KR102536423B1 - Method for producing of PU foam sheet with high elasticity and flame retardancy and PU foam sheet produced by the same - Google Patents
Method for producing of PU foam sheet with high elasticity and flame retardancy and PU foam sheet produced by the same Download PDFInfo
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- KR102536423B1 KR102536423B1 KR1020220125918A KR20220125918A KR102536423B1 KR 102536423 B1 KR102536423 B1 KR 102536423B1 KR 1020220125918 A KR1020220125918 A KR 1020220125918A KR 20220125918 A KR20220125918 A KR 20220125918A KR 102536423 B1 KR102536423 B1 KR 102536423B1
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- 229920005830 Polyurethane Foam Polymers 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 34
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003063 flame retardant Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 229920005862 polyol Polymers 0.000 claims abstract description 19
- 150000003077 polyols Chemical class 0.000 claims abstract description 18
- KIQKWYUGPPFMBV-UHFFFAOYSA-N diisocyanatomethane Chemical compound O=C=NCN=C=O KIQKWYUGPPFMBV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006260 foam Substances 0.000 claims abstract description 16
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 13
- 229920000570 polyether Polymers 0.000 claims abstract description 13
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 13
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 13
- 230000005484 gravity Effects 0.000 claims abstract description 12
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 238000005187 foaming Methods 0.000 claims abstract description 7
- 239000004604 Blowing Agent Substances 0.000 claims abstract description 6
- 239000003381 stabilizer Substances 0.000 claims abstract description 6
- 150000005846 sugar alcohols Polymers 0.000 claims description 7
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 150000003017 phosphorus Chemical class 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 6
- -1 Isocyanate compounds Chemical class 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000008186 active pharmaceutical agent Substances 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000012948 isocyanate Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000011496 polyurethane foam Substances 0.000 description 4
- 230000001988 toxicity Effects 0.000 description 4
- 231100000419 toxicity Toxicity 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 150000002513 isocyanates Chemical class 0.000 description 3
- 229920005906 polyester polyol Polymers 0.000 description 3
- 150000007519 polyprotic acids Polymers 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- HOVAGTYPODGVJG-UVSYOFPXSA-N (3s,5r)-2-(hydroxymethyl)-6-methoxyoxane-3,4,5-triol Chemical compound COC1OC(CO)[C@@H](O)C(O)[C@H]1O HOVAGTYPODGVJG-UVSYOFPXSA-N 0.000 description 1
- OBWAHMFFZIWBDX-UHFFFAOYSA-N CC(COC(C)CO)O.C(C(C)O)O.C(COCCOCCO)O.C(COCCO)O.C(CO)O Chemical compound CC(COC(C)CO)O.C(C(C)O)O.C(COCCOCCO)O.C(COCCO)O.C(CO)O OBWAHMFFZIWBDX-UHFFFAOYSA-N 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- 150000007824 aliphatic compounds Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- HZGUCDLMOBUAHV-UHFFFAOYSA-N butanedioic acid;hexanedioic acid;pentanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)CCCC(O)=O.OC(=O)CCCCC(O)=O HZGUCDLMOBUAHV-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- HOVAGTYPODGVJG-UHFFFAOYSA-N methyl beta-galactoside Natural products COC1OC(CO)C(O)C(O)C1O HOVAGTYPODGVJG-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000582 polyisocyanurate Polymers 0.000 description 1
- 239000011495 polyisocyanurate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/721—Two or more polyisocyanates not provided for in one single group C08G18/73 - C08G18/80
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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Abstract
