CN106832762A - A kind of preparation method of low-density flame melamine formaldehyde resin rigid foam - Google Patents
A kind of preparation method of low-density flame melamine formaldehyde resin rigid foam Download PDFInfo
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- CN106832762A CN106832762A CN201710108206.XA CN201710108206A CN106832762A CN 106832762 A CN106832762 A CN 106832762A CN 201710108206 A CN201710108206 A CN 201710108206A CN 106832762 A CN106832762 A CN 106832762A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/052—Closed cells, i.e. more than 50% of the pores are closed
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to a kind of preparation method of low-density flame melamine formaldehyde resin rigid foam, the method is modified by introducing ethoxy substituted melamine to melamine resin, by control system moisture content, modified melamine-formaldehyde resin performed polymer of the solid content higher than 72% is obtained；Curing agent, foam stabiliser, emulsifying agent, foaming agent and toughener are added in performed polymer, is cast in mould after being well mixed；Then mould is placed in constant temperature oven, foams and cure, low-density flame melamine formaldehyde resin rigid foam is obtained.Melamine resin rigid foam density prepared by the present invention is less than 50kg/m3, oxygen index (OI) is higher than 30, and low production cost can be applied to building exterior wall heat preserving.
Description
Technical field
The invention belongs to macromolecule field of new, and in particular to a kind of low-density flame melamine formaldehyde resin hard
The preparation method of foam.
Background technology
Melamine resin foam is a kind of fire-retardant bubble of Intrinsical obtained in melamine resin as matrix
Foam plastics.Melamine resin foam only just burns when being contacted with naked light, decomposes and produces a large amount of inert gases, together
When surface quickly form fine and close coking layer, can effectively slow down the further development of flame, in the case of without fire retardant
Reach China B1 grades of flame-retardant standard.Compared with existing organic insulation material styrofoam, extruded sheet, polyurethane sheet etc., melamine
Formaldehyde resin foam burn when not drip, amount of smoke it is small, from fiery self-extinguishment, can thoroughly eliminate the fire safety evaluating of conventional foams
Hidden danger.However, the intrinsic triazine ring structure of melamine resin foam has larger rigidity, by methylene between triazine ring
Base or dimethylene ehter bond are connected with each other, the degree of cross linking is high, and intramolecule deformability is small, these structures shapes melamine first
Urea formaldehyde foam haves the shortcomings that fragility is big, easy dry linting.
At present, soft bubble is focused primarily upon for the research that melamine resin foam brittleness and application performance improve
Foam aspect, and achieve huge progress.As sound-absorbing insulation material, melamine resin flexible foam successful Application
In fields such as large stadium, factory, large scale equipment, pipeline, the vehicles.
But melamine resin flexible foam be open-celled structure, hygroscopic and its mechanical strength is low, causes its nothing
Method is applied to wall field of thermal insulation.By comparison, not only to remain flexible foam excellent for melamine resin rigid foam
Sound insulation, insulation and flame-retarding characteristic, and be also equipped with compared with rate of closed hole high and mechanical strength, building exterior wall heat preserving requirement can be met.
Patent CN102898778A discloses a kind of preparation method of melamine formaldehyde resin closed-cell foam, by the method
The melamine formaldehyde resin closed-cell foam with rate of closed hole high is obtained, while solving the fragility of melamine resin foam
Greatly, the problems such as compression strength is low, dry linting is serious, can be used for building exterior wall heat preserving.Patent CN104250386A discloses one kind
The preparation method of flame melamine rigid foam, powder is difficult using melamine formaldehyde resin closed-cell foam obtained in the method
Change, compression strength is high.But foam density prepared by above two method is larger, thus production cost is higher.Patent
CN103665287A discloses a kind of Synthetic method of resin for hard melamine foam material, the melamino-formaldehyde tree of preparation
Fat hard foam performance is uniform, and physical property preferably, but does not provide rate of closed hole data.
