CN107674408A - A kind of high tenacity high flame-retardant polyurethane circuit board material - Google Patents
A kind of high tenacity high flame-retardant polyurethane circuit board material Download PDFInfo
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- CN107674408A CN107674408A CN201711090685.3A CN201711090685A CN107674408A CN 107674408 A CN107674408 A CN 107674408A CN 201711090685 A CN201711090685 A CN 201711090685A CN 107674408 A CN107674408 A CN 107674408A
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- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
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Abstract
The invention discloses a kind of high tenacity high flame-retardant polyurethane circuit board material, its raw material includes：PEPA, 2,6 diisopropyl phenylisocyanates, dimethyl diphenyl diisocyanate, terephthalyl alcohol, 1,4 butanediols, 4,4' diaminourea 3,3' dichloro diphenyl methanes, dibutyl tin laurate, catalyst DMP 30, bicyclopentadiene dioxide expoxy resin, polyvinyl chloride, maleic anhydride, nano-calcium carbonate, α, ω dialkyl polydimethylsiloxanes, 1 oxygen, 42,6,7 trioxa of methylol 1 phosphabicyclo [2.2.2] octane, phosphonium flame retardant.High tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, it has excellent anti-flammability and toughness, and heat-resist, service life length.
Description
Technical field
The present invention relates to polyurethane circuit boards technical field, more particularly to a kind of high tenacity high flame-retardant polyurethane circuit board
Material.
Background technology
Polyurethane is described as " the fifth-largest plastics ", because it has good physical and mechanical properties, wear-resisting, oil resistant, resistance toization
Learn tear-resistant burn into, resistance to ozone, radiation hardness, the remarkable performance such as damping capaicty is strong, adhesion is good and be widely used in gently
The fields such as work, chemical industry, electronics, weaving, medical treatment, building, building materials, automobile, national defence, space flight, aviation.But the resistance of polyurethane material
Combustion property and toughness are less desirable, use it in circuit board, the defects of anti-flammability and not good enough toughness be present, and limiting it should
With the defects of in order to improve polyurethane, meeting the performance of circuit board material, generally require to be modified polyurethane.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of high tenacity high flame-retardant polyurethane circuit boards
Material, it has excellent anti-flammability and toughness, and heat-resist, service life length.
A kind of high tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, its raw material include by weight：Polyester
Polyalcohol 50-70 parts, 2,6- diisopropyl phenylisocyanate 30-55 parts, dimethyl diphenyl diisocyanate 40-60 parts, to benzene
Dimethanol 5-18 parts, BDO 3-15 parts, 4,4'- diaminourea -3,3'- dichloro diphenyl methane 2-14 parts, tin dilaurate two
Butyl tin 1-2.5 parts, catalyst DMP-30 1-1.3 parts, bicyclopentadiene dioxide expoxy resin 2-14 parts, polyvinyl chloride 3-
10 parts, maleic anhydride 2-10 parts, nano-calcium carbonate 3-15 parts, α, alpha, omega-dihydroxy polydimethyl siloxane 2-3.8 parts, 1-
Oxygen -4- methylol -2,6,7- trioxa -1- phosphabicyclos [2.2.2] octane 2-10 parts, phosphonium flame retardant 3-15 parts.
Preferably, the PEPA is PCDL, polyethylene glycol adipate glycol, polyadipate the third two
One or more kinds of mixtures in alcohol esterdiol, polybutylene glyool adipate.
Preferably, the epoxide number of bicyclopentadiene dioxide expoxy resin is 0.5-0.87.
Preferably, the average grain diameter of the nano-calcium carbonate is 20-45nm.
Preferably, the phosphonium flame retardant is prepared according to following technique：Pentaerythrite and POCl3 are added anti-
Answer in device, the stirring reaction 4-7h at 70-80 DEG C, react after terminating through washing, being dried to obtain material A；By para hydroxybenzene first
Sour methyl esters is added in dioxane, is stirring evenly and then adding into material A, the stirring reaction 8-12h at 80-90 DEG C, after reaction terminates
It is scrubbed, be dried to obtain the phosphonium flame retardant.
Preferably, in the preparation process of phosphonium flame retardant, pentaerythrite, the weight ratio of POCl3 are 5-7：30-40.
