CN102898778A - Preparation method for melamine formaldehyde resin closed-cell foam - Google Patents

Preparation method for melamine formaldehyde resin closed-cell foam Download PDF

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Publication number
CN102898778A
CN102898778A CN201210328428XA CN201210328428A CN102898778A CN 102898778 A CN102898778 A CN 102898778A CN 201210328428X A CN201210328428X A CN 201210328428XA CN 201210328428 A CN201210328428 A CN 201210328428A CN 102898778 A CN102898778 A CN 102898778A
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foam
formaldehyde resin
terpolycyantoamino
preparation
closed
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CN102898778B (en
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杨斌峰
朱国清
沈铁清
马立新
姚尧
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NANTONG ZIXIN INDUSTRIAL CO LTD
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NANTONG ZIXIN INDUSTRIAL CO LTD
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Abstract

The present invention discloses a preparation method for melamine formaldehyde resin closed-cell foam. The preparation method comprises the following steps: introducing a modifier to a melamine formaldehyde resin synthesis process to carry out copolymerization, and carrying out a dehydration treatment on the synthesized resin to obtain a modified melamine formaldehyde solid resin with a solid content of more than 85%; adding a viscosity adjusting agent, dissolving the solid resin, respectively adding a curing agent, a foam stabilizer, an emulsifier and a foaming agent, and uniformly stirring; placing the resulting mixture in an oven or a microwave oven to carry out foaming to achieve a predetermined density; and placing the resulting material in the oven or the microwave oven to carry out aging to obtain the melamine formaldehyde foam with a closed-cell rate of more than 90%. The melamine formaldehyde resin closed-cell foam produced by the preparation method has excellent mechanical strength and flame retardant property, and can be applicable for building exterior wall thermal insulation.

Description

A kind of preparation method of terpolycyantoamino-formaldehyde resin closed-cell foam
Technical field
The present invention relates to a kind of preparation method who can be used for the terpolycyantoamino-formaldehyde resin closed-cell foam material of various building exterior wall heat preservings, belong to field of new.
Background technology
In various organic resin foam materialss, the terpolycyantoamino-formaldehyde resin foam materials has good flame retardant properties, thermostability, low smokiness, high ageing-resistant performance.In recent years, domestic universities and colleges are to the exploitation pay attention to day by day of terpolycyantoamino-formaldehyde resin foam.
From domestic external, producing at present terpolycyantoamino-formaldehyde resin foam materials enterprise has German BASF, and Japan is aboveground, largeization of Central Plains, Henan, Sichuan petrochemical industry, and the terpolycyantoamino-formaldehyde resin foam principal item of its production is the terpolycyantoamino-formaldehyde resin open celled foam.This terpolycyantoamino-formaldehyde resin open celled foam has been successfully applied to automobile, rail vehicle, kino, public place and has used as sound-proof material.But use has no report as architecture exterior wall insulating materials.Analyze the high opening rate that its major cause is the terpolycyantoamino-formaldehyde resin foam, cause its effect of heat insulation not as materials such as polyurethane foam, polystyrene foam, phenolic resin foams, and also there is the shortcoming of easy efflorescence in the terpolycyantoamino-formaldehyde resin foam, and the terpolycyantoamino-formaldehyde resin foamy body that makes can not satisfy the required basic demand of external-wall heat-insulation material.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of terpolycyantoamino-formaldehyde resin closed-cell foam, the terpolycyantoamino-formaldehyde resin closed-cell foam material for preparing has high mechanical property and flame retardant properties, can be used for building exterior wall heat preserving.
To achieve these goals, the technical solution used in the present invention is: a kind of preparation method of terpolycyantoamino-formaldehyde resin closed-cell foam is characterized in that comprising the steps:
1), in the terpolycyantoamino-formaldehyde resin building-up process, introduce the properties-correcting agent copolymerization, then through processed, obtain solids content and be higher than 85% modified melamine-formaldehyde solid resin;
2), with step 1) the modified melamine-formaldehyde solid resin that obtains adds adjusting adhesive, after the dissolving, adds respectively solidifying agent, foam stabilizer, emulsifying agent, whipping agent, stir; Each material addition adds adjusting adhesive 10 ~ 200g, solidifying agent 5 ~ 200g, foam stabilizer 5 ~ 10g, emulsifying agent 5 ~ 10g, whipping agent 5 ~ 30g take the modified melamine-formaldehyde solid resin as reference in every 200g modified melamine-formaldehyde solid resin;
3), with step 2) mixture put into microwave or baking oven foams, after reaching predetermined density 36 ~ 100kg/cm3, again foam is transferred in the baking oven, under 100-120 degree condition slaking 3-30 minute, obtain the terpolycyantoamino-formaldehyde resin closed-cell foam, rate of closed hole is 94.9 ~ 98.3%, and oxygen index is 30.0 ~ 35.2, thermal conductivity is 0.022 ~ 0.031, compression performance 156.1 ~ 198.7kPa.
