CN103275459A - Urea resin foam thermal-insulation composite material and preparation method thereof - Google Patents
Urea resin foam thermal-insulation composite material and preparation method thereof Download PDFInfo
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- CN103275459A CN103275459A CN2013102368032A CN201310236803A CN103275459A CN 103275459 A CN103275459 A CN 103275459A CN 2013102368032 A CN2013102368032 A CN 2013102368032A CN 201310236803 A CN201310236803 A CN 201310236803A CN 103275459 A CN103275459 A CN 103275459A
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Abstract
The invention relates to a urea resin foam thermal-insulation composite material and a preparation method thereof, belongs to the field of foam thermal-insulation composite materials and aims to solve technical problems that conventional urea resin foam cannot be used as a thermal-insulation material for a building due to the fact that urea resin foam is fragile, prone to drop slags and lower in strength and contains trace formaldehyde. The composite material is prepared by urea resin, a foaming agent, a surface active agent, a curing agent, a toughening agent and filler. The preparation method includes steps as follows: raw materials are weighed; the urea resin, the foaming agent and the surface active agent are mixed and stirred, the toughening agent is added and stirred, the filler is added and stirred, the curing agent is added and stirred, and a foaming body is obtained; and the foaming body is poured into a mold preheated in advance and placed in a drying oven for freely foaming, and a product is obtained after foaming is finished. According to the urea resin foam thermal-insulation composite material, the apparent density is 0.093-0.105g/cm<3>, the compression strength is 170-220kPa, the impact strength is 400-530 kPa, the heat conductivity is 0.028-0.036 w/(m*k), and the oxygen index is larger than 33.3%. The urea resin foam thermal-insulation composite material is used for heat preservation of an outer wall of the building.
Description
Technical field
The invention belongs to the foam thermal insulation field of compound material; Be specifically related to urea-formaldehyde resin foam thermal insulation matrix material and preparation method thereof.
Background technology
At present, the main polymer heat preserving material of cellular insulant and litaflex two big classes, the polymer heat preserving material mainly contains polystyrene foam, polyurethane foam and phenolic resin foam, polystyrene foam is low because of its price, heat insulation property is good, water-absorbent is little, water vapour permeability is low, absorb advantages such as impact is good is used for the building heat preservation field in a large number, but its flame retardant resistance is relatively poor, will discharge the polystyrene poisonous gas when being heated to 60 ℃ to environment and human health risk; Polyurethane foam is one of best lagging material of heat-proof quality, also do not absorb water simultaneously, be the thermal-insulating waterproof material of enjoying a double blessing, development in recent years rapidly, but the polyurethane foam flame retardant resistance is relatively poor, discharge a large amount of toxic gases during burning, and price is expensive, improve its flame retardant properties, needs to add a large amount of properties-correcting agent it is carried out modification, this will improve its production cost greatly, reduce other premium properties of polyurethane foam simultaneously; Phenolic resin foam does not need to add fire retardant and just has excellent fireproof performance, toxicity is very little during burning, at present, the a lot of countries in Eastern Europe have extensively adopted phenolic resin foam, progressively substituted polystyrene foam and polyurethane foamed material in certain fields, but the urea-formaldehyde resin foam that compares, the phenolic resin foam production cost is higher.
The urea-formaldehyde resin foam has the performance similar to phenolic resin foam: flame retardant resistance is good, combustion toxicity is lower, high temperature does not have under the molten drop, unit weight is light, thermal conductivity is low etc., but urea-formaldehyde resin foam production cost is lower, it only is about 1/8 of phenol formaldehyde foam, about 1/4 of polystyrene foam, about 1/9 of polyurethane foam.
But the urea-formaldehyde resin spumescence is crisp, easily fall slag, intensity is lower, also contains trace formaldehyde, therefore uses also less in the building heat preservation field.
Summary of the invention
The present invention to solve existing urea-formaldehyde resin foam crisp because of property, easily fall slag, intensity is lower, and contains the technical problem that trace formaldehyde can't use as building thermal insulation material; And provide urea-formaldehyde resin foam thermal insulation matrix material and preparation method thereof.