Preferably, in the preparation process of phosphonium flame retardant, methyl p-hydroxybenzoate, the weight ratio of material A are 11-
14：8-17.
High tenacity high flame-retardant polyurethane circuit board material of the present invention, in its raw material, the titanium dioxide bicyclic penta 2 of addition
Alkene epoxy resin forms inierpeneirating network structure with polyurethane, adds the crosslink density of network, bicyclopentadiene dioxide ring
The rigid structure formed after oxygen resin solidification significantly improves the mechanical property of composite, and assigns composite excellent resistance to
It is hot；With terephthalyl alcohol, BDO, 4,4'- diaminourea -3,3'- dichloro diphenyl methane for chain extender, with tin dilaurate
Dibutyl tin and catalyst DMP-30 are catalyst, using maleic anhydride as curing agent, significantly improve consolidating for composite
Change speed and curing degree；In polyvinyl chloride addition system, hydrogen bond can be formed with polyurethane and nano-calcium carbonate respectively, so that receiving
Rice calcium carbonate has uniformly been diffused into the strand gap of blend, significantly improves the impact strength of composite, is assigned multiple
The excellent toughness of condensation material, it is therefore prevented that the composite impact toughness caused by the addition of bicyclopentadiene dioxide expoxy resin
The defects of decline；In the preparation process of preferred embodiment phosphonium flame retardant, first using pentaerythrite and POCl3 as raw material, make season
The chlorine in hydroxyl and POCl3 in penta tetrol is reacted, by controlling the condition of reaction to obtain chloride material A,
Material A is mixed with methyl p-hydroxybenzoate, the chlorine in material A is further reacted with methyl p-hydroxybenzoate
Phosphonium flame retardant has been obtained, has been added into system, has been uniformly dispersed in system, on the one hand, has coordinated with nano-calcium carbonate and assigns
The excellent toughness of circuit board material, on the other hand, and α, alpha, omega-dihydroxy polydimethyl siloxane, 1- oxygen -4- methylols -2,6,
7- trioxa -1- phosphabicyclos [2.2.2] octanes and polyvinyl chloride coordinate, and assign the excellent heat resistance of circuit board material and fire-retardant
Property.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of high tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, its raw material include by weight：Polyester
70 parts of polyalcohol, 30 parts of 2,6- diisopropyls phenylisocyanate, 40 parts of dimethyl diphenyl diisocyanate, terephthalyl alcohol 18
Part, 3 parts of BDO, 14 parts of 4,4'- diaminourea -3,3'- dichloro diphenyl methane, 1 part of dibutyl tin laurate, catalyst
1.3 parts of DMP-30,2 parts of bicyclopentadiene dioxide expoxy resin, 10 parts of polyvinyl chloride, 2 parts of maleic anhydride, nano-sized carbon
Sour 15 parts of calcium, α, 2 parts of alpha, omega-dihydroxy polydimethyl siloxane, 1- oxygen -4- methylol -2,6,7- trioxa -1- phosphabicyclos
10 parts of [2.2.2] octane, 3 parts of phosphonium flame retardant.
Embodiment 2
A kind of high tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, its raw material include by weight：Polyester
50 parts of polyalcohol, 55 parts of 2,6- diisopropyls phenylisocyanate, 60 parts of dimethyl diphenyl diisocyanate, 5 parts of terephthalyl alcohol,
15 parts of BDO, 2 parts of 4,4'- diaminourea -3,3'- dichloro diphenyl methane, 2.5 parts of dibutyl tin laurate, catalyst
1 part of DMP-30,14 parts of bicyclopentadiene dioxide expoxy resin, 3 parts of polyvinyl chloride, 10 parts of maleic anhydride, nano-calcium carbonate
3 parts of calcium, α, 3.8 parts of alpha, omega-dihydroxy polydimethyl siloxane, 1- oxygen -4- methylol -2,6,7- trioxa -1- phosphabicyclos
2 parts of [2.2.2] octane, 15 parts of phosphonium flame retardant.