The content of the invention
A kind of low-density flame melamine formaldehyde tree is provided it is an object of the invention to solve above-mentioned technical problem
The preparation method of fat rigid foam.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of low-density flame melamine formaldehyde resin rigid foam, including step：
(1) in melamine resin building-up process, ethoxy substituted melamine, ethoxy substitution trimerization are added
Cyanamide and the 0.05~0.55 of melamine weight：1, by control system moisture content, obtain modified three of solid content higher than 72%
Melamine-formaldehyde resin prepolymer.
(2) performed polymer for obtaining step (1) is by weight, steady with 8~15 parts of curing agent, foam with 100 parts of performed polymer
Determine to be cast in mould after 1~8 part of agent, 0.5~5 part of emulsifying agent, 1~10 part of foaming agent, 5~30 parts of toughener are well mixed,
Then mould is placed in 80~120 DEG C of baking ovens 10~60min of foaming, after 10~30min is cured at 120~150 DEG C, obtain
Melamine resin rigid foam, its density is 30~50kg/m3, and compression strength is 130~170kPa, and oxygen index (OI) is 30
~38, rate of closed hole 85~98%.
The detailed process of step (1) is：By melamine, ethoxy substituted melamine, paraformaldehyde, 37% formalin
Solution adds band stirring, in the reaction vessel of attemperating unit, using sodium hydroxide solution regulation and control pH value of reaction system positioned at 8~
10, unlatching is stirred and heated, and is warming up to 85~95 DEG C, continues to react 1h after reaction to the transparent shape of system, and reaction is terminated afterwards,
Modified melamine-formaldehyde resin performed polymer is obtained.
Wherein, the mol ratio of paraformaldehyde and formaldehyde total amount contained by 37% formalin and melamine for 1.8~
2.2：1.
Ethoxy substituted melamine is N- (2- ethoxys) melamine, N, (the 2- hydroxyl second of N '-two in the step (1)
Base) melamine, N, N ', N "-three (2- ethoxys) melamines, N, N, N ', N " in-four (2- ethoxys) melamines one
Plant or more than one.
In the step (2) curing agent be ATMP, ethylene diamine tetra methylene phosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid,
One or more in diethylene triamine pentamethylene phosphonic.
Foam stabiliser is polyether modified silicon oil in the step (2), and structure is polysiloxanes-oxyalkylene block copolymerization
Thing, molecular weight is between 1500~15000.
Emulsifying agent is isooctanol polyethoxylate phosphate, nonyl phenol polyethers phosphate, poly alkyl alcohol ether phosphoric acid in the step (2)
One or more in ester.
In the step (2) foaming agent be n-hexane, pentane, petroleum ether in one or more.
Toughener is PPG, PEPA, polyolefin polyhydric alcohol, vegetable oil polyol in the step (2)
In one or more.
In view of melamine resin foam brittleness is big, easy dry linting shortcoming, the present invention is by melamino-formaldehyde
In resin synthesis process, ethoxy substituted melamine is introduced as modifying agent, reduce in synthetic resin between methylol and hydroxyl first
Crosslinking degree between base and amino, it is corresponding to increase soft segment length between triazine ring, so as to reduce the fragility of foam, improve bubble
Foam dry linting, the intensity for increasing foam.
Additionally, in melamine resin foaming process, amino can in its molecule while solidified resin for curing agent
The formaldehyde reaction of release is condensed between methylol in foaming process, improves environment friendly, and make using cooperative flame retardant between phosphorus-nitrogen
With the flame-retarding characteristic of increase foam；Because phosphorous in emulsifying agent, equally acted on using cooperative flame retardant between phosphorus-nitrogen, increase foam
Flame-retarding characteristic；Contain soft segment using toughener, add its fragility, improvement foam dry linting, the increasing that can further reduce foam
Plus the intensity of foam.