Isomeric Methylene diisocyanate 5-15 중량부와, NCO 28-30 중량%를 갖는 Modified Methylene diisocyanate 20-40 중량부와, Isomeric Tolylene diisocyanate 15-25 중량부와, NCO 18-32 중량%를 갖는 Prepolymerized Polyisocyanate 30-50 중량부를 배합하여 조성물A 형성단계와;
수평균 분자량 6,520 g/mole인 폴리에테르 폴리올 56-59 중량부와, 수평균 당량이 73.24g/mole인 다중 올리고머 6-9 중량부와, 난연 첨가제 30-34 중량부와, 촉매, 발포제 및 안정제 2-4 중량부를 One Shot 배합하는 조성물B 형성단계와;
조성물A 100 중량부에 대하여 조성물B 200-250 중량부를 혼합한 다음, 전동기 임펠러 4,000 rpm 이상으로 소정시간 고속혼합한 후 25-32 ℃에서 소정시간 발포시켜 하기 입체규칙성구조(2)가 규칙적으로 형성된 저비중(0.06이하)의 발포체 형성단계;로 이루어진 것을 특징으로 하는 고탄성 및 난연성의 PU 발포시트 제조방법 및 이의 제조방법에 의해 제조된 PU 발포시트에 관한 것이다.5-15 parts by weight of isomeric methylene diisocyanate, 20-40 parts by weight of Modified Methylene diisocyanate with 28-30 parts by weight of NCO, 15-25 parts by weight of isomeric Tolylene diisocyanate, and 30-40 parts by weight of Prepolymerized Polyisocyanate with 18-32 parts by weight of NCO Forming composition A by blending 50 parts by weight;
56-59 parts by weight of a polyether polyol having a number average molecular weight of 6,520 g/mole, 6-9 parts by weight of a multi-oligomer having a number average equivalent of 73.24 g/mole, 30-34 parts by weight of a flame retardant additive, catalyst, blowing agent and stabilizer Composition B forming step of mixing 2-4 parts by weight of One Shot;
After mixing 200-250 parts by weight of Composition B with respect to 100 parts by weight of Composition A, high-speed mixing at 4,000 rpm or more for a predetermined time with a motor impeller, and then foaming at 25-32 ° C. for a predetermined time to form the following stereoregular structure (2) regularly It relates to a method for producing a high elasticity and flame retardant PU foam sheet comprising a step of forming a foam of low specific gravity (0.06 or less) and a PU foam sheet manufactured by the method.
Description
본 발명은 Isomeric Methylene diisocyanate 5-15 중량부와, NCO 28-30 중량%를 갖는 Modified Methylene diisocyanate 20-40 중량부와, Isomeric Tolylene diisocyanate 15-25 중량부와, NCO 18-32 중량%를 갖는 Prepolymerized Polyisocyanate 30-50 중량부를 배합하여 조성물A 형성단계와;
수평균 분자량 6,520 g/mole인 폴리에테르 폴리올 56-59 중량부와, 수평균 당량이 73.24g/mole인 다중 올리고머 6-9 중량부와, 난연 첨가제 30-34 중량부와, 촉매, 발포제 및 안정제 2-4 중량부를 One Shot 배합하는 조성물B 형성단계와;
조성물A 100 중량부에 대하여 조성물B 200-250 중량부를 혼합한 다음, 전동기 임펠러 4,000 rpm 이상으로 소정시간 고속혼합한 후 25-32 ℃에서 소정시간 발포시켜 하기 입체규칙성구조(2)가 규칙적으로 형성된 저비중(0.06g/㎤이하)의 발포체 형성단계;로 이루어진 것을 특징으로 하는 고탄성 및 난연성의 PU 발포시트 제조방법 및 그 방법에 의해 제조된 고탄성 및 난연성의 PU 발포시트에 관한 것이다.
Rm = - UL-[-(A)-UL-(B)-]n-UL- ------------------- (2)
위의 식(2)에서 Rm은 본 발명의 고탄성 및 난연성 발포체 내에 규칙적으로 형성된 입체규칙성구조이며, UL은 우레탄결합(Urethane Linkage)으로서 N(H)-C(O)-O 구조이며, (A)는 Isomeric Methylene diisocyanate, Modified Methylene diisocyanate, Isomeric Tolylene diisocyanate 및 Prepolymerized Polyisocyanate에 의해 형성된 Isomeric Polyisocyanate의 분자구조이이며, (B)는 폴리에테르 폴리올 및 다중 올리고머에 의해 형성된 수평균분자량 100-500 g/mole인 올리고머 형태의 다가 알코올 구조이며, n은 3-16이다.The present invention is prepolymerized with 5-15 parts by weight of isomeric methylene diisocyanate, 20-40 parts by weight of Modified Methylene diisocyanate having 28-30 parts by weight of NCO, 15-25 parts by weight of isomeric Tolylene diisocyanate, and 18-32 parts by weight of NCO. Forming composition A by blending 30-50 parts by weight of polyisocyanate;
56-59 parts by weight of a polyether polyol having a number average molecular weight of 6,520 g/mole, 6-9 parts by weight of a multi-oligomer having a number average equivalent of 73.24 g/mole, 30-34 parts by weight of a flame retardant additive, catalyst, blowing agent and stabilizer Composition B forming step of mixing 2-4 parts by weight of One Shot;
After mixing 200-250 parts by weight of Composition B with respect to 100 parts by weight of Composition A, high-speed mixing at 4,000 rpm or more for a predetermined time with a motor impeller, and then foaming at 25-32 ° C. for a predetermined time to form the following stereoregular structure (2) regularly It relates to a method for producing a highly elastic and flame retardant PU foam sheet comprising a step of forming a foam of low specific gravity (0.06 g/cm 3 or less) and a highly elastic and flame retardant PU foam sheet produced by the method.