Step 1) detailed process is: formaldehyde is packed in the reactor, stir with agitator, add a small amount of caustic soda, adjust pH8.0 ~ 10.0, add the buffer reagent trolamine, be warmed up to 50 degree with temperature controller simultaneously, add trimeric cyanamide, then add the properties-correcting agent copolyreaction after 60 minutes, vacuum hydro-extraction is kept below dehydration temperaturre 100 degree, until solids content is higher than 85%, cooling gets the modified melamine-formaldehyde solid resin.The properties-correcting agent add-on be the trimeric cyanamide consumption 10~95% between (weight ratio).
Described properties-correcting agent is one or more in phenol, benzoguanamine, first substituted melamine, polyester, polyethers, the Dyhard RU 100.
Described adjusting adhesive is one or more in ethylene glycol, glycol ether, diglycolamine, thanomin, butanolamine, diethanolamine, methyl alcohol, ethanol, butanols, triglycol, trolamine, the low molecular weight polycaprolactone ether compound (molecular weight is less than 2000).
Described solidifying agent be in formic acid, acetic acid, sulfuric acid, phosphoric acid, tosic acid, hexanodioic acid, oxalic acid, hydrochloric acid, tolylene diisocyanate (TDI), diphenylmethanediisocyanate (MDI), the polymethylene multi-phenenyl isocyanate (PAPI) one or more.
Described foam stabilizer be in organosilicon and the poly organic silicon one or more.
Described emulsifying agent is one or more in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, the alkylphenol polyoxyethylene (OP-10).
Described whipping agent is one or more in butane, Skellysolve A, normal hexane, hexanaphthene, pentamethylene, sherwood oil, ethylene dichloride, dichlorotrifluoroethane (HCFC-123), dichloro one fluoroethane (HCFC-141b), the chlorodifluoroethane.
Prepared foam has high rate of closed hole, is the terpolycyantoamino-formaldehyde resin closed-cell foam.Can be used for building exterior wall heat preserving.
The ultimate principle that the present invention prepares the terpolycyantoamino-formaldehyde resin closed-cell foam is:
Adopt the modified melamine-formaldehyde solid resin to foam, reduce the moisture content in the terpolycyantoamino-formaldehyde resin, improve the rate of closed hole of terpolycyantoamino-formaldehyde resin foam, reduce the thermal conductivity of terpolycyantoamino-formaldehyde resin foam.
Adopt properties-correcting agent to improve water repelling property, dimensional stability and the flexility of foam, the fragility that solves the terpolycyantoamino-formaldehyde resin foam is large, and ultimate compression strength is low, the dry linting serious problems.
Adopt adjusting adhesive can allow the melamino-formaldehyde solid resin fully dissolve, obtain the resin solution of appropriate viscosity.Prevent that viscosity is excessive, the foam density of generation is excessive, even can't foam; Prevent that the too small whipping agent that causes of viscosity from escaping in heat-processed, even the foam bubble phenomenon of collapsing occurs.The solvent based compound that preferential selection has the well blend ability with resin.
Solidifying agent is the key factor of foam size stability, under the precondition that guarantees resin solidification speed, answers its usage quantity of reduce, reduces the corrosive nature to base material.
Beneficial effect: the preparation method of terpolycyantoamino-formaldehyde resin closed-cell foam provided by the invention, simple to operate, by add different adjusting adhesive, solidifying agent, foam stabilizer, emulsifying agent, whipping agent on modified melamine-formaldehyde solid resin basis, the terpolycyantoamino-formaldehyde resin closed-cell foam that foam, slaking production obtains having high rate of closed hole, the fragility that can solve the terpolycyantoamino-formaldehyde resin foam is large, ultimate compression strength is low, the dry linting serious problems, the gained foam can be used for building exterior wall heat preserving.