Melamine resin foam prepared by the present invention has that high mechanical strength, rate of closed hole be high, not dry linting, anti-flammability
Can be excellent the features such as, and foam density is higher than 30, low production cost less than 50kg/m3, oxygen index (OI), can be applied to external wall guarantor
Temperature.
Specific embodiment
Below, substantive distinguishing features of the invention and advantage are further described with reference to example, but the present invention not office
It is limited to listed embodiment.
Embodiment 1：
The synthesis of modified melamine-formaldehyde resin (modified melamine-formaldehyde resin performed polymer)：By melamine
126g, N, N ', N "-three (2- ethoxys) melamine 6.3g, paraformaldehyde 13g, 37% formalin 111g add band to stir
Mix, in the reaction vessel of attemperating unit (paraformaldehyde and formaldehyde total amount contained by 37% formalin and melamine mole
Than being 1.8：1) 10, are equal to using 30% sodium hydrate aqueous solution regulation and control pH value of reaction system, unlatching is stirred and heated, and is warming up to
85 DEG C, continue to react 1h after reaction to the transparent shape of system, reaction is terminated afterwards, modified melamine-formaldehyde resin solution is obtained
(modified melamine-formaldehyde resin performed polymer).
The preparation of melamine resin rigid foam：Modified melamine-formaldehyde resin solution 100g, curing agent two
The methylenephosphonic acid 8g of ethene triamine five, foam stabiliser DC5098 (U.S. Air Products Companies) 3g, emulsifying agent are different pungent
Alcohol polyether phosphate 2g, foaming agent n-hexane the 10g, (Germany of toughener castor oil polyhydric alcohol Lupranol Balance 50
Elastogran Companies) it is cast in mould after 30g is well mixed.Then mould is placed in 80 DEG C of baking ovens and is foamed
60min, after cure 30min at 120 DEG C, obtain melamine resin rigid foam, its density be 30.2kg/m3, resist
Compressive Strength is 131kPa, and oxygen index (OI) is 30.5, rate of closed hole 86.3%.
Embodiment 2：
The synthesis of modified melamine-formaldehyde resin：By melamine 126g, N, N '-two (2- ethoxys) melamine
69.3g, paraformaldehyde 22g, 37% formalin 119g are added with (paraformaldehyde in stirring, the reaction vessel of attemperating unit
And 37% formaldehyde total amount contained by formalin and the mol ratio of melamine be 2.2：1), using 30% sodium hydrate aqueous solution
Regulation and control pH value of reaction system is equal to 8, and unlatching is stirred and heated, and is warming up to 95 DEG C, continues to react after reaction to the transparent shape of system
1h, terminates reaction afterwards, and modified melamine-formaldehyde resin solution is obtained.
The preparation of melamine resin rigid foam：Modified melamine-formaldehyde resin solution 100g, curing agent hydroxyl
Base ethylene-diphosphonic acid 15g, foam stabiliser B8404 (Germany wins wound industrial group Company) 8g, emulsifying agent laureth
Phosphoesterase 30 .5g, 60~90 DEG C of 1g of foaming agent petroleum ether, (Taiwan Changxing chemical industry share is limited for toughener polyester-diol 5330
Company) it is cast in mould after 5g is well mixed.Then mould is placed in the 10min that foamed in 120 DEG C of baking ovens, after 150
30min is cured at DEG C, melamine resin rigid foam is obtained, its density is 49.2kg/m3, compression strength is
169kPa, oxygen index (OI) is 34.7, rate of closed hole 97.8%.
Embodiment 3：
The synthesis of modified melamine-formaldehyde resin：By melamine 126g, N- (2- ethoxys) melamine 12.6g,
N, N ', N "-three (2- ethoxys) melamine 12.6g, paraformaldehyde 23g, 37% formalin 100g add band stirring, temperature
(paraformaldehyde and formaldehyde total amount contained by 37% formalin are with the mol ratio of melamine in the reaction vessel of control device
2.0：1) 8.5, are located at using 30% sodium hydrate aqueous solution regulation and control pH value of reaction system, unlatching is stirred and heated, and is warming up to 90
DEG C, continue to react 1h after reaction to the transparent shape of system, reaction is terminated afterwards, modified melamine-formaldehyde resin solution is obtained.