R m = -UL-[-(A)-UL-(B)-] n -UL- ------------------- (2)
In the above formula (2), R m is a tactic structure regularly formed in the highly elastic and flame retardant foam of the present invention, and UL is a urethane linkage, N (H) -C (O) -O structure, (A) is the molecular structure of isomeric polyisocyanate formed by isomeric methylene diisocyanate, modified methylene diisocyanate, isomeric tolylene diisocyanate and prepolymerized polyisocyanate, and (b) is the number average molecular weight of polyether polyol and multiple oligomers of 100-500 g/mole It is a polyhydric alcohol structure in the form of a phosphorus oligomer, and n is 3-16.
일반적으로 폴리우레탄(PU)이라 함은 하기의 반응식과 같이 이소시아네이트기(-NCO)를 함유하는 물질과 수산기를 가진 화합물과의 화학반응에 의해 생성된 우레탄 결합을 갖는 고분자 화합물을 말한다. 여분의 이소시아네이트는 Polyisocyanurate로 생성된다.
상기 폴리올은 화학적 구조에 따라 여러 종류가 있는데, 가장 일반적으로 사용되는 것으로는 폴리에스터(polyester)폴리올과 폴리에테르(polyether)폴리올 등이 있다.
상기 폴리에스터 폴리올은 다염기산과 다가알코올의 축합반응에 의해 생성되어 진다.
이때 다염기산으로는 석시닌산 - 글루타린산 - 아디핀산 - 이소말레인산 - 무수말레인산 및 테레말레인산 등을 사용할 수 있고, 다가 알코올로는 에틸렌글리콜 - 디에틸렌글리콜 - 트리에틸렌글리콜 - 프로필렌글리콜 - 디프로필렌글리콜 - 트리프로필렌글리콜 - 부탄디올 - 펜탄디올 - 헥산디올 - 헵탄디올 - 글리세린 - 트리메틸올프로판 - 펜타에리트리톨 및 메틸글루코시드 등을 사용할 수 있다.
폴리에테르 폴리올은 수산기를 지니는 다가 알코올 또는 다가 아민 화합물을 개시제로 하여 KOH 등의 촉매 존재하에 Ethylene Oxide (EO), Propylene Oxide (PO) 등을 Ring Openning Addition Reaction(개환부가 반응)에 의해 여러 가지 폴리올을 얻게 된다.
폴리에테르 폴리올을 합성하기 위한 다가알콜 개시제로는 에틸렌글리콜 - 디에틸렌글리콜 - 트리에틸렌글리콜 - 프로필렌글리콜 - 디프로필렌글리콜 - 트리프로필렌글리콜 - 부탄디올 - 펜탄디올 - 헥산디올 - 헵탄디올 - 글리세린 - 트리메틸올프로판 - 펜타에리트리톨 및 메틸글루코시드- 등 이며 디 아민 개시제로는 에칠렌 디아민, 프로필렌 디아민-톨릴렌 디 아민 등을 사용하여 폴리올을 합성하여 얻게 된다.
종래기술로서 특허등록 제10-0666140호에 제1폴리올 화합물, 방향족폴리이소시아네이트 화합물, 사슬연장제, 가소제, 충진물 및 첨가제, 착색안료의 혼합물에 제2폴리올화합물, 물 및 각색 염료를 주성분으로 하는 경화제를 배합하여 친환경 폴리우레탄 방수 바닥재 수지조성물이 공지되어 있으며, 공개특허 제10-2008-0080762호에 난연성 폴리에스테르 폴리올과 그 제조방법이 공지되어 있다.
이와 같이 종래기술들은 탄성의 폴리우레탄 발포시트 또는 난연성의 폴리우레탄 발포시트 공지되어 있으나 고탄성과 난연성을 동시에 구현된 폴리우레탄 발포시트는 충분히 개발되고 있지 못하는 실정이었다.
이에 본 발명은 고탄성 및 난연성을 동시에 만족하는 PU 발포시트 개발에 착수하여, 소정의 조성물A와 조성물B를 고속 RPM 혼합 후 발포공정을 통하여 폴리우레탄 반응이 형성되어 식(2)의 입체규칙성구조 Rm 가 발포체 내에 규칙적으로 형성된 고탄성 및 난연성의 PU 발포시트를 개발할 수 있었다.