For solving the problems of the technologies described above, urea-formaldehyde resin foam thermal insulation matrix material of the present invention is made by 74%~97% urea-formaldehyde resin, 0.50%~4% whipping agent, 1%~6% tensio-active agent, 0.50%~4% solidifying agent, 0.1%~2% toughner and 1%~15% filler by weight percentage; The preparation method is specifically finished by following step:
Step 1, take by weighing 74%~97% urea-formaldehyde resin, 0.50%~4% whipping agent, 1%~6% tensio-active agent, 0.50%~4% solidifying agent, 0.1%~2% toughner and 1%~15% filler respectively by weight percentage;
5~10min (make in the reaction system and mix between the raw material) is stirred in step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, whipping agent, tensio-active agent mixing at ambient temperature, add toughner maintenance stirring 10~15min that step 1 takes by weighing subsequently, add filler stirring 10~20min that step 1 takes by weighing again, add solidifying agent that step 1 takes by weighing then and be heated under 30~45 ℃ of temperature and stir 3~5min, obtain foam; In the foam preparation process, temperature is higher than 45 ℃, urea-formaldehyde resin is solidified in advance solidify, and urea-formaldehyde resin can not fully foam; Being lower than 30 ℃ will cause urea-formaldehyde resin foamed composite foams edge and foams center cell size gap bigger.Influence the whole apparent mass of foam.
Step 3, to pour foam into temperature be in 70~85 ℃ the tile mould, then mould placed 70~90 baking oven free foamings, and foaming namely obtains urea-formaldehyde resin foam thermal insulation matrix material after finishing.
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.01~1.45: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0%~1.5% of urea total mass, add the urea that accounts for urea total mass 66%, in 30~45min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃~82 ℃ conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is prepared by 1: 1 volume ratio with formic acid and water) adjusting pH value to 4.7~5.2, be warming up to 91~95 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, add the urea that accounts for urea total mass 16.4%, under 75 ℃ of conditions, react 10min again, regulate pH value to 7.5~8.5 then, be cooled to 40 ℃ again with bottom discharge, namely obtain urea-formaldehyde resin; The urea-formaldehyde resin performance that obtains is as follows: viscosity (being coated with 4 glasss of surveys): 19~25s; Solid content: 49%~53%; Set time: 65~80s; Free formaldehyde content: 0.1%~0.35%.
Described whipping agent is that boiling point is 40~85 ℃ whipping agent.
A kind of in the preferred bicarbonate of ammonia of whipping agent, sodium bicarbonate, yellow soda ash, Skellysolve A, normal hexane, sherwood oil, hexanaphthene, the chloro alkyl thing or wherein several combination; When described whipping agent is composition, press between various whipping agents arbitrarily than mixing.
Described tensio-active agent is anion surfactant or nonionogenic tenside, and anion surfactant is a kind of in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, the allyl polyether vitriol or wherein several combination; Nonionogenic tenside is alkyl alcohol polyethers and/or alkylphenol-polyethenoxy base ether; When described anion surfactant is composition, press between various anion surfactants arbitrarily than mixing.
Described solidifying agent is a kind of in phosphoric acid, tartrate, the citric acid or wherein several combination; When described solidifying agent is composition, press between various solidifying agent arbitrarily than mixing.
Described toughner is carboxymethyl cellulose, nano imvite, glycerol, polyvinyl alcohol or xylogen.
Described filler is fiber or perlite; But a kind of in described fiber old paper stock fiber, xylon and the glass fibre or wherein several combination; The preferred fine perlite of perlite; When described fiber is composition, press between various fibers arbitrarily than mixing.
Urea-formaldehyde resin foam thermal insulation composite material toughness of the present invention and compressive strength are good, and keep premium propertiess such as the original insulation of urea-formaldehyde resin foam, difficult combustion, can directly apply to building exterior wall heat preserving.
The present invention has following benefit:
(1) the urea-formaldehyde resin foam thermal insulation composite technology of the present invention preparation simple, with low cost, take full advantage of waste paper fibre, turn waste into wealth, realize the resource circulation utilization.
(2) the present invention adopts acid and alkali-resistance, ganoid ceramic tile as foaming mould, and the demoulding is easy, with low cost, reusable edible.
