CN105199310B - A kind of phenolic foam warming plate with core shell structure and preparation method thereof - Google Patents

A kind of phenolic foam warming plate with core shell structure and preparation method thereof Download PDF

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CN105199310B
CN105199310B CN201510545264.XA CN201510545264A CN105199310B CN 105199310 B CN105199310 B CN 105199310B CN 201510545264 A CN201510545264 A CN 201510545264A CN 105199310 B CN105199310 B CN 105199310B
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parts
reactor
foam
phenolic
phenolic resin
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CN105199310A (en
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葛铁军
肖尚雄
王佳
陈瑞杰
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Shenyang University of Chemical Technology
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Abstract

A kind of phenolic foam warming plate with core shell structure and preparation method thereof, is related to a kind of warming plate and preparation method thereof, and material surface composition of the present invention is phenol formaldehyde foam, and sandwich layer is polyurethane foam.Mass ratio is 100 parts of phenolic resin system;20 parts of base polyurethane prepolymer for use as system;Foamed under predetermined synthesis technique via in mould, be molded by solidification, curing, can obtain the phenolic foam warming plate of good-toughness, overcome traditional toughness reinforcing method to sacrifice the phenolic foam sheet with certain toughness that anti-flammability is obtained as cost.And its flexibility is imparted phenolic resin by sandwich layer polyurethane foam so that its thermal conductivity factor is further reduced, while also add the water resistance of phenolic foam board.It can be used as heat-insulation and heat-preservation, acoustic material.

