는 추론을 하였고 이에따라 불포화폴리에스테르에 물유리를 혼합하여 저렴한 난연성 폴리머 소재를 만들고자한다I used ice as a mold, mixed TPO with unsaturated polyester, and then irradiated with UV light to cure it, so I deduced that curing would be possible by mixing water glass with unsaturated polyester and irradiating UV light. We want to make an inexpensive flame-retardant polymer material by mixing water glass with

우선 첨가제에 대한 기본설명을 하면 액체로 된 유리 또는 물에 녹는(녹은) 유리. 대표적 규산염인 규산나트륨(Na2SiO3)의 수용액. 또는 하얀 고체 가루인 규산나트륨 자체를 물유리라고 부르기도 하며 여기서는 물유리로 설명하도록 한다.First of all, if you give a basic explanation about additives, it is liquid glass or water-soluble (melted) glass. Aqueous solution of sodium silicate (Na2SiO3), a representative silicate. Alternatively, sodium silicate itself, a white solid powder, is sometimes called water glass, and it will be described as water glass here.

FRP를 만드는 수지는 열경화성 수지로서 일반적으로 2액형으로 사용되며 비닐에스테르 수지와 불포화 에스테르 수지에 경화제를 0.3~1% 혼합하여 사용하며 필요에따라 촉진제나 지연제를 첨가하여 사용된다 The resin for making FRP is a thermosetting resin, which is generally used as a two-component type. It is used by mixing 0.3 to 1% of a curing agent with vinyl ester resin and unsaturated ester resin, and adding accelerators or retarders as needed.

경화를 촉진하거나, 가열경화반응을 상온경화반응으로 바꾸는 약제를 경화촉진제라고 한다. 불포화 폴리에스터 경화에 유기과산화물과 같이 사용하는 3급 아민 등이 대표적인 예이다. 경화제에는 이 밖에 미가황(未加黃) 고무에 배합하여 흐름을 방지하기 위한 배합제(配合劑)나 분자를 다리결합시키기 위한 다리결합제, 시멘트·석고에 첨가하여 경화를 촉진하는 경화촉진제 등이 있다.An agent that accelerates curing or converts a heat curing reaction into a room temperature curing reaction is called a curing accelerator. A typical example is a tertiary amine used together with an organic peroxide to cure unsaturated polyester. In addition to hardening agents, there are compounding agents to prevent flow by mixing with unvulcanized rubber, crosslinking agents for bridging molecules, hardening accelerators added to cement and gypsum to accelerate hardening, etc. have.

경화제는 알콜성분이 주종이므로 휘발되므로 농도가 낮아지고 물이 생겨 선입선출이 요망된다. 저장은 냉암소에 보관하고 직사광선이나 열이 있는곳은 절대 금물이며 사용하는 용기는 스텐레스,PE,유리외에는 피하고 철,동합금된 철재는 절대 않된다. 충격이나 마찰을 주면은 폭발한다. Since alcohol is the main type of curing agent, it volatilizes, so the concentration is lowered and water is generated, so first-in-first-out is desired. Store in a cool and dark place, avoid direct sunlight or heat, and avoid using containers other than stainless steel, PE, and glass, and never use iron or copper alloyed steel. It explodes when subjected to impact or friction.

1.MEKPO-무색액체-상온경화용(일반용) 1.MEKPO-Colorless liquid-For curing at room temperature (for general use)

2.BPO-분말-중온경화제(80-120℃),열경화제2.BPO-powder-medium temperature curing agent (80-120℃), thermosetting agent