The preparation of melamine resin rigid foam：Modified melamine-formaldehyde resin solution 100g, curing agent hydroxyl
Base ethylene-diphosphonic acid 10g, foam stabiliser Niax L-580 (U.S. GE Toshiba Silicones Companies) 3g, emulsification
The phosphate 2g of agent nonyl phenol polyethers -9, foaming agent n-hexane 3g, toughener polyether triol GEP-330N (Shanghai Gaoqiao petrochemical industries
Company) it is cast in mould after 15g is well mixed.Then mould is placed in the 40min that foamed in 100 DEG C of baking ovens, after 120
30min is cured at DEG C, melamine resin rigid foam is obtained, its density is 40.2kg/m3, compression strength is
152kPa, oxygen index (OI) is 33.1, rate of closed hole 92.0%.
Embodiment 4：
The synthesis of modified melamine-formaldehyde resin：By melamine 126g, N, N ', N "-three (2- ethoxys) melamines
Amine 12.6g, paraformaldehyde 23g, 37% formalin 100g are added with (poly first in stirring, the reaction vessel of attemperating unit
Aldehyde and formaldehyde total amount contained by 37% formalin and the mol ratio of melamine are 2.0：1) it is, water-soluble using 30% NaOH
Liquid regulation and control pH value of reaction system is located at 8.5, and unlatching is stirred and heated, and is warming up to 90 DEG C, continues after reaction to the transparent shape of system
Reaction 1h, terminates reaction afterwards, and modified melamine-formaldehyde resin solution is obtained.
The preparation of melamine resin rigid foam：Modified melamine-formaldehyde resin solution 100g, curing agent second
The methylenephosphonic acid 10g of diamines four, foam stabiliser AK-158 (Nanjing Dymatic Shichuang Chemical Co., Ltd.'s sale) 1g, emulsifying agent are different pungent
It is cast in mould after alcohol polyether phosphate 5g, foaming agent n-hexane 7g, toughener polybutadiene polyol 18g are well mixed.
Then mould is placed in the 40min that foamed in 100 DEG C of baking ovens, after cure 10min at 150 DEG C, obtain melamine resin
Rigid foam, its density is 35.1kg/m3, compression strength is 138kPa, and oxygen index (OI) is 30.5, rate of closed hole 86.9%.
Embodiment 5：
The synthesis of modified melamine-formaldehyde resin：By melamine 126g, N, N '-two (2- ethoxys) melamine
6.3g, N, N, N ', N "-four (2- ethoxys) melamine 6.3g, paraformaldehyde 23g, 37% formalin 100g add band
Stirring, (paraformaldehyde and formaldehyde total amount contained by 37% formalin and melamine rub in the reaction vessel of attemperating unit
You are than being 2.0：1) 8.5, are located at using 30% sodium hydrate aqueous solution regulation and control pH value of reaction system, unlatching is stirred and heated, and is risen
Temperature continues to react 1h to 90 DEG C, after reaction to the transparent shape of system, and reaction is terminated afterwards, and modified melamine-formaldehyde resin is obtained
Solution.