Description

A kind of phenolic foam warming plate with core shell structure and preparation method thereof
Technical field
The present invention relates to a kind of warming plate and preparation method thereof, more particularly to a kind of phenolic foam with core shell structure Warming plate and preparation method thereof.
Background technology
Phenolic resin is from starting to mass produce into product, always with heat-resist, high mechanical strength, electrical insulating property and resistance to The advantages of high temperature wriggling is excellent, is widely used in fields such as electrician, aviation, building and space flight.
Phenol formaldehyde foam generally by resol, surfactant, foaming agent, it is well mixed after add curing agent, Generally there is density height in foamable after stirring, the phenol formaldehyde foam formed, fragility is big, and water absorption rate height etc. lacks Fall into, so the phenolic resin that phenolic foam foaming is used needs to use flexible material to be modified, to solve the portion of phenol formaldehyde foam Divide defect.The phenol formaldehyde foam of foaming preparation is carried out by modified phenolic resin, its fragility can have some improvement.
Publication No. CN201510039644 application for a patent for invention, under agitation, 0.2g resorcinols are dissolved In deionized water, the resorcinol aqueous solution that concentration is 0.06 ~ 0.12mol/L, i.e. reaction solution is made, the reaction solution is put In -5 DEG C ~ 5 DEG C cryostats;B, to(a)Middle addition 4 ~ 15mL absolute ethyl alcohols;C, stirring 2min are backward(b)Middle addition formaldehyde Solution;D, stirring 2min are backward(c)Middle addition ammoniacal liquor;E, 24 ~ 48h of stirring, obtain milky white solution, centrifuge, freeze-drying The phenolic resin of microcosmic core shell structure is produced afterwards, and the phenolic resin toughness has a small amount of raising, but fire resistance and thermal insulation are corresponding Reduction.
Publication No. CN201510164958 application for a patent for invention, describes a kind of phenolic resin and base polyurethane prepolymer for use as Composite foam material and preparation method.The material composition and quality proportioning are phenolic resin:Base polyurethane prepolymer for use as:Closed perlite:Table Face activating agent:Foaming agent:Curing agent=1:0.05-0.25:0.10-0.30:0.02-0.06:0.05-0.15:0.80-0.15 ; Phenolic resin is mixed with base polyurethane prepolymer for use as and various auxiliary agents, then after being mixed with closed perlite, inputs mould It is interior, it is molded by foaming, solidification, curing.The anti-flammability of the light weight of the material, good toughness, but phenolic resin has certain reduction.
Therefore, needing a kind of modified pnenolic aldehyde foam material of excellent performance in a hurry, make while its fire resistance is ensured It possesses good mechanical property, relatively low manufacturing cost and simple technological process, is conveniently used for fireproof heat insulating field.
The content of the invention
It is an object of the invention to provide a kind of phenolic foam warming plate with core shell structure and preparation method thereof, the party Method solves the shortcoming of traditional low frangibility of phenol formaldehyde foam toughness in technique.This core shell structure structure phenolic aldehyde cystosepiment is by poly- ammonia The sets of advantages of ester foam and phenol formaldehyde foam is together with, and the presence of the phenol formaldehyde foam of extexine overcomes conventional polyurethane foams plate The shortcoming of poor fire, and due to the presence of sandwich layer polyurethane foam, the cost of phenol formaldehyde foam is not only reduced, improve heat conduction Coefficient, further improves the toughness of traditional phenol formaldehyde foam.This synthesis technique is reasonable, it is easy to industrialized production.
The purpose of the present invention is achieved through the following technical solutions:
A kind of phenolic foam warming plate with core shell structure, the warming plate outer layer is phenolic resin foam and sandwich layer is The core shell structure phenolic aldehyde composition of polyurethane foam:
Wherein:100 parts of phenolic resin foam;10-30 parts of base polyurethane prepolymer for use as foam;
Phenolic resin foam is by phenol, paraformaldehyde, sodium hydroxide, surfactant, foaming agent, curing agent and nucleator It is made:
100 parts of phenol;50-70 parts of paraformaldehyde;2-5 parts of sodium hydroxide;10-15 parts of surfactant;Foaming agent 8-20 Part;12-20 parts of curing agent;1-5 part of nucleator;
The pre- foam of polyurethane is made by polymer polyatomic alcohol, isocyanates, nucleator, foam stabilizer, foaming agent and catalyst:
100 parts of polymer polyatomic alcohol;10-20 parts of diisocyanate;0.1-0.3 parts of catalyst;2 parts of foam stabilizer;Foaming agent 12-14 parts.
A kind of described phenolic foam warming plate with core shell structure, the phenolic resin foam surfactant is to tell One or more in temperature -80, silicone oil.
A kind of described phenolic foam warming plate with core shell structure, the phenolic resin foam foaming agent is positive penta One or more in alkane, isopentane, petroleum ether and dichloromethane.
A kind of described phenolic foam warming plate with core shell structure, the phenolic resin foam curing agent is to hydroxyl One or more in benzene sulfonic acid, phosphoric acid, hydrochloric acid.
A kind of described phenolic foam warming plate with core shell structure, the phenolic resin foam nucleator is micron order Spherical Al2O3 particles, 10 ~ 200 μm of particle diameter, and nano level spherical silica particles, the nm of particle diameter < 100, in one kind or It is a variety of.
A kind of described phenolic foam warming plate with core shell structure, the polyurethane foam degree of functionality is that 2, number is divided equally The polymer polyatomic alcohol that son amount is 2000 is the one or more in PEA2000, PCL2000, PPG2000, PTMG2000.