본 발명은 발포체 비중이 0.06g/㎤이하의 저비중 발포체로서 이와 같은 저비중의 발포체 속에 입체규칙성구조 Rm를 규칙적으로 형성함으로서 우수한 탄성 및 난연성의 PU 발포시트를 형성할 수 있었다.In general, polyurethane (PU) refers to a polymer compound having a urethane bond formed by a chemical reaction between a material containing an isocyanate group (-NCO) and a compound having a hydroxyl group, as shown in the following reaction formula. Excess isocyanate is produced as Polyisocyanurate.
There are several types of polyols according to their chemical structures, and the most commonly used ones include polyester polyols and polyether polyols.
The polyester polyol is produced by a condensation reaction between a polybasic acid and a polyhydric alcohol.
In this case, succinic acid - glutaric acid - adipic acid - isomaleic acid - maleic anhydride and teremaleic acid may be used as the polybasic acid, and ethylene glycol - diethylene glycol - triethylene glycol - propylene glycol - dipropylene glycol - as the polybasic acid. Tripropylene glycol - butanediol - pentanediol - hexanediol - heptanediol - glycerin - trimethylolpropane - pentaerythritol and methyl glucoside may be used.
Polyether polyol uses a polyhydric alcohol or polyhydric amine compound having a hydroxyl group as an initiator, and in the presence of a catalyst such as KOH, Ethylene Oxide (EO), Propylene Oxide (PO), etc. are reacted by Ring Opening Addition Reaction (Ring Opening Addition Reaction). polyols are obtained.
Polyhydric alcohol initiators for synthesizing polyether polyol include ethylene glycol - diethylene glycol - triethylene glycol - propylene glycol - dipropylene glycol - tripropylene glycol - butanediol - pentanediol - hexanediol - heptanediol - glycerin - trimethylolpropane. -Pentaerythritol and methyl glucoside-, etc. It is obtained by synthesizing a polyol using ethylene diamine, propylene diamine-tolylene diamine, etc. as a diamine initiator.
As a prior art, Patent Registration No. 10-0666140 discloses a first polyol compound, an aromatic polyisocyanate compound, a chain extender, a plasticizer, a filler and an additive, and a second polyol compound in a mixture of color pigments, a curing agent containing water and various dyes as main components Eco-friendly polyurethane waterproof flooring resin composition is known, and flame retardant polyester polyol and its manufacturing method are known in Patent Publication No. 10-2008-0080762.
In this way, the prior art is known as an elastic polyurethane foam sheet or a flame retardant polyurethane foam sheet, but a polyurethane foam sheet having high elasticity and flame retardancy at the same time has not been sufficiently developed.
Therefore, the present invention started to develop a PU foam sheet that satisfies high elasticity and flame retardancy at the same time, and after mixing predetermined composition A and composition B at high speed RPM, a polyurethane reaction was formed through a foaming process to form a stereoregular structure of formula (2) It was possible to develop a highly elastic and flame retardant PU foam sheet in which R m was regularly formed in the foam.
The present invention is a low specific gravity foam having a specific gravity of 0.06 g/cm 3 or less, and a PU foam sheet having excellent elasticity and flame retardancy can be formed by regularly forming the stereoregular structure R m in such a low specific gravity foam.
본 발명은 소정의 조성물A 및 조성물B를 형성하고, 형성된 조성물A 및 조성물B를 소정 비율로 혼합한 후 고속 RPM 혼합 후 발포공정을 통하여 폴리우레탄(PU) 반응이 진행되어 입체규칙성구조 Rm 이 규칙적으로 형성된 저비중(0.06이하)의 고탄성 및 난연성의 PU 발포시트를 제조하는 방법 및 그 제조 방법에 의해 제조된 PU 발포시트를 제공하는 것을 본 발명의 목적으로 한다.In the present invention, a predetermined composition A and a composition B are formed, the formed composition A and composition B are mixed in a predetermined ratio, and a polyurethane (PU) reaction proceeds through a foaming process after mixing at high speed RPM to form a stereoregular structure R m It is an object of the present invention to provide a method for producing a regularly formed, low specific gravity (less than 0.06), highly elastic and flame retardant PU foam sheet and a PU foam sheet manufactured by the method.