3.TPO-분말-광개시제3.TPO-powder-photoinitiator

등이 있으며 본 발명에서는 2번과 3번 항목에 대해서만 적용되며 1번 항목은 비닐에스테르나 불포화폴리에스테르는 물하고는 상극으로 물이 적은 양만 들어가도 경화불량이 일어나는데 물유리에는 물성분이 50~70%함유하고 있어 MEKPO를 경화제로 사용시 경화가 되지 않으며 불포화 폴리에스테르에 광개시제인 TPO를 0.5%혼합후 물유리1호를 30~70%를 혼합후 교반중 1차반응을 보였고 자외선에 노출하면 경화가 일어나는것을 확인하였으며 자외선은 외부반응시에만 적용할수 있어 다시 불포화 폴리에스테르에 BPO분말 0.5%혼합후 물유리1호를 30~70%를 혼합후 교반중 1차반응을 보였고 80℃ 온도위 챔버에 넣고 10분후 꺼내니 경화가 완료되었으며 경화전과 경화후의 질량을 재어보니 질량의 변화가 없었다.In the present invention, it is applied only to items 2 and 3, and item 1 is opposite to water for vinyl ester or unsaturated polyester. When MEKPO is used as a curing agent, curing does not occur, and after mixing 0.5% of TPO, a photoinitiator, with unsaturated polyester, 30~70% of water glass No. 1 is mixed and the primary reaction is shown during stirring. It is confirmed that curing occurs when exposed to ultraviolet rays UV light can be applied only during external reaction, so after mixing 0.5% of BPO powder with unsaturated polyester, 30~70% of water glass No. 1 was mixed and the first reaction was shown during stirring. Put it in a chamber above 80℃ and take it out after 10 minutes Curing was completed, and when the mass before and after curing was measured, there was no change in mass.

질량의 변화가 없다는것은 경화제를 첨가후 uv빛이나 열을가해 경화반을을 유도하면 경화반응에 따라 물유리 성분의 30~70%의 물이 비닐에스테르나 불포화폴리에스테르 와 반응하여 새로운 폴리머가 형성되었다고 본다 The fact that there is no change in mass means that after adding a curing agent, UV light or heat is applied to induce a hardening plate. According to the curing reaction, 30~70% of water in the water glass component reacts with vinyl ester or unsaturated polyester to form a new polymer. see

비닐에스테르 수지와 불포화 에스테르 수지에 물유리(1호기준)를 에스테르 수지 1에 대한 물유리(1호기준) 0.3(무게비)이상 을 혼합하면 자기소화성이 주어지며 물유리(1호기준) 2.5(무게비)까지 혼합하여도 경화에는 지장이 없었고 물유리 혼합비기 많을수록 난연화 정도가 좋았으며 물유리 가격이 기존 인계난연제나 할로겐족 난연제의 10%정도 이하의 가격으로 아주저렴한 상품을 난연상품으로 만드는 효과가 있다.When water glass (based on No. 1) and water glass (based on No. 1) to ester resin 1 are mixed with vinyl ester resin and unsaturated ester resin in an amount of 0.3 (weight ratio) or more, self-extinguishing properties are given and water glass (based on No. 1) 2.5 (weight ratio) There was no problem in curing even when mixed, and the higher the mixing ratio of water glass, the better the degree of flame retardancy.

우선 첨가제에 대한 기본설명을 하면 액체로 된 유리 또는 물에 녹는(녹은) 유리. 대표적 규산염인 규산나트륨(Na2SiO3)의 수용액. 또는 하얀 고체 가루인 규산나트륨 자체를 물유리라고 부르기도 하며 여기서는 물유리로 설명하도록 한다.First of all, if you give a basic explanation about additives, it is liquid glass or water-soluble (melted) glass. Aqueous solution of sodium silicate (Na2SiO3), a representative silicate. Alternatively, sodium silicate itself, a white solid powder, is sometimes called water glass, and will be described as water glass here.

FRP를 만드는 수지는 열경화성 수지로서 일반적으로 2액형으로 사용되며 비닐에스테르 수지와 불포화 에스테르 수지에 경화제를 0.3~1% 혼합하여 사용하며 필요에따라 촉진제나 지연제를 첨가하여 사용된다 The resin for making FRP is a thermosetting resin, which is generally used as a two-component type. It is used by mixing 0.3 to 1% of a curing agent with vinyl ester resin and unsaturated ester resin, and adding accelerators or retarders as needed.

경화를 촉진하거나, 가열경화반응을 상온경화반응으로 바꾸는 약제를 경화촉진제라고 한다. 불포화 폴리에스터 경화에 유기과산화물과 같이 사용하는 3급 아민 등이 대표적인 예이다. 경화제에는 이 밖에 미가황(未加黃) 고무에 배합하여 흐름을 방지하기 위한 배합제(配合劑)나 분자를 다리결합시키기 위한 다리결합제, 시멘트·석고에 첨가하여 경화를 촉진하는 경화촉진제 등이 있다.An agent that accelerates curing or changes a heat curing reaction to a room temperature curing reaction is called a curing accelerator. A typical example is a tertiary amine used together with an organic peroxide to cure unsaturated polyester. In addition to the curing agent, a compounding agent to prevent flow by mixing with unvulcanized rubber, a bridge bonding agent to bridge molecules, and a curing accelerator added to cement and gypsum to accelerate curing. have.