A kind of described phenolic foam warming plate with core shell structure, the polyurethane foam degree of functionality for 2 it is two different Cyanate is the one or more in TDI-80, TDI-100, MDI-100, MDI-50, liquefied mdi.
A kind of described phenolic foam warming plate with core shell structure, the polyurethane foam catalyst is dibutyl two One or more in tin laurate, triethylenediamine, triethanolamine.
A kind of described phenolic foam warming plate with core shell structure, the polyurethane foam foam stabilizer is Tween-80.
A kind of phenolic foam warming plate with core shell structure and preparation method thereof, the described method comprises the following steps:
(1)Reactor A and C are equipped with phenolic resin component in mass ratio, and reactor B is equipped with base polyurethane prepolymer for use as in mass ratio Component, the shower nozzle of 3 reactors is arranged in order above conveyer belt by same intervals;
(2)After conveyer belt is started, reactor A is first begin to the phenolic resin of lasting ejection Rack and specific thickness In on conveyer belt, when resin is transported to conveyer belt below reactor B after the several seconds, the time depending on the specific speed of conveyer belt, instead Kettle B is answered to start the base polyurethane prepolymer for use as of lasting ejection Rack and specific thickness, when resin with conveyer belt is transported to reactor C During lower section, reactor C starts the phenolic resin of lasting ejection Rack and specific thickness on conveyer belt, now on conveyer belt Transport has outer layer to be the prefoam system that phenolic aldehyde internal layer is polyurethane, is foamed into insulating box.
Advantages of the present invention is with effect:
The present invention with the addition of nucleator in phenolic resin, improve the expansion ratio of phenolic resin, to prevent sandwich layer from gathering Urethane makes phenol formaldehyde foam split because expansion ratio is too high.After addition nucleator substantial amounts of bubble can be formed in phenolic resin A large amount of fine and closely woven uniform minute bubbles can be formed in core, melt, abscess densification, the small phenol formaldehyde foam of apparent density is ultimately formed.Add The Added Nucleating Agents effect that also restricted foaming agent volatilizees, foaming agent is not volatile, so as to improve the utilization rate of foaming agent, therefore The foam of high foamability can be obtained.And be that abscess is big, quantity is few, foaming without what is obtained in the phenolic resin of nucleator The low foam of multiplying power.
The present invention improves its toughness by synthesizing the phenolic foam board with core shell structure, obtains the toughness for being modified foam To greatly improving, while thermal conductivity factor, water absorption rate and combination property are obtained for improvement.The raising of toughness is due to poly- ammonia Its flexibility is imparted phenolic resin by ester foam, and thermal conductivity factor is further reduced, while also add phenol formaldehyde foam The water resistance of plate.Flexible base polyurethane prepolymer for use as and phenolic resin are foamed simultaneously, mutual shape in the foam of both joints Into the structure of interpenetrating networks, the degree of engagement of polyurethane and phenol formaldehyde foam is improved, while so that rigid phenol formaldehyde foam has Flexibility, cost reduction by 20% ~ 30%.And the toughness of whole cystosepiment is also improved, reduction volume phenol formaldehyde foam is in use The possibility of fracture.Phenolic foam heat insulation plate with core shell structure is better than traditional toughener method part and is, the polyurethane of sandwich layer The oxygen index (OI) of top layer phenolic resin is not reduced, and traditional toughener method is to sacrifice anti-flammability as cost.
Brief description of the drawings
Fig. 1 is three reactors square location drawing on a moving belt;
In figure:Reactor A, B, C are followed successively by from left to right;
Fig. 2 is conveyer belt stereogram;
Fig. 3 is the ideally cross section accompanying drawing of resin on a moving belt;
In figure:Internal layer is base polyurethane prepolymer for use as, and outer layer is phenolic resin.
Embodiment
With reference to embodiment, the present invention is described in detail.
Embodiment 1
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:30:1 adds in reactor, 60 DEG C of bath temperature Solid polyformaldehyde is added in batches, control half an hour adds, continue to react half an hour, increase the temperature to 90 DEG C, continue Reaction 1.5 hours, that is, obtain phenolic resin.Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, foaming agent pentane 15 Part, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by.
(2)Take poly- hexanedioic acid glycol ester glycol(PEA2000)100 parts, toluene di-isocyanate(TDI)(TDI-80)10 parts, two Butyl tin dilaurate tin(DBTDL)In 0.1 part of addition reactor, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C.Take 100 parts of base polyurethane prepolymer for use as, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by.
(3)Fill to fill in the phenolic resin as made from step 1, reactor B in reactor A and C and gather as made from step 2 Urethane performed polymer, 3 reactors are arranged in conveyer belt by interval 0.5m(Width is 1m, and groove depth is more than 0.1m, and speed is 1m/ min)Top.After conveyer belt is started, it is the phenolic resin that 1m thickness is 0.03m that reactor A, which is first begin to lasting ejection width, In on conveyer belt, after 30 seconds when resin is transported to conveyer belt below reactor B, reactor B starts lasting ejection width and is 0.5m thickness is 0.04m base polyurethane prepolymer for use as, after after 30 seconds when resin is transported to below reactor C with conveyer belt, instead Answer kettle C start lasting ejection width be 1m thickness be 0.03m phenolic resin on conveyer belt, now being transported on conveyer belt has outer Layer is the prefoam system that phenolic aldehyde internal layer is polyurethane, is foamed into insulating box.Reactor A, B, C spray the quality of liquid Than for 2:1:2.The thermal insulation foaming 10min at a temperature of 50 DEG C, is warming up to 80 DEG C, solidifies 10min, obtains the phenol of core shell structure Urea formaldehyde expanded material.