이러한 목적을 달성하기 위하여, 본 발명은 Isomeric Methylene diisocyanate 5-15 중량부와, NCO 28-30 중량%를 갖는 Modified Methylene diisocyanate 20-40 중량부와, Isomeric Tolylene diisocyanate 15-25 중량부와, NCO 18-32 중량%를 갖는 Prepolymerized Polyisocyanate 30-50 중량부를 배합하여 조성물A 형성단계와;
수평균 분자량 6,520 g/mole인 폴리에테르 폴리올 56-59 중량부와, 수평균 당량이 73.24g/mole인 다중 올리고머 6-9 중량부와, 난연 첨가제 30-34 중량부와, 촉매, 발포제 및 안정제 2-4 중량부를 One Shot 배합하는 조성물B 형성단계와;
조성물A 100 중량부에 대하여 조성물B 200-250 중량부를 혼합한 다음, 전동기 임펠러 4,000 rpm 이상으로 소정시간 고속혼합한 후 25-32 ℃에서 소정시간 발포시켜 하기 입체규칙성구조(2)가 규칙적으로 형성된 저비중(0.06이하)의 발포체 형성단계;로 이루어진 것을 특징으로 하는 고탄성 및 난연성의 PU 발포시트 제조방법.
Rm = - UL-[-(A)-UL-(B)-]n-UL- ------------------- (2)
위의 식(2)에서 Rm은 본 발명의 고탄성 및 난연성 발포체 내에 규칙적으로 형성된 입체규칙성구조이며, UL은 우레탄결합(Urethane Linkage)으로서 N(H)-C(O)-O 구조이며, (A)는 Isomeric Methylene diisocyanate, Modified Methylene diisocyanate, Isomeric Tolylene diisocyanate 및 Prepolymerized Polyisocyanate에 의해 형성된 Isomeric Polyisocyanate의 분자구조이이며, (B)는 폴리에테르 폴리올 및 다중 올리고머에 의해 형성된 수평균분자량 100-500 g/mole인 올리고머 형태의 다가 알코올 구조이며, n은 3-16이다.
또한 본 발명은 상기 제조방법에 의해 제조된 입체규칙성구조가 규칙적으로 형성된 저비중(0.06이하)인 것을 특징으로 하는 고탄성 및 난연성의 PU 발포시트에 관한 것이다.
본 발명의 폴리우레탄(PU)는 다음 식(1)과 같이 표시된다.
HO-〔-P-UL-Rm-UL-K]n -NCO ------------------ (1)
Rm = - UL-[-(A)-UL-(B)-]n-UL- ----------------- (2)
상기 식에서 K는 유기탄소 C가 6-24개인 다중 이소시아네이트 화합물이며, P는 수평균분자량이 3,000-7,000 g/mole인 폴리에테르 폴리올로서 수산기 2-4개를지니는 폴리올 구조이며, Rm은 본 발명의 고탄성 및 난연성 발포체 내에 규칙적으로 형성된 입체규칙성구조이며, (B)는 수평균분자량 100-500 g/mole인 올리고머 형태의 다가 알코올 구조이며, UL은 우레탄결합(Urethane Linkage)으로서 N(H)-C(O)-O 구조이며, B는 (A)는 방향족 또는 지방족 방향족 화합물로서 관능기(NCO)가 2 이상인 다중 분자구조의 형태이며, 식(1)에서 n은 1이상이며, 식(2)에서 n은 3-16이다.
본 발명은 소정의 조성물을 고속RPM 혼합 후 발포공정을 통하여 입체규칙성구조 Rm 를 발포체 내에 규칙적으로 형성함으로써 고탄성 및 난연성의 저비중 PU 발포시트를 제조할 수 있었으며, 제조된 시제품에 대한 물성시험을 통해 우수한 탄성 및 난연성을 확인할 수 있었다.
본 발명에 사용되는 조성물A는 Isomeric Methylene diisocyanate, NCO 28-30 중량%를 갖는 Moified Methylene diisocyanate, Isomeric Tolylene diisocyanate 및 NCO 18-32 중량%를 갖는 Prepolymerized Polyisocyanate이 소정량씩 배합된 이소시아네이트 조성물(Polymeric Isocyanate Mixture)이며, 조성물B는 수평균 분자량 6,520 g/mole인 폴리에테르 폴리올, 수평균 당량이 73.24g/mole인 다중 올리고머, 난연 첨가제, 촉매, 발포제 및 안정제를 One Shot 소정량씩 배합한 것이다.