Embodiment 3
A kind of high tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, its raw material include by weight：Poly- carbon
66 parts of acid esters glycol, 38 parts of 2,6- diisopropyls phenylisocyanate, 58 parts of dimethyl diphenyl diisocyanate, terephthalyl alcohol 9
Part, 13 parts of BDO, 5 parts of 4,4'- diaminourea -3,3'- dichloro diphenyl methane, 2.1 parts of dibutyl tin laurate, catalysis
1 part of agent DMP-30,12 parts of bicyclopentadiene dioxide expoxy resin, 4.8 parts of polyvinyl chloride, 8.5 parts of maleic anhydride, receive
4.8 parts of calcium carbonate of rice, α, 3.2 parts of alpha, omega-dihydroxy polydimethyl siloxane, 1- oxygen -4- methylol -2,6,7- trioxa -1- phosphorus
Miscellaneous bicyclic 2.6 parts of [2.2.2] octane, 5 parts of phosphonium flame retardant；
Wherein, the epoxide number of bicyclopentadiene dioxide expoxy resin is 0.87；
The average grain diameter of the nano-calcium carbonate is 20nm；
The phosphonium flame retardant is prepared according to following technique：Pentaerythrite and POCl3 are added into reaction unit
In, wherein, pentaerythrite, the weight ratio of POCl3 are 5：40, the stirring reaction 7h at 70 DEG C, reaction terminate after through washing,
It is dried to obtain material A；Methyl p-hydroxybenzoate is added in dioxane, is stirring evenly and then adding into material A, wherein, to hydroxyl
Yl benzoic acid methyl esters, the weight ratio of material A are 11：17, the stirring reaction 12h at 80 DEG C, reaction terminate after through washing, it is dry
To the phosphonium flame retardant.
Embodiment 4
A kind of high tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, its raw material include by weight：Gather oneself
25 parts of naphthalate glycol, 28 parts of polypropylene glycol adipate glycol, 52 parts of 2,6- diisopropyls phenylisocyanate, diformazan
47 parts of base biphenyl diisocyanate, 15 parts of terephthalyl alcohol, 6 parts of BDO, 4,4'- diaminourea -3,3'- dichloro first
12 parts of alkane, 1.6 parts of dibutyl tin laurate, 1.3 parts of catalyst DMP-30,4 parts of bicyclopentadiene dioxide expoxy resin,
9 parts of polyvinyl chloride, 5 parts of maleic anhydride, 13 parts of nano-calcium carbonate, α, 2.7 parts of alpha, omega-dihydroxy polydimethyl siloxane, 1-
8 parts of oxygen -4- methylols -2,6,7- trioxa -1- phosphabicyclos [2.2.2] octane, 12 parts of phosphonium flame retardant；
Wherein, the epoxide number of bicyclopentadiene dioxide expoxy resin is 0.5；
The average grain diameter of the nano-calcium carbonate is 45nm；
The phosphonium flame retardant is prepared according to following technique：Pentaerythrite and POCl3 are added into reaction unit
In, wherein, pentaerythrite, the weight ratio of POCl3 are 7：30, the stirring reaction 4h at 80 DEG C, reaction terminate after through washing,
It is dried to obtain material A；Methyl p-hydroxybenzoate is added in dioxane, is stirring evenly and then adding into material A, wherein, to hydroxyl
Yl benzoic acid methyl esters, the weight ratio of material A are 14：8, the stirring reaction 8h at 90 DEG C, react after terminating through washing, being dried to obtain
The phosphonium flame retardant.