Embodiment 2
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:35:1 adds in reactor, 60 DEG C of bath temperature Solid polyformaldehyde is added in batches, control half an hour adds, continue to react half an hour, increase the temperature to 90 DEG C, continue Instead
Answer 1.5 hours, that is, obtain phenolic resin.Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, foaming agent just 15 parts of pentane, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by.
(2)Take poly- hexanedioic acid glycol ester glycol(PEA2000)100 parts, toluene di-isocyanate(TDI)(TDI-80)10 parts, two Butyl tin dilaurate tin(DBTDL)In 0.1 part of addition reactor, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C.Take 100 parts of base polyurethane prepolymer for use as, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by.
(3)The step of be the same as Example 1 the 3rd.
Embodiment 3
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:40:1 adds in reactor, 60 DEG C of bath temperature Solid polyformaldehyde is added in batches, control half an hour adds, continue to react half an hour, increase the temperature to 90 DEG C, continue Reaction 1.5 hours, that is, obtain phenolic resin.Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, foaming agent pentane 15 Part, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by.
(2)Take poly- hexanedioic acid glycol ester glycol(PEA2000)100 parts, toluene di-isocyanate(TDI)(TDI-80)10 parts, two Butyl tin dilaurate tin(DBTDL)In 0.1 part of addition reactor, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C.Take 100 parts of base polyurethane prepolymer for use as, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by.
(3)The step of be the same as Example 1 the 3rd.
Embodiment 4
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:35:1 adds in reactor, 60 DEG C of bath temperature Solid polyformaldehyde is added in batches, control half an hour adds, continue to react half an hour, increase the temperature to 90 DEG C, continue Reaction 1.5 hours, that is, obtain phenolic resin.Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, foaming agent pentane 15 Part, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by.
(2)Take poly- hexanedioic acid glycol ester glycol(PEA2000)100 parts, toluene di-isocyanate(TDI)(TDI-80)10 parts, two Butyl tin dilaurate tin(DBTDL)In 0.1 part of addition reactor, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C.Take 100 parts of base polyurethane prepolymer for use as, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by.
(3)The step of be the same as Example 1 the 3rd.
Embodiment 5
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:35:1 adds in reactor, 60 DEG C of bath temperature Solid polyformaldehyde is added in batches, control half an hour adds, continue to react half an hour, increase the temperature to 90 DEG C, continue Reaction 1.5 hours, that is, obtain phenolic resin.Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, foaming agent pentane 15 Part, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by.
(2)Take poly- hexanedioic acid glycol ester glycol(PEA2000)100 parts, toluene di-isocyanate(TDI)(TDI-80)15 parts, two Butyl tin dilaurate tin(DBTDL)In 0.1 part of addition reactor, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C.Take 100 parts of base polyurethane prepolymer for use as, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by.
(3)The step of be the same as Example 1 the 3rd.
Embodiment 6
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:35:1 adds in reactor, 60 DEG C of bath temperature Solid polyformaldehyde is added in batches, control half an hour adds, continue to react half an hour, increase the temperature to 90 DEG C, continue Reaction 1.5 hours, that is, obtain phenolic resin.Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, foaming agent pentane 15 Part, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by.
(2)Take poly- hexanedioic acid glycol ester glycol(PEA2000)100 parts, toluene di-isocyanate(TDI)(TDI-80)20 parts, two Butyl tin dilaurate tin(DBTDL)In 0.1 part of addition reactor, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C.Take 100 parts of base polyurethane prepolymer for use as, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by.
(3)The step of be the same as Example 1 the 3rd.
Comparative example
The performance comparison of phenol formaldehyde foam and common anacardol phenol formaldehyde foam prepared by the embodiment of the present invention 1 to 6 is as follows Table:
Table
Bending Deformation mm Compressive strength MPa Volume water absorption rate %
Embodiment 1 12.19 1.010 4.3
Embodiment 2 16.35 1.026 5.3
Embodiment 3 14.84 1.008 4.8
Embodiment 4 13.71 1.013 4.9
Embodiment 5 14.16 1.014 5.1
Embodiment 6 12.41 1.016 5.0
Basis contrast 5.19 0.089 9.2
As seen from the above table, the toughness of core shell structure phenol formaldehyde foam of the invention is greatly improved, and density rises, water absorption rate Reduction, the combination property of product is improved.This is due to that its flexibility is imparted phenolic resin by polyurethane foam, and causes heat conduction Coefficient is further reduced, while the water resistance of phenolic foam board is also add, cost reduction by 20% ~ 30%.
What is changed in embodiment 1,2,3 is the mass ratio of phenol, paraformaldehyde and sodium hydroxide, from result, quality Than 65:35:Effect is best when 1.What is changed in embodiment 4,5,6 is poly- hexanedioic acid glycol ester glycol, toluene di-isocyanate(TDI) With the mass ratio of dibutyl tin dilaurate, from result, mass ratio is 100:15:Effect is best when 0.1.