The preparation of melamine resin rigid foam：Modified melamine-formaldehyde resin solution 100g, curing agent ammonia
The methylenephosphonic acid 10g of base three, foam stabiliser Niax L-580 (U.S. GE Toshiba Silicones Companies) 3g, emulsification
Agent isooctanol polyethoxylate phosphate 2g, foaming agent pentane 2g, toughener polyether triol TEP-3033 (Tianjin Petrochemical Company sale)
It is cast in mould after 18g is well mixed.Then mould is placed in the 40min that foamed in 100 DEG C of baking ovens, after at 120 DEG C cure
30min, obtains melamine resin rigid foam, and its density is 46.4kg/m3, compression strength is 161kPa, oxygen index (OI)
It is 33.4, rate of closed hole 94.1%.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of low-density flame melamine formaldehyde resin rigid foam, it is characterised in that including following steps
Suddenly：
(1) in melamine resin building-up process, ethoxy substituted melamine, ethoxy substituted melamine are added
With the 0.05~0.55 of melamine weight：1, by control system moisture content, obtain modified melamine of the solid content higher than 72%
Amine-formaldehyde resins performed polymer.
(2) performed polymer for obtaining step (1) by weight, with 100 parts of performed polymer and 8~15 parts of curing agent, foam stabiliser 1
~8 parts, 0.5~5 part of emulsifying agent, 1~10 part of foaming agent, 5~30 parts of toughener it is well mixed after be cast in mould, then will
Mould is placed in 80~120 DEG C of baking ovens 10~60min of foaming, after 10~30min is cured at 120~150 DEG C, obtain melamine
Amine-formaldehyde resins rigid foam, its density is 30~50kg/m3, compression strength is 130~170kPa, and oxygen index (OI) is 30~38,
Rate of closed hole 85~98%.
2. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In the detailed process of step (1) is：By melamine, ethoxy substituted melamine, paraformaldehyde, 37% formalin
In adding with stirring, the reaction vessel of attemperating unit, 8~10 are located at using sodium hydroxide solution regulation and control pH value of reaction system, opened
Open and stir and heat, be warming up to 85~95 DEG C, continue to react 1h after reaction to the transparent shape of system, reaction is terminated afterwards, be obtained
Modified melamine-formaldehyde resin performed polymer.
3. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In ethoxy substituted melamine is N- (2- ethoxys) melamine, N, N '-two (2- ethoxys) melamine in step (1)
Amine, N, N ', N "-three (2- ethoxys) melamine, N, N, N ', N " one kind or one kind in-four (2- ethoxys) melamines
More than.
4. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In curing agent is ATMP, ethylene diamine tetra methylene phosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, diethylenetriamine in step (2)
One or more in five methylenephosphonic acids.
5. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In foam stabiliser is polyether modified silicon oil in step (2), and structure is polysiloxanes-oxyalkylene block copolymer, molecular weight
Between 1500~15000.
6. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In emulsifying agent is in isooctanol polyethoxylate phosphate, nonyl phenol polyethers phosphate, poly alkyl alcohol ether phosphate in step (2)
Plant or more than one.
7. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In, in step (2) foaming agent be n-hexane, pentane, petroleum ether in one or more.
8. the preparation method of low-density flame melamine formaldehyde resin rigid foam according to claim 1, its feature exists
In, in step (2) toughener be PPG, PEPA, polyolefin polyhydric alcohol, vegetable oil polyol in one kind or
More than one.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987307A (en) * | 2017-12-22 | 2018-05-04 | 河南金大地化工有限责任公司 | A kind of melamine resin foam production method |
| CN108252088A (en) * | 2017-12-12 | 2018-07-06 | 江苏新瑞贝科技股份有限公司 | A kind of textile flame-retardant finishing agent and preparation method thereof |
| CN109293862A (en) * | 2018-10-12 | 2019-02-01 | 合肥工业大学 | A kind of high-ductility hard melamine foams and preparation method thereof |
| CN110181747A (en) * | 2019-05-14 | 2019-08-30 | 中国民用航空总局第二研究所 | A method of seat cushions are prepared based on soft melamine foamed plastic |
| CN113185745A (en) * | 2021-04-08 | 2021-07-30 | 峰特(浙江)新材料有限公司 | Melamine formaldehyde foam with inorganic filler |
| CN114773827A (en) * | 2021-04-12 | 2022-07-22 | 池秀林 | Soft polyurethane foam plastic |
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Application publication date: 20170613 |