경화제는 알콜성분이 주종이므로 휘발되므로 농도가 낮아지고 물이 생겨 선입선출이 요망된다. 저장은 냉암소에 보관하고 직사광선이나 열이 있는곳은 절대 금물이며 사용하는 용기는 스텐레스,PE,유리외에는 피하고 철,동합금된 철재는 절대 않된다. 충격이나 마찰을 주면은 폭발한다. Since alcohol is the main type of curing agent, it volatilizes, so the concentration is lowered and water is generated, so first-in-first-out is desired. Store in a cool and dark place, avoid direct sunlight or heat, and avoid using containers other than stainless steel, PE, and glass, and never use iron or copper alloyed steel. It explodes when subjected to impact or friction.

1.MEKPO-무색액체-상온경화용(일반용) 1.MEKPO-Colorless liquid-For curing at room temperature (for general use)

2.BPO-분말-중온경화제(80-120℃),열경화제2.BPO-powder-medium temperature curing agent (80-120℃), thermosetting agent

3.TPO-분말-광개시제3.TPO-powder-photoinitiator

등이 있으며 본 발명에서는 2번과 3번 항목에 대해서만 적용되며 1번 항목은 비닐에스테르나 불포화폴리에스테르는 물하고는 상극으로 물이 적은 양만 들어가도 경화불량이 일어나는데 물유리에는 물성분이 50~70%함유하고 있어 MEKPO를 경화제로 사용시 경화가 되지 않으며 불포화 폴리에스테르에 광개시제인 TPO를 0.5%혼합후 물유리1호를 30~70%를 혼합후 교반중 1차반응을 보였고 자외선에 노출하면 경화가 일어나는것을 확인하였으며 자외선은 외부반응시에만 적용할수 있어 다시 불포화 폴리에스테르에 BPO분말 0.5%혼합후 물유리1호를 30~70%를 혼합후 교반중 1차반응을 보였고 80℃ 온도위 챔버에 넣고 10분후 꺼내니 경화가 완료되었으며 경화전과 경화후의 질량을 재어보니 질량의 변화가 없었다.In the present invention, it is applied only to items 2 and 3, and item 1 is opposite to water for vinyl ester or unsaturated polyester. When MEKPO is used as a curing agent, curing does not occur, and after mixing 0.5% of TPO, a photoinitiator, with unsaturated polyester, 30~70% of water glass No. 1 is mixed and the primary reaction is shown during stirring. It is confirmed that curing occurs when exposed to ultraviolet rays UV light can be applied only during external reaction, so after mixing 0.5% of BPO powder with unsaturated polyester, 30~70% of water glass No. 1 was mixed and the first reaction was shown during stirring. Put it in a chamber above 80℃ and take it out after 10 minutes Curing was completed, and when the mass before and after curing was measured, there was no change in mass.

질량의 변화가 없다는것은 경화제를 첨가후 uv빛이나 열을가해 경화반을을 유도하면 경화반응에 따라 물유리 성분의 30~70%의 물이 비닐에스테르나 불포화폴리에스테르 와 반응하여 새로운 폴리머가 형성되었다고 생각되며The fact that there is no change in mass means that after adding a curing agent, UV light or heat is applied to induce a hardening plate. According to the curing reaction, 30~70% of water in the water glass component reacts with vinyl ester or unsaturated polyester to form a new polymer. is thought

또한 물유리 경화제가 아직까지 나오지 않은 상태로 이를 역으로 적용하면In addition, if the water glass curing agent is applied in the reverse state,

불포화폴리에스테르에 TPO또는 BPO을 0.1~1.5% 혼합하여 물유리에 중량비 5~30% 를혼합하여 교반하여 적용처에 적용후 빛이나 열을가해 경화제로 사용할수있다It can be used as a curing agent by mixing 0.1 to 1.5% of TPO or BPO with unsaturated polyester, mixing 5 to 30% by weight in water glass, stirring, and applying light or heat to the application area.