(3) product of the present invention has improved intensity and the toughness of urea-formaldehyde resin foam simultaneously, and thermal conductivity is lower, and under 23 ℃ of conditions, thermal conductivity belongs to thermal insulation material between 0.028~0.036w/ (mk).
(4) product flame retardant resistance of the present invention is better, and oxygen index>33.2 belong to difficult combustion lagging material.
(5) performance comparison is as follows before and after the modification of this product:
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but do not limit to so, every technical solution of the present invention is made amendment or is equal to replacement, and do not break away from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment one: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 86% urea-formaldehyde resin, 2% normal hexane, 5% tween-80,2% tartrate (mass concentration is 15%), 2% toughner and 1% old paper stock fiber by weight percentage; Described toughner is made up of 45% carboxymethyl cellulose and 55% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 86% urea-formaldehyde resin, 2% normal hexane, 5% tween-80,2% tartrate (mass concentration is 15%), 2% toughner and 1% old paper stock fiber respectively by weight percentage;
Step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 mix under the room temperature condition of back with 1500 commentaries on classics/min speed mechanical stirring 10min, adding the toughner that step 1 takes by weighing subsequently continues with 1500 commentariess on classics/min speed mechanical stirring 10min, adding the old paper stock fiber that step 1 takes by weighing again continues with 1500 commentariess on classics/min speed mechanical stirring 15min, add then and continue under 15% or tartaric acid for heating to the 40 ℃ temperature that step 1 takes by weighing to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (being preheated to 70 ℃) of prior preheating, then mould is placed 75 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.17: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.096g/cm
3, compressive strength is 201kPa, and shock strength is 420kPa, and thermal conductivity is that 0.031w/ (mk) oxygen index is 33.4%.
Embodiment two: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 89% urea-formaldehyde resin, 1.5% normal hexane, 3% tween-80,2.5% citric acid (mass concentration is 15%), 1.2% toughner and 2.8% old paper stock fiber by weight percentage; Described toughner is made up of 50% carboxymethyl cellulose and 50% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 89% urea-formaldehyde resin, 1.5% normal hexane, 3% tween-80,2.5% citric acid (mass concentration is 15%), 1.2% toughner and 2.8% old paper stock fiber respectively by weight percentage;
After mixing, step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 stir 10min with 1500 commentaries on classics/min speed mechanical at ambient temperature, adding the toughner that step 1 takes by weighing subsequently continues with 1500 commentariess on classics/min speed mechanical stirring 10min, adding the old paper stock fiber that step 1 takes by weighing again continues with 1500 commentariess on classics/min speed mechanical stirring 15min, adding 15% citric acid that step 1 takes by weighing then is heated to 40 ℃ of temperature condition and continues to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (being preheated to 75 ℃) of prior preheating, then mould is placed 75 ℃ of baking oven free foamings, foaming namely obtains urea-formaldehyde resin foam thermal insulation matrix material after finishing.
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.10: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0%~1.5% of urea total mass, add the urea that accounts for urea total mass 66%, in 30~45min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃~82 ℃ conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid (1: 1) conditioned reaction liquid pH value to 4.7~5.2, be warming up to 91~95 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.098g/cm
3, compressive strength is 193kPa, and shock strength is 470kPa, and thermal conductivity is that 0.030w/ (mk) oxygen index is 33.7%.
Embodiment three: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 90% urea-formaldehyde resin, 1% normal hexane, 2.5% tween-80,1.5% citric acid (mass concentration is 15%), 1% toughner and 4% old paper stock fiber by weight percentage; Described toughner is made up of 70% carboxymethyl cellulose and 30% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 90% urea-formaldehyde resin, 1% normal hexane, 2.5% tween-80,1.5% citric acid (mass concentration is 15%), 1% toughner and 4% old paper stock fiber respectively by weight percentage;
After mixing, step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 stir 10min with 1500 commentaries on classics/min speed mechanical at ambient temperature, add the toughner that step 1 takes by weighing subsequently and stir 10min with 1500 commentaries on classics/min speed mechanical, add the old paper stock fiber that step 1 takes by weighing again and stir 15min with 1500 commentaries on classics/min speed mechanical, adding 15% citric acid that step 1 takes by weighing then is heated to and continues under 40 ℃ of temperature to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (preheating temperature is 80 ℃) of prior preheating, then mould is placed 85 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.20: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5S (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.103g/cm
3, compressive strength is 205kPa, and shock strength is 440kPa, and thermal conductivity is that 0.033w/ (mk) oxygen index is 33.3%.