본 발명은 조성물A 100 중량부에 대하여 조성물B 200-250 중량부를 혼합한 다음, 고속 rpm으로 소정시간 혼합한 후 성형틀에서 25-32 ℃에서 소정시간 발포시켜 폴리우레탄(PU) 반응이 형성되고 폴리우레탄(PU) 내 식(2)의 결정성 입체구조가 발포체 내에 규칙적으로 형성됨으로써 저비중의 고탄성 및 난연성 PU 발포체를 얻을 수 있었으며, 발포체 밀도, 경도, 반복 영구 압축 줄음율, 영구압축 줄음율, 열방출율, 난연성을 나타내는 연기밀도, 독성지수 등 시험을 통하여 확인할 수 있었다.In order to achieve this object, the present invention provides 5-15 parts by weight of isomeric Methylene diisocyanate, 20-40 parts by weight of Modified Methylene diisocyanate having 28-30% by weight of NCO, 15-25 parts by weight of isomeric Tolylene diisocyanate, and NCO 18 Forming Composition A by blending 30-50 parts by weight of Prepolymerized Polyisocyanate having -32% by weight;
56-59 parts by weight of a polyether polyol having a number average molecular weight of 6,520 g/mole, 6-9 parts by weight of a multi-oligomer having a number average equivalent of 73.24 g/mole, 30-34 parts by weight of a flame retardant additive, catalyst, blowing agent and stabilizer Composition B forming step of mixing 2-4 parts by weight of One Shot;
After mixing 200-250 parts by weight of Composition B with respect to 100 parts by weight of Composition A, high-speed mixing at 4,000 rpm or more for a predetermined time with a motor impeller, and then foaming at 25-32 ° C. for a predetermined time to form the following stereoregular structure (2) regularly Forming a foam of low specific gravity (0.06 or less) formed; high elasticity and flame retardant PU foam sheet manufacturing method, characterized in that consisting of.
R m = -UL-[-(A)-UL-(B)-] n -UL- ------------------- (2)
In the above formula (2), R m is a tactic structure regularly formed in the highly elastic and flame retardant foam of the present invention, and UL is a urethane linkage, N (H) -C (O) -O structure, (A) is the molecular structure of isomeric polyisocyanate formed by isomeric methylene diisocyanate, modified methylene diisocyanate, isomeric tolylene diisocyanate and prepolymerized polyisocyanate, and (b) is the number average molecular weight of polyether polyol and multiple oligomers of 100-500 g/mole It is a polyhydric alcohol structure in the form of a phosphorus oligomer, and n is 3-16.
In addition, the present invention relates to a high elasticity and flame retardant PU foam sheet characterized in that the stereoregular structure produced by the above production method is regularly formed and has a low specific gravity (0.06 or less).
The polyurethane (PU) of the present invention is represented by the following formula (1).
HO-[-P-UL-R m -UL-K] n -NCO ------------------ (1)
R m = -UL-[-(A)-UL-(B)-] n -UL- ----------------- (2)
In the above formula, K is a polyisocyanate compound having 6 to 24 organic carbon atoms, P is a polyether polyol having a number average molecular weight of 3,000 to 7,000 g/mole and has a polyol structure having 2 to 4 hydroxyl groups, and R m is the present invention. is a stereoregular structure regularly formed in the highly elastic and flame retardant foam, (B) is an oligomeric polyhydric alcohol structure with a number average molecular weight of 100-500 g/mole, and UL is a urethane linkage, N(H) -C (O) -O structure, B is (A) is an aromatic or aliphatic aromatic compound in the form of a multi-molecular structure in which the functional group (NCO) is 2 or more, in formula (1) n is 1 or more, formula (2 ), n is 3-16.
The present invention was able to manufacture a high elasticity and flame retardant low specific gravity PU foam sheet by regularly forming the stereoregular structure R m in the foam through a foaming process after mixing a predetermined composition at high RPM, and physical property tests on the manufactured prototype It was confirmed through excellent elasticity and flame retardancy.
Composition A used in the present invention is an isocyanate composition (Polymeric Isocyanate Mixture ), and composition B is a polyether polyol having a number average molecular weight of 6,520 g/mole, a multi-oligomer having a number average equivalent of 73.24 g/mole, a flame retardant additive, a catalyst, a blowing agent, and a stabilizer in predetermined amounts in one shot.
In the present invention, 200-250 parts by weight of composition B is mixed with 100 parts by weight of composition A, mixed at high rpm for a predetermined time, and then foamed in a mold at 25-32 ° C. for a predetermined time to form a polyurethane (PU) reaction The crystalline three-dimensional structure of Formula (2) in polyurethane (PU) was regularly formed in the foam, thereby obtaining a high elasticity and flame retardant PU foam with low specific gravity, foam density, hardness, repeated compression set, and compression set. , heat release rate, smoke density indicating flame retardancy, toxicity index, etc. were confirmed through tests.