Claims (18)

불포화 폴리에스테르 수지에 있어서
광개시제인 TPO를 0.1%~2.5% 혼합후 물유리1호를 중량비 30~70%를 혼합하는 방법
In the unsaturated polyester resin
A method of mixing 0.1% to 2.5% of TPO, a photoinitiator, and then mixing 30 to 70% of water glass No. 1 by weight
 상기 1항에 있어서 불포화 폴리에스테르 수지를 비닐 에스테르수지 를 적용하는 방법The method according to claim 1, wherein the unsaturated polyester resin is a vinyl ester resin. 상기 1항에 있어서 광개시제인 TPO 대신에 열개시제 인 BPO를 적용하는 방법The method according to claim 1, wherein BPO, which is a thermal initiator, is applied instead of TPO, which is a photoinitiator. 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 0.1~10%를 첨가하는 방법A method of adding 0.1 to 10% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 10~20%를 첨가하는 방법A method of adding 10 to 20% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 20~30%를 첨가하는 방법A method of adding 20 to 30% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 70~100%를 첨가하는 방법A method of adding 70-100% by weight of water glass No. 1 in the water glass addition ratio of item 1 above 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 100~150%를 첨가하는 방법A method of adding 100 to 150% by weight of water glass No. 1 in the water glass addition ratio of item 1 above 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 150~200%를 첨가하는 방법A method of adding 150 to 200% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 200~250%를 첨가하는 방법A method of adding 200 to 250% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 250~300%를 첨가하는 방법A method of adding 250 to 300% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 300~400%를 첨가하는 방법A method of adding 300 to 400% by weight of water glass No. 1 in the above 1 water glass addition ratio 상기 1항 물유리 첨가비율에 있어서 물유리1호를 중량비 400~500%를 첨가하는 방법A method of adding 400 to 500% by weight of water glass No. 1 in the above 1 water glass addition ratio 불포화폴리에스테르에 TPO또는 BPO을 0.1~2.5% 혼합하여 물유리에 대한 중량비 5~30% 를혼합하여 교반하여 적용처에 적용후 빛이나 열을가해 경화제로 적용하는방법A method of mixing 0.1~2.5% of TPO or BPO with unsaturated polyester, mixing 5~30% of the weight with respect to water glass, stirring, applying to the application area, and applying light or heat as a curing agent 상기 14항에 있어서 불포화폴리에스테르를 비닐에스테르로 대신적용하는 방법The method according to claim 14, wherein the unsaturated polyester is used instead of vinyl ester. 상기 14항에 있어서 물유리에 대한 중량비 1~5% 를 혼합하여 적용하는 방법[Claim 14] The method according to claim 14, wherein the mixture is applied in a weight ratio of 1 to 5% with respect to water glass. 상기 14항에 있어서 물유리에 대한 중량비 30~50% 를 혼합하여 적용하는 방법[Claim 14] The method according to claim 14, wherein 30 to 50% by weight of water glass is mixed and applied. 상기 14항에 있어서 물유리에 대한 중량비 50~75% 를 혼합하여 적용하는 방법[Claim 14] The method according to claim 14, wherein 50 to 75% by weight of water glass is mixed and applied.
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KR102508014B1 (en) * 2022-11-11 2023-03-08 박상철 Infectious wastewater treatment tank FRP coating material and coating method therefor

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US3926905A (en) * 1973-06-13 1975-12-16 Osaka Soda Co Ltd Flame retardant hardenable composition of water glass and decorative products made by using the same
US4011195A (en) * 1974-04-12 1977-03-08 H. H. Robertson Company Polymerizable compositions containing unsaturated polyester resins and aqueous alkali metal silicate, method of preparing shaped articles from such compositions and thermoset products thereof
KR20080070485A (en) * 2007-01-25 2008-07-30 정맥산업개발(주) Method for coating agent composite having retardent flame
MX2011005592A (en) * 2008-12-08 2011-06-16 3M Innovative Properties Co Halogen-free flame retardants for epoxy resin systems.
KR20110065590A (en) * 2009-12-10 2011-06-16 (주)엘지하우시스 Wood plastic composite having excellent flame retardant and low manufacturing cost, and method of making the same

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* Cited by examiner, † Cited by third party
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