Embodiment 5
A kind of high tenacity high flame-retardant polyurethane circuit board material proposed by the present invention, its raw material include by weight：Polyester
65 parts of polyalcohol, 35 parts of 2,6- diisopropyls phenylisocyanate, 53 parts of dimethyl diphenyl diisocyanate, terephthalyl alcohol 11
Part, 12 parts of BDO, 9 parts of 4,4'- diaminourea -3,3'- dichloro diphenyl methane, 1.9 parts of dibutyl tin laurate, catalysis
1.2 parts of agent DMP-30,9 parts of bicyclopentadiene dioxide expoxy resin, 7 parts of polyvinyl chloride, 6 parts of maleic anhydride, nano-sized carbon
Sour 12 parts of calcium, α, 2.9 parts of alpha, omega-dihydroxy polydimethyl siloxane, 1- oxygen -4- methylol -2,6,7- trioxa -1- phosphabicyclos
7.3 parts of [2.2.2] octane, 12 parts of phosphonium flame retardant；
Wherein, the PEPA is PCDL, polyethylene glycol adipate glycol, polyadipate propane diols
The mixture of esterdiol, polybutylene glyool adipate, and PCDL, polyethylene glycol adipate glycol, gather oneself
Two acid propylene glycol ester glycol, the weight ratio of polybutylene glyool adipate are 4：4：2：3；
The epoxide number of bicyclopentadiene dioxide expoxy resin is 0.63；
The average grain diameter of the nano-calcium carbonate is 30nm；
The phosphonium flame retardant is prepared according to following technique：Pentaerythrite and POCl3 are added into reaction unit
In, wherein, pentaerythrite, the weight ratio of POCl3 are 6：37, the stirring reaction 6h at 75 DEG C, reaction terminate after through washing,
It is dried to obtain material A；Methyl p-hydroxybenzoate is added in dioxane, is stirring evenly and then adding into material A, wherein, to hydroxyl
Yl benzoic acid methyl esters, the weight ratio of material A are 12：13, the stirring reaction 11h at 86 DEG C, reaction terminate after through washing, it is dry
To the phosphonium flame retardant.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of high tenacity high flame-retardant polyurethane circuit board material, it is characterised in that its raw material includes by weight：Polyester polyols
Alcohol 50-70 parts, 2,6- diisopropyl phenylisocyanate 30-55 parts, dimethyl diphenyl diisocyanate 40-60 parts, terephthaldehyde
Alcohol 5-18 parts, BDO 3-15 parts, 4,4'- diaminourea -3,3'- dichloro diphenyl methane 2-14 parts, di lauric dibutyl
Tin 1-2.5 parts, catalyst DMP-30 1-1.3 parts, bicyclopentadiene dioxide expoxy resin 2-14 parts, polyvinyl chloride 3-10 parts,
Maleic anhydride 2-10 parts, nano-calcium carbonate 3-15 parts, α, alpha, omega-dihydroxy polydimethyl siloxane 2-3.8 parts, 1- oxygen -4-
Methylol -2,6,7- trioxa -1- phosphabicyclos [2.2.2] octane 2-10 parts, phosphonium flame retardant 3-15 parts.
2. high tenacity high flame-retardant polyurethane circuit board material according to claim 1, it is characterised in that the PEPA
For PCDL, polyethylene glycol adipate glycol, polypropylene glycol adipate glycol, polybutylene glyool adipate
In one or more kinds of mixtures.
3. high tenacity high flame-retardant polyurethane circuit board material according to claim 1 or claim 2, it is characterised in that titanium dioxide is bicyclic
The epoxide number of pentadiene epoxy resin is 0.5-0.87.
4. according to high tenacity high flame-retardant polyurethane circuit board material any one of claim 1-3, it is characterised in that described
The average grain diameter of nano-calcium carbonate is 20-45nm.
5. according to high tenacity high flame-retardant polyurethane circuit board material any one of claim 1-4, it is characterised in that described
Phosphonium flame retardant is prepared according to following technique：Pentaerythrite and POCl3 are added in reaction unit, at 70-80 DEG C
Stirring reaction 4-7h, react after terminating through washing, being dried to obtain material A；Methyl p-hydroxybenzoate is added in dioxane,
Material A is stirring evenly and then adding into, the stirring reaction 8-12h at 80-90 DEG C, is reacted after terminating through washing, being dried to obtain described contain
Phosphorus fire retardant.
6. high tenacity high flame-retardant polyurethane circuit board material according to claim 5, it is characterised in that in phosphonium flame retardant
In preparation process, pentaerythrite, the weight ratio of POCl3 are 5-7：30-40.
7. according to the high tenacity high flame-retardant polyurethane circuit board material of claim 5 or 6, it is characterised in that in phosphor-containing flame-proof
In the preparation process of agent, methyl p-hydroxybenzoate, the weight ratio of material A are 11-14：8-17.
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| CN110819100A (en) * | 2019-11-15 | 2020-02-21 | 安徽德科科技有限公司 | High-thermal-stability circuit board material and preparation method thereof |
| CN115403916A (en) * | 2022-05-16 | 2022-11-29 | 上海年与轻科技(集团)有限公司 | Piezoelectric power generation device shell material for chip in shoe and preparation method thereof |
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Application publication date: 20180209 |