본 발명은 소정의 조성물A 및 조성물B를 고속 RPM 혼합 후 발포과정을 통하여 폴리우레탄(PU) 반응을 형성하여 입체규칙성구조 Rm를 발포체 내 규칙적으로 형성함으로써 저비중(0.06이하)의 고탄성 및 난연성 PU발포시트를 얻는 효과가 있었다. The present invention provides high elasticity and There was an effect of obtaining a flame retardant PU foam sheet.
도 1: 본 발명의 제조공정도를 보여주는 것이다.
도 2: 본 발명의 일 실시예로서 제조된 고탄성 및 난연성 PU 발포시트 시제품을 보여주는 것이다.Figure 1: shows the manufacturing process diagram of the present invention.
Figure 2: shows a high elasticity and flame retardant PU foam sheet prototype manufactured as an embodiment of the present invention.
실시예
Isomeric Methylene diisocyanate 5-15 중량부와, NCO 29 중량%를 갖는 Modified Methylene diisocyanate 30 중량부와, Isomeric Tolylene diisocyanate 20 중량부와, NCO 20 중량%를 갖는 Prepolymerized Polyisocyanate 40 중량부를 배합하여 조성물A 형성하였다.
수평균 분자량 6,520 g/mole인 폴리에테르 폴리올 57.85 중량부와, 수평균 당량이 73.24g/mole인 다중 올리고머 7.23 중량부와, 난연 첨가제 31.82 중량부와, 촉매, 발포제 및 안정제 2-4 중량부를 One Shot 배합하는 조성물B를 제조하였다.
본 발명은 상기 조성물A 100 중량부에 대하여 조성물B 230 중량부를 혼합한 다음, 전동기 임펠러 4,500 rpm 이상으로 10초간 고속혼합한 후 30℃에서 11분간 발포시켜 하기 식(2)의 입체규칙성구조 Rm 를 규칙적으로 형성한 발포체를 얻을 수 있었다.
Rm = - UL-[-(A)-UL-(B)-]n-UL- ------------------- (2)
상기 실시예를 통하여 얻은 시제품에 대한 시험결과는 다음과 같다.
시험조건: 50 % 압축, 80000회.
시험조건: 70±1℃, 22 Hrs, 50% 압축.
(지속적인 불꽃 연소에 도달한 시간)
종료 시점사이
90% 사이
(독성지수)
상술한 시험결과에서 알 수 있는 바와 같이, 본 발명의 제조방법에 의해 제조된 폴리우레탄(PU) 발포시트의 우수한 탄성 및 난연성의 폴리우레탄 발포시트임을 확인할 수 있었으며 독성지수 시험으로 우수한 인체무해성을 확인할 수 있었다.
본 발명의 구성은 상기 실시예에 한정되는 것은 아니며 통상의 기술범주에서 실시할 수 있는 다양한 실시예를 포함하는 것이다.Example
Composition A was formed by mixing 5-15 parts by weight of isomeric methylene diisocyanate, 30 parts by weight of modified methylene diisocyanate with 29 wt% of NCO, 20 parts by weight of isomeric tolylene diisocyanate, and 40 parts by weight of prepolymerized polyisocyanate with 20 wt% of NCO.
57.85 parts by weight of a polyether polyol having a number average molecular weight of 6,520 g/mole, 7.23 parts by weight of a multi-oligomer having a number average equivalent of 73.24 g/mole, 31.82 parts by weight of a flame retardant additive, and 2-4 parts by weight of a catalyst, a blowing agent, and a stabilizer, One Composition B for shot mixing was prepared.
In the present invention, 230 parts by weight of composition B is mixed with 100 parts by weight of composition A, mixed at high speed for 10 seconds at 4,500 rpm or more with a motor impeller, and then foamed at 30 ° C. for 11 minutes to form a stereoregular structure R of the following formula (2) A foam in which m was regularly formed was obtained.
R m = -UL-[-(A)-UL-(B)-] n -UL- ------------------- (2)
The test results of the prototypes obtained through the above examples are as follows.
Test conditions: 50 % compression, 80000 cycles.
Test conditions: 70±1°C, 22 Hrs, 50% compression.
(time to reach continuous flame burning)
between end points
between 90%
(toxicity index)
As can be seen from the above test results, it was confirmed that the polyurethane foam sheet produced by the manufacturing method of the present invention has excellent elasticity and flame retardancy, and it was confirmed that the toxicity index test showed excellent harmlessness to the human body. I was able to confirm.
The configuration of the present invention is not limited to the above embodiments, but includes various embodiments that can be implemented in the general technical category.