Embodiment four: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is 15% by 85.5% urea-formaldehyde resin, 3% normal hexane, 5% tween-80,3% tartrate mass concentration by weight percentage), 1.5% toughner and 2% old paper stock fiber make; Described toughner is made up of 45% carboxymethyl cellulose and 55% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 85.5% urea-formaldehyde resin, 3% normal hexane, 5% tween-80,3% tartrate (mass concentration is 15%), 1.5% toughner and 2% old paper stock fiber respectively by weight percentage;
After mixing, step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 stir 10min with 1500 commentaries on classics/min speed mechanical at ambient temperature, adding the toughner that step 1 takes by weighing subsequently continues with 1500 commentariess on classics/min speed mechanical stirring 10min, add the old paper stock fiber that step 1 takes by weighing again and stir 15min with 1500 commentaries on classics/min speed mechanical, add then and continue under 15% or tartaric acid for heating to the 40 ℃ temperature that step 1 takes by weighing to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (preheating temperature is 80 ℃) of prior preheating, then mould is placed 85 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.20: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5S (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.093g/cm
3, compressive strength is 190kPa, and shock strength is 490kPa, and thermal conductivity is that 0.032w/ (mk) oxygen index is 33.6%.
Embodiment five: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 88% urea-formaldehyde resin, 2% normal hexane, 3% tween-80,2% tartrate (mass concentration is 15%), 1.5% toughner and 3.5% old paper stock fiber by weight percentage; Described toughner is made up of 60% carboxymethyl cellulose and 40% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 88% urea-formaldehyde resin, 2% normal hexane, 3% tween-80,2% tartrate (mass concentration is 15%), 1.5% toughner and 3.5% old paper stock fiber respectively by weight percentage;
Step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 mix under the room temperature condition of back with 1500 commentaries on classics/min speed mechanical stirring 10min, add the toughner that step 1 takes by weighing subsequently and stir 10min with 1500 commentaries on classics/min speed mechanical, add the old paper stock fiber that step 1 takes by weighing again and stir 15min with 1500 commentaries on classics/min speed mechanical, add then and continue under 15% or tartaric acid for heating to the 40 ℃ temperature that step 1 takes by weighing to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (preheating temperature is 80 ℃) of prior preheating, then mould is placed 85 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.27: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.097g/cm
3, compressive strength is 178kPa, and shock strength is 510kPa, and thermal conductivity is that 0.032w/ (mk) oxygen index is 33.5%.
Embodiment six: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 75% urea-formaldehyde resin, 4% normal hexane, 4% tween-80,2% tartrate (mass concentration is 15%), 1.0% toughner and 14% filler by weight percentage; Described toughner is made up of 65% carboxymethyl cellulose and 35% nano imvite by mass percentage, and described filler is made up of 20% old paper stock fiber and 80%60 purpose pearlstones by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 75% urea-formaldehyde resin, 4% normal hexane, 4% tween-80,2% tartrate (mass concentration is 15%), 1.0% toughner and 14% filler respectively by weight percentage;
After mixing, step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 stir 10min with 1500 commentaries on classics/min speed mechanical at ambient temperature, add the toughner that step 1 takes by weighing subsequently and stir 10min with 1500 commentaries on classics/min speed mechanical, add the filler that step 1 takes by weighing again and stir 15min with 1500 commentaries on classics/min speed mechanical, add then and continue under 15% or tartaric acid for heating to the 40 ℃ temperature that step 1 takes by weighing to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (preheating temperature is 80 ℃) of prior preheating, then mould is placed 85 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.27: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.105g/cm
3, compressive strength is 203kPa, and shock strength is 510kPa, and thermal conductivity is that 0.035w/ (mk) oxygen index is 34.3%.