Embodiment
The embodiment of the invention given below just is further described specifically the present invention.It is important to point out, embodiment only for the present invention is further elaborated, can not be interpreted as limiting the scope of the invention.The present embodiment is done an amount of improvement or change, still belong to protection scope of the present invention.
Embodiment one
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust pH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product), 1052 grams, after adding phenol 200 grams, Dyhard RU 100 100 grams are reacted to 60 minutes, vacuum hydro-extraction, keep below dehydration temperaturre 100 degree, until solids content reaches 89.2%, cooling gets the modified melamine-formaldehyde solid resin.
Above-mentioned solid resin 200 grams are added adjusting adhesive ethylene glycol 10 grams, after the dissolving, add again solidifying agent phosphoric acid 20 grams, emulsifier sodium lauryl sulfate 5 grams, foam stabilizer organosilicon AK8805 10 grams (Nanjing dolantin generation wound company limited), whipping agent Skellysolve A 10 grams, strong stirring hybrid resin 5 minutes.Put into microwave and foam, reach predetermined density 36 ~ 100kg/cm3 after, change again baking oven slaking 5 minutes under 120 degree conditions over to, obtain closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 45.1kg/cm3, rate of closed hole 95.3%, and oxygen index: 35.2, thermal conductivity is 0.031, compression performance 175kPa(deformation 10%).
Embodiment two
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product) 1052 gram, add benzoguanamine 200 grams, add Dyhard RU 100 100 grams, be reacted to one hour after, beginning dehydration below 100 degree, until solids content reaches 87.7%, cooling gets the modified melamine-formaldehyde solid resin.
Above-mentioned solid resin 200 grams are added adjusting adhesive glycol ether 10 grams, ethylene glycol 10 grams, after the dissolving, add again solidifying agent formic acid 20 grams, emulsifier sodium lauryl sulfate 5 grams, foam stabilizer organosilicon 580# 5 grams (Jiangsu Yoke Technology Co., Ltd.), whipping agent ethylene dichloride 5 grams, stir.Mixture is put into microwave foams, reach predetermined density after, change again baking oven slaking 15 minutes under 120 degree conditions over to, obtain closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 53.5kg/cm3, rate of closed hole, and 97.6%, oxygen index: 32.1, thermal conductivity is 0.025, compression performance 156.1kPa(deformation 10%).
Embodiment three
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 10 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product), 1052 grams, add first substituted melamine 200 grams, polyethers 204# 100 grams [Nantong Lv Yuan novel material company limited], after being reacted to one hour, beginning dehydration below 100 degree, resin solid content reaches 90.5%, and cooling gets the modified melamine-formaldehyde solid resin.
Above-mentioned solid resin 200 grams are added adjusting adhesive butanols 10 grams, butanolamine 10 grams, after the dissolving, add again solidifying agent acetic acid 5 grams, emulsifier sodium lauryl sulfate 10 grams, foam stabilizer organosilicon 580# 10 grams (Jiangsu Yoke Technology Co., Ltd.), whipping agent hexanaphthene 5 grams, stir, put into baking oven and foam, reach predetermined height after, change again baking oven slaking 10 minutes under 120 degree are regulated over to, obtain closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 65kg/cm3, rate of closed hole, and 94.9%, oxygen index: 33.5, thermal conductivity is 0.026, compression performance 198.7kPa(deformation 10%).
Embodiment four
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product), 1052 grams, add benzoguanamine 200 grams, add Dyhard RU 100 300 grams, after being reacted to one hour, add Amino Terminated polyether(ATPE) 450# 200 gram (Nantong Lv Yuan novel material company limited) beginning dehydrations below 100 degree, until solids content reaches 88.8%, cooling gets the modified melamine-formaldehyde solid resin.
Above-mentioned solid resin 200 grams are added adjusting adhesive diglycolamine 10 grams, triglycol 10g, after the dissolving, add again solidifying agent oxalic acid 10 grams, tolylene diisocyanate (TDI) 10 grams, alkylphenol polyoxyethylene emulsifying agent (OP-10) 5 grams, foam stabilizer organosilicon AK8805 10 grams (Nanjing Dymatic Shichuang Chemical Co., Ltd.), whipping agent dichloro one fluoroethane (HCFC-141b) 5 grams, dichlorotrifluoroethane 5g, stir, after the microwave foaming, change again baking oven slaking 30 minutes under 120 degree are regulated over to, obtain closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 45.7kg/cm3, rate of closed hole, and 96.4%, oxygen index: 30.2, thermal conductivity is 0.022, compression performance 173.2kPa(deformation 10%).