Claims (2)
수평균 분자량 6,520 g/mole인 폴리에테르 폴리올 56-59 중량부와, 수평균 당량이 73.24g/mole인 다중 올리고머 6-9 중량부와, 난연 첨가제 30-34 중량부와, 촉매, 발포제 및 안정제 2-4 중량부를 One Shot 배합하는 조성물B 형성단계와;
조성물A 100 중량부에 대하여 조성물B 200-250 중량부를 혼합한 다음, 전동기 임펠러 4,000 rpm 이상으로 소정시간 고속혼합한 후 25-32 ℃에서 소정시간 발포시켜 하기 입체규칙성구조(2)가 규칙적으로 형성된 저비중(0.06이하)의 발포체 형성단계;로 이루어진 것을 특징으로 하는 고탄성 및 난연성의 PU 발포시트 제조방법.
Rm = - UL-[-(A)-UL-(B)-]n-UL- ------------------- (2)
위의 식(2)에서 Rm은 본 발명의 고탄성 및 난연성 발포체 내에 규칙적으로 형성된 입체규칙성구조이며, UL은 우레탄결합(Urethane Linkage)으로서 N(H)-C(O)-O 구조이며, (A)는 Isomeric Methylene diisocyanate, Modified Methylene diisocyanate, Isomeric Tolylene diisocyanate 및 Prepolymerized Polyisocyanate에 의해 형성된 Isomeric Polyisocyanate의 분자구조이이며, (B)는 폴리에테르 폴리올 및 다중 올리고머에 의해 형성된 수평균분자량 100-500 g/mole인 올리고머 형태의 다가 알코올 구조이며, n은 3-16이다.5-15 parts by weight of isomeric methylene diisocyanate, 20-40 parts by weight of Modified Methylene diisocyanate with 28-30 parts by weight of NCO, 15-25 parts by weight of isomeric Tolylene diisocyanate, and 30-40 parts by weight of Prepolymerized Polyisocyanate with 18-32 parts by weight of NCO Forming composition A by blending 50 parts by weight;
56-59 parts by weight of a polyether polyol having a number average molecular weight of 6,520 g/mole, 6-9 parts by weight of a multi-oligomer having a number average equivalent of 73.24 g/mole, 30-34 parts by weight of a flame retardant additive, catalyst, blowing agent and stabilizer Composition B forming step of mixing 2-4 parts by weight of One Shot;
After mixing 200-250 parts by weight of Composition B with respect to 100 parts by weight of Composition A, high-speed mixing at 4,000 rpm or more for a predetermined time with a motor impeller, and then foaming at 25-32 ° C. for a predetermined time to form the following stereoregular structure (2) regularly Forming a foam of low specific gravity (0.06 or less) formed; high elasticity and flame retardant PU foam sheet manufacturing method, characterized in that consisting of.
R m = -UL-[-(A)-UL-(B)-] n -UL- ------------------- (2)
In the above formula (2), R m is a tactic structure regularly formed in the highly elastic and flame retardant foam of the present invention, and UL is a urethane linkage, N (H) -C (O) -O structure, (A) is the molecular structure of isomeric polyisocyanate formed by isomeric methylene diisocyanate, modified methylene diisocyanate, isomeric tolylene diisocyanate and prepolymerized polyisocyanate, and (b) is the number average molecular weight of polyether polyol and multiple oligomers of 100-500 g/mole It is a polyhydric alcohol structure in the form of a phosphorus oligomer, and n is 3-16.
A highly elastic and flame retardant PU foam sheet, characterized in that the stereoregular structure R m prepared by the manufacturing method of claim 1 has a low specific gravity (0.06 or less) regularly formed in the foam.
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| KR20210071256A (en) * | 2019-12-06 | 2021-06-16 | 금호미쓰이화학 주식회사 | Eco-friendly Integral skin polyurethane foam composition with excellent durability and elongation and Integral skin polyurethane foam manufactured using the same |
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- 2022-10-03 KR KR1020220125918A patent/KR102536423B1/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR970011714A (en) * | 1995-08-31 | 1997-03-27 | 배순훈 | Defrost cycle determination device and method of the refrigerator |
| WO2004007595A1 (en) * | 2002-07-11 | 2004-01-22 | Lendell Manufacturing, Inc. | Antimicrobial polyurethane foam |
| JP2010527400A (en) * | 2007-05-15 | 2010-08-12 | ダウ グローバル テクノロジーズ インコーポレイティド | High elastic foam |
| JP2010260932A (en) * | 2009-04-30 | 2010-11-18 | Bridgestone Corp | Polyurethane foam molding |
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