Claims (1)

1. a kind of preparation method of the phenolic foam warming plate with core shell structure, it is characterised in that methods described includes following Step:
(1)By phenol, paraformaldehyde, sodium hydroxide, in mass ratio 65:35:1 adds in reactor, and 60 DEG C of bath temperature is in batches Amount adds solid polyformaldehyde, and control half an hour adds, and continues to react half an hour, increases the temperature to 90 DEG C, sustained response 1.5 hours, that is, obtain phenolic resin;Take 100.0 parts of phenolic resin, 6.0 parts of surfactant, 15 parts of foaming agent pentane, 15 parts of curing agent, 1 part of nucleator, mix, stir it is stand-by;
(2)Take 100 parts of polyethylene glycol adipate glycol PEA2000,15 parts of toluene di-isocyanate(TDI) TDI-80, dibutyl two In 0.1 part of addition reactor of tin laurate DBTDL, base polyurethane prepolymer for use as is made in vacuum reaction 1h at 80 DEG C;Take polyurethane 100 parts of performed polymer, 2 parts of foam stabilizer, 12 parts of foaming agent, mix, stir it is stand-by;
(3)Filled in reactor A and C by step(1)Filled in obtained phenolic resin, reactor B by step(2)It is obtained poly- Urethane performed polymer, 3 reactors are arranged in above conveyer belt by interval 0.5m, and the width of conveyer belt is 1m, and groove depth is more than 0.1m, Speed is 1m/min;After conveyer belt is started, it is the phenolic aldehyde that 1m thickness is 0.03m that reactor A, which is first begin to lasting ejection width, Resin is on conveyer belt, and after 30 seconds when resin is transported to conveyer belt below reactor B, it is wide that reactor B starts lasting ejection Degree is the base polyurethane prepolymer for use as that 0.5m thickness is 0.04m, after after 30 seconds when resin is transported to below reactor C with conveyer belt When, reactor C start lasting ejection width be 1m thickness be 0.03m phenolic resin on conveyer belt, now transported on conveyer belt It is the prefoam system that phenolic aldehyde internal layer is polyurethane to send outer layer, is foamed into insulating box;
The mass ratio that reactor A, B, C spray liquid is 2:1:2;Thermal insulation foaming 10min, is warming up to 80 at a temperature of 50 DEG C DEG C, solidify 10min, obtain the Foaming of phenolic resin warming plate of core shell structure.
CN201510545264.XA 2015-08-31 2015-08-31 A kind of phenolic foam warming plate with core shell structure and preparation method thereof Active CN105199310B (en)

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Publication number Priority date Publication date Assignee Title
CN105601856B (en) * 2016-02-15 2018-09-28 安徽美克思科技有限公司 A kind of preparation method of isocyanate-modified phenolic resin foam
CN112063157A (en) * 2020-09-20 2020-12-11 深圳市知猪互联科技有限公司 Preparation process of high-flame-retardant polyurethane foam heat-insulation material
CN113462119A (en) * 2021-08-12 2021-10-01 北海市传创环保科技有限公司 Heat-insulation and heat-preservation plastic and preparation method thereof

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AU1304083A (en) * 1982-04-22 1983-10-27 W.R. Grace & Co. Foam laminate with acoustic constraining layer
CN101735553A (en) * 2010-01-07 2010-06-16 上海雅达特种涂料有限公司 Material for manufacturing modified phenolic fireproof insulating plate
CN202577625U (en) * 2012-03-26 2012-12-05 北京建筑技术发展有限责任公司 Composite insulation board with organic materials coated by inorganic materials
CN203049814U (en) * 2013-02-01 2013-07-10 万华节能科技集团股份有限公司 Building heat preservation composite board
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DE2130279A1 (en) * 1971-06-18 1972-12-21 Lentia Gmbh Laminated short ski - with polyurethane foam core and plastic covering layers bonded to fibreglass laminates
AU1304083A (en) * 1982-04-22 1983-10-27 W.R. Grace & Co. Foam laminate with acoustic constraining layer
CN101735553A (en) * 2010-01-07 2010-06-16 上海雅达特种涂料有限公司 Material for manufacturing modified phenolic fireproof insulating plate
CN202577625U (en) * 2012-03-26 2012-12-05 北京建筑技术发展有限责任公司 Composite insulation board with organic materials coated by inorganic materials
CN103374196A (en) * 2012-04-24 2013-10-30 合肥杰事杰新材料股份有限公司 Flame retardant toughening phenolic foam and preparation method thereof
CN203049814U (en) * 2013-02-01 2013-07-10 万华节能科技集团股份有限公司 Building heat preservation composite board

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