Embodiment five
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product) 1052 gram, add benzoguanamine 200 grams, add Dyhard RU 100 100 grams, be reacted to one hour after, beginning dehydration below 100 degree, until solids content reaches 89.2%, cooling gets the modified melamine-formaldehyde solid resin.
After above-mentioned solid resin 200 gram adding adjusting adhesive low molecular polyether compound L Y204# 20 grams (Nantong Lv Yuan novel material company limited), dissolving, add again solidifying agent hexanodioic acid 20 gram, emulsifying agent alkylphenol polyoxyethylene (OP-10) 5 grams, foam stabilizer organosilicon 3363#(Nanjing dolantin generation wound company limited) 5 grams, whipping agent sherwood oil (boiling range 60-90 degree) 5 grams, stir.Put into microwave foaming behind predetermined density, change again baking oven slaking 30 minutes under 120 degree are regulated over to, obtain closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 52.9kg/cm3, rate of closed hole, and 97.1%, oxygen index: 34.7, thermal conductivity is 0.028, compression performance 183.6kPa(deformation 10%).
Embodiment six
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product) 1052 gram, add benzoguanamine 200 grams, be reacted to one hour after, beginning dehydration below 100 degree, until solids content reaches 90.7%, cooling gets the modified melamine-formaldehyde solid resin.
After above-mentioned solid resin 200 gram adding adjusting adhesive methyl alcohol 20 grams, dissolving, add again solidifying agent tosic acid 20 grams, emulsifying agent Sodium dodecylbenzene sulfonate 10 grams, foam stabilizer organosilicon 8805# (Nanjing dolantin generation is created company limited) 10 grams, whipping agent chlorodifluoroethane 15 grams, stir.Put into baking oven and foam, change again baking oven slaking 30 minutes under 120 degree are regulated over to, obtain closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 56.5kg/cm3, rate of closed hole, and 98.3%, oxygen index: 31.7, thermal conductivity is 0.025, compression performance 196.5kPa(deformation 10%).
Embodiment seven
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product), 1052 grams, add benzoguanamine 200 grams, after polyethers 310# 100 grams (Nantong Lv Yuan novel material company limited) 100 grams are reacted to one hour, beginning dehydration below 100 degree, until solids content reaches 90.4%, cooling gets the modified melamine-formaldehyde solid resin.
After above-mentioned solid resin 200 gram adding adjusting adhesive ethanol 20 grams, dissolving, add again emulsifying agent Sodium dodecylbenzene sulfonate 5 grams, alkylphenol polyoxyethylene (OP-10) 10 grams, whipping agent butane 5g, normal hexane 10 grams, solidifying agent acetic acid 20 grams, diphenylmethanediisocyanate PM200 200 restrains (Yantai Wan Hua company), stirs.Foaming changes baking oven slaking 5 minutes under 120 degree are regulated again over to, obtains closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 57.8kg/cm3, rate of closed hole, and 95.6%, oxygen index: 30.0 thermal conductivitys are 0.022, compression performance 166.5kPa(deformation 10%).
Embodiment eight
37% formalin 2527 is restrained in the reactor of packing into, stir with agitator, add a small amount of caustic soda (40%) and adjust PH 10, add trolamine 5 grams (analytical pure), be warmed up to 50 degree with temperature controller simultaneously, add 99% trimeric cyanamide (top grade product), 1052 grams, add benzoguanamine 200 grams, polyethers 210# 200 gram (Nantong Lv Yuan novel material company limited) reactions are after one hour, beginning dehydration below 100 degree, until solids content reaches 90.4%, cooling gets the modified melamine-formaldehyde solid resin.
After above-mentioned solid resin 200 gram adding adjusting adhesive thanomins 20 grams, dissolving, add again emulsifying agent Sodium dodecylbenzene sulfonate 5 gram, foam stabilizer organosilicon FQ5003# 10 grams (Nanjing dolantin generation wound company limited), whipping agent methylene dichloride 15 grams, solidifying agent sulfuric acid 20 grams, polymethylene multi-phenenyl isocyanate PAPI 5005 # 20 grams (German Hensel Man), stir.Foaming changes baking oven slaking 10 minutes under 120 degree are regulated again over to, obtains closed pore terpolycyantoamino-formaldehyde resin foam.