Embodiment seven: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 82% urea-formaldehyde resin, 2% normal hexane, 3% tween-80,1.5% tartrate (mass concentration is 15%), 1.0% toughner and 10.5%80 purpose pearlstones by weight percentage; Described toughner is made up of 55% carboxymethyl cellulose and 45% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 82% urea-formaldehyde resin, 2% normal hexane, 3% tween-80,1.5% tartrate (mass concentration is 15%), 1.0% toughner and 10.5%80 purpose pearlstones respectively by weight percentage;
After mixing, step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 stir 10min with 1500 commentaries on classics/min speed mechanical at ambient temperature, add the toughner that step 1 takes by weighing subsequently and stir 10min with 1500 commentaries on classics/min speed mechanical, add the pearlstone that step 1 takes by weighing again and stir 15min with 1500 commentaries on classics/min speed mechanical, add then and continue under 15% or tartaric acid for heating to the 40 ℃ temperature that step 1 takes by weighing to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (preheating temperature is 80 ℃) of prior preheating, then mould is placed 85 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.27: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.104g/cm
3, compressive strength is 185kPa, and shock strength is 400kPa, and thermal conductivity is that 0.036w/ (mk) oxygen index is 34.7%.
Embodiment eight: the urea-formaldehyde resin foam thermal insulation matrix material in the present embodiment is made by 87% urea-formaldehyde resin, 2% normal hexane, 3% tween-80,1.5% tartrate (mass concentration is 15%), 1.0% toughner and 5.5%80 purpose pearlstones by weight percentage; Described toughner is made up of 55% carboxymethyl cellulose and 45% nano imvite by mass percentage.
The preparation method is specifically finished by following step:
Step 1, take by weighing 87% urea-formaldehyde resin, 2% normal hexane, 3% tween-80,1.5% tartrate (mass concentration is 15%), 1.0% toughner and 5.5%80 purpose pearlstones respectively by weight percentage;
After mixing, step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, normal hexane, tween-80 stir 10min with 1500 commentaries on classics/min speed mechanical at ambient temperature, add the toughner that step 1 takes by weighing subsequently and stir 10min with 1500 commentaries on classics/min speed mechanical, add the pearlstone that step 1 takes by weighing again and stir 15min with 1500 commentaries on classics/min speed mechanical, add then and continue under 15% or tartaric acid for heating to the 40 ℃ temperature that step 1 takes by weighing to obtain foam with 1500 commentariess on classics/min speed mechanical stirring 5min;
Step 3, foam is poured in the mould (preheating temperature is 80 ℃) of prior preheating, then mould is placed 85 ℃ of baking oven free foamings, foaming finishes namely to obtain urea-formaldehyde resin foam thermal insulation matrix material after (about half hour of foaming process).
Wherein, described urea-formaldehyde resin prepares by following step:
Step a, be that 1.27: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0% of urea total mass, add the urea that accounts for urea total mass 66%, in 40min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃ of ℃ of conditions, be incubated 30min, insulation finishes before measurement pH value, with formic acid solution (formic acid solution is to prepare by 1: 1 volume ratio with formic acid and water) accent reaction solution pH to 4.7~5.2, be warming up to 93 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, adds the urea that accounts for urea total mass 16.4%, reacts 10min under 75 ℃ of conditions, regulates pH value to 7.5~8.5.Be cooled to 40 ℃ with bottom discharge, namely obtain urea-formaldehyde resin.
The urea-formaldehyde resin foam thermal insulation matrix material apparent density that present embodiment obtains is 0.100g/cm
3, compressive strength is 192kPa, and shock strength is 460kPa, and thermal conductivity is that 0.034w/ (mk) oxygen index is 34.3%.
Claims (10)
1. urea-formaldehyde resin foam thermal insulation matrix material is characterized in that what urea-formaldehyde resin foam thermal insulation matrix material was made by 74%~97% urea-formaldehyde resin, 0.50%~4% whipping agent, 1%~6% tensio-active agent, 0.50%~4% solidifying agent, 0.1%~2% toughner and 1%~15% filler by weight percentage.
2. urea-formaldehyde resin foam thermal insulation matrix material according to claim 1 is characterized in that described urea-formaldehyde resin prepares by following step:
Step a, be that 1.01~1.45: 1 proportioning takes by weighing formaldehyde and urea respectively by formaldehyde and urea mol ratio;
Step b, it is 37% formalin that formaldehyde is mixed with mass percent concentration, be pH value to 8.4~8.6 that 30% aqueous sodium hydroxide solution is regulated formalin with mass percent concentration, adding mass percent concentration again is that 25% ammoniacal liquor stirs evenly, ammonia volume is 1.0%~1.5% of urea total mass, add the urea that accounts for urea total mass 66%, in 30~45min, be warming up to 80 ℃, regulate the pH value 6.5~7.3, under 80 ℃~82 ℃ conditions, be incubated 30min, insulation finishes before measurement pH value, be that 1: 1 formic acid solution is regulated pH value to 4.7~5.2 with formic acid and water volume ratio, be warming up to 91~95 ℃ then, insulation reaction is to till being coated with 4 glasss of viscosimetrics and being 17.5~18.5s (30 ℃);
Step c, be that 30% aqueous sodium hydroxide solution is regulated pH value to 5.3~5.6 with mass percent concentration immediately, fast cooling to 78 ℃ adds the urea that accounts for urea total mass 17.6% simultaneously, treats to react 30min after the urea dissolving under 75 ℃ of conditions;
Steps d, mass percent concentration is that 30% sodium hydroxide is transferred reacting liquid pH value to 7.0~7.5 then, add the urea that accounts for urea total mass 16.4%, under 75 ℃ of conditions, react 10min again, regulate pH value to 7.5~8.5 then, be cooled to 40 ℃ again with bottom discharge, namely obtain urea-formaldehyde resin.
3. urea-formaldehyde resin foam thermal insulation matrix material according to claim 1 is characterized in that described whipping agent is that boiling point is 40~85 ℃ whipping agent.
4. urea-formaldehyde resin foam thermal insulation matrix material according to claim 3 is characterized in that described whipping agent is a kind of in bicarbonate of ammonia, sodium bicarbonate, yellow soda ash, Skellysolve A, normal hexane, sherwood oil, hexanaphthene, the chloro alkyl thing or wherein several combination.
5. urea-formaldehyde resin foam thermal insulation matrix material according to claim 1, it is characterized in that described tensio-active agent is anion surfactant or nonionogenic tenside, anion surfactant is a kind of in sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, the allyl polyether vitriol or wherein several combination; Nonionogenic tenside is alkyl alcohol polyethers and/or alkylphenol-polyethenoxy base ether.
6. urea-formaldehyde resin foam thermal insulation matrix material according to claim 1 is characterized in that described solidifying agent is a kind of in phosphoric acid, tartrate, the citric acid or wherein several combination.
7. urea-formaldehyde resin foam thermal insulation matrix material according to claim 1 is characterized in that described toughner is Walocel MT 20.000PV, nano imvite, glycerol, polyvinyl alcohol or xylogen.
8. urea-formaldehyde resin foam thermal insulation matrix material according to claim 1 is characterized in that described filler is fiber or perlite.
9. urea-formaldehyde resin foam thermal insulation matrix material according to claim 8 is characterized in that described fiber is a kind of in old paper stock fiber, xylon and the glass fibre or wherein several combination; Perlite is fine perlite.
10. the preparation method of urea-formaldehyde resin foam thermal insulation matrix material according to claim 1 is characterized in that urea-formaldehyde resin foam thermal insulation composite material and preparation method thereof finished by following step:
Step 1, take by weighing 74%~97% urea-formaldehyde resin, 0.50%~4% whipping agent, 1%~6% tensio-active agent, 0.50%~4% solidifying agent, 0.1%~2% toughner and 1%~15% filler respectively by weight percentage;
5~10min (make in the reaction system and mix between the raw material) is stirred in step 2, the urea-formaldehyde resin that earlier step 1 is taken by weighing, whipping agent, tensio-active agent mixing at ambient temperature, add toughner maintenance stirring 10~15min that step 1 takes by weighing subsequently, add filler stirring 10~20min that step 1 takes by weighing again, add solidifying agent that step 1 takes by weighing then and be heated under 30~45 ℃ of temperature and stir 3~5min, obtain foam;
Step 3, to pour foam into temperature be in 70~85 ℃ the tile mould, then mould placed 70~90 baking oven free foamings, and foaming namely obtains urea-formaldehyde resin foam thermal insulation matrix material after finishing.
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