Foam density is 50.8kg/cm3, rate of closed hole, and 90.6%, oxygen index: 28.0 thermal conductivitys are 0.035, compression performance 130.5kPa(deformation 10%).

Claims (7)

1. the preparation method of a terpolycyantoamino-formaldehyde resin closed-cell foam is characterized in that comprising the steps:
1), in the terpolycyantoamino-formaldehyde resin building-up process, introduces the properties-correcting agent copolymerization, then through processed, obtain solids content and be higher than 85% modified melamine-formaldehyde solid resin, the properties-correcting agent add-on be the trimeric cyanamide consumption 10~95% between (weight ratio);
2), with step 1) the modified melamine-formaldehyde solid resin that obtains adds adjusting adhesive, after the dissolving, adds respectively solidifying agent, foam stabilizer, emulsifying agent, whipping agent, stir; Each material addition adds adjusting adhesive 10 ~ 200g, solidifying agent 5 ~ 200g, foam stabilizer 5 ~ 10g, emulsifying agent 5 ~ 10g, whipping agent 5 ~ 30g take the modified melamine-formaldehyde solid resin as reference in every 200g modified melamine-formaldehyde solid resin;
3), with step 2) mixture foam, reach predetermined density 36 ~ 100kg/cm 3After, under 100-120 degree condition slaking 3-30 minute, obtain the terpolycyantoamino-formaldehyde resin closed-cell foam, rate of closed hole is 94.9 ~ 98.3%, oxygen index is 30.0 ~ 35.2, thermal conductivity is 0.022 ~ 0.031, compression performance 156.1 ~ 198.7kPa.
2. according to the preparation method of right 1 described terpolycyantoamino-formaldehyde resin closed-cell foam, it is characterized in that: described properties-correcting agent is one or more in phenol, benzoguanamine, first substituted melamine, polyester, Dyhard RU 100, the polyethers.
3. according to the preparation method of right 1 described terpolycyantoamino-formaldehyde resin closed-cell foam, it is characterized in that: described adjusting adhesive is that ethylene glycol, glycol ether, diglycolamine, thanomin, butanolamine, diethanolamine, methyl alcohol, ethanol, butanols, triglycol, trolamine, molecular weight are one or more in 600 ~ 1600 the low molecular weight polycaprolactone ether compound.
4. according to the preparation method of right 1 described terpolycyantoamino-formaldehyde resin closed-cell foam, it is characterized in that: described solidifying agent be in formic acid, acetic acid, sulfuric acid, phosphoric acid, tosic acid, hexanodioic acid, oxalic acid, hydrochloric acid, tolylene diisocyanate (TDI), diphenylmethanediisocyanate (MDI), the polymethylene multi-phenenyl isocyanate (PAPI) one or more.
5. according to the preparation method of right 1 described terpolycyantoamino-formaldehyde resin closed-cell foam, it is characterized in that: described foam stabilizer be in organosilicon and the poly organic silicon one or more.
6. according to the preparation method of right 1 described terpolycyantoamino-formaldehyde resin closed-cell foam, it is characterized in that: described emulsifying agent is one or more in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, the alkylphenol polyoxyethylene (OP-10).
7. according to the preparation method of right 1 described terpolycyantoamino-formaldehyde resin closed-cell foam, it is characterized in that: described whipping agent is one or more in butane, Skellysolve A, normal hexane, hexanaphthene, sherwood oil, ethylene dichloride, dichlorotrifluoroethane, dichloro one fluoroethane, the chlorodifluoroethane.
CN201210328428.XA 2012-09-07 2012-09-07 Preparation method for melamine formaldehyde resin closed-cell foam Expired - Fee Related CN102898778B (en)

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CN103214641A (en) * 2013-05-09 2013-07-24 沙县宏盛塑料有限公司 Production method of melamine-formaldehyde resin
CN103665755A (en) * 2013-11-28 2014-03-26 南通紫鑫实业有限公司 Preparation methods of melamino-formaldehyde resin for foam and melamino-formaldehyde resin foam
CN104250386A (en) * 2014-09-25 2014-12-31 四川金象赛瑞化工股份有限公司 Preparation method of flame-retardant melamine hard foam
CN104277416A (en) * 2013-07-03 2015-01-14 合肥杰事杰新材料股份有限公司 Modified melamine foam plastic and preparation method thereof
CN104774426A (en) * 2015-04-17 2015-07-15 李�杰 Antistatic melamino-formaldehyde foam and preparation method thereof
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