CN111087753A - Modified melamine rigid foam with high closed cell rate and low water absorption and preparation method thereof - Google Patents
Modified melamine rigid foam with high closed cell rate and low water absorption and preparation method thereof Download PDFInfo
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- 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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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
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- 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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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/32—Modified amine-aldehyde condensateS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
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Abstract
The invention relates to modified melamine rigid foam with high closed cell rate and low water absorption and a preparation method thereof, belonging to the technical field of high polymer materials. The density of the modified melamine rigid foam is less than 60kg/m3The closed porosity is 80-85%, the water absorption is 7.6-10.5%, the compressive strength is 339-356 kPa, the bending strength is 0.36-0.43 MPa, and the limiting oxygen index is 38.5-39.5%. The preparation of the modified melamine rigid foam is modified by two aspects of chemistry and physics. Organic silicon is introduced as a modifier through chemical modification, and the whole molecular chain is nonpolar due to the encapsulation of the pendant alkyl group of the modifier, so that the organic silicon modified waterborne polyurethane adhesive has good hydrophobicity and reduces water absorption; preparation of physical modification in foaming liquidIn the stage, the toughness and the mechanical property of the foam are improved by adding the toughening filler carbon fibers, and the carbon fibers are uniformly dispersed to the foam wall, so that the support can be effectively reinforced and the deformation of the pores can be weakened, the closed pore structure can be formed, the pores can be stabilized, and the compression strength is improved.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to modified melamine rigid foam with high closed cell rate and low water absorption and a preparation method thereof.
Background
The melamine rigid foam is also called melamine formaldehyde rigid foam. Is a foam material prepared from melamine resin through a certain foaming process. The melamine foam has excellent mechanical properties due to the fact that the melamine foam contains a large number of triazine ring structures with high strength. And the flame retardance and the heat resistance are the most outstanding performances of the melamine foam, and the decomposition temperature of the melamine foam can reach about 420 ℃. During combustion, melamine foam decomposes to produce large amounts of nitrogen (N)2And) and carbon dioxide (CO)2Meanwhile, a compact carbon layer is formed on the surface of the foam, so that oxygen can be isolated, and a certain flame retardant effect is achieved. This feature is an advantage over mainstream rigid foam materials such as polyurethane foam, phenolic resin foam, and the like. However, most of common melamine foams are of open-cell structures, and the applications of the melamine foams in materials such as insulation boards of refrigeration houses and external walls of buildings are greatly limited due to low closed-cell rate, high water absorption and poor heat insulation and preservation performance. Therefore, in order to further expand the application field of the rigid melamine foam, the closed cell rate of the rigid melamine foam material needs to be improved and the water absorption rate of the rigid melamine foam material needs to be reduced by modifying the prepolymer, adjusting the foaming process and the like.
Disclosure of Invention
In order to further improve the closed cell rate, reduce the water absorption rate and improve the heat preservation effect and the mechanical property of the melamine rigid foam material, the invention aims to provide the modified melamine rigid foam with high closed cell rate and low water absorption rate, and the invention also aims to provide the preparation method of the modified melamine rigid foam with high closed cell rate and low water absorption rate.
The density of the modified melamine rigid foam with high closed cell rate and low water absorption is lower than 60kg/m3The bending strength is 0.36-0.43 MPa;
in the preparation process of the modified melamine rigid foam, the organosilicon is used as a modifier, so that the water absorption of the modified melamine rigid foam is reduced to 7.6-10.5%, and the compressive strength reaches 339-356 kPa; the carbon fiber is used as a physical toughening and flame-retardant modifier, so that the closed-cell rate of the modified melamine rigid foam reaches 80-85%, and the limiting oxygen index reaches 38.5-39.5%.
The preparation operation steps of the modified melamine rigid foam with high closed cell rate and low water absorption rate are as follows:
(1) adding 222.5g of paraformaldehyde and 353.6g of distilled water into 300g of melamine, and dissolving for 10-20min at the temperature of 80-85 ℃ under stirring to obtain a clear melamine formaldehyde solution;
(2) adding 3.75g of a pH value regulator hexamethylene tetramine and 6-21g of an organic silicon modifier into a melamine formaldehyde solution, and reacting for 2-3h under the condition of constant stirring at the temperature of 80-85 ℃; adding 4.5g of retarder sodium tetraborate, and rapidly cooling to below 30 ℃ to obtain a chemically modified melamine resin prepolymer;
the organic silicon modifier is an alkoxy silane modifier;
(3) adding 3-5g of dimethyl silicone oil, 6-10g of foaming agent n-hexane and 0.05-2g of micron-sized carbon fibers into 200g of chemically modified melamine resin prepolymer, and stirring at a high speed for 2-3min to obtain a melamine resin prepolymer, wherein the viscosity of the modified melamine resin prepolymer is 70-75 Pa.s;
(4) and adding 0.8-1.4g of curing agent hydrochloric acid into the melamine resin prepolymer, stirring at a high speed for 1-2min, carrying out oven foaming at 100 ℃ for 30-40min, and curing to obtain the hard melamine foam material with high closed cell rate and low water absorption.
The preparation technical scheme is further defined as follows:
in the step (2), the alkoxy silane modifier is one of a silane coupling agent KH-550, methyl trialkoxy silane and 3- (2, 3-epoxypropoxy) propyl trimethoxy silane.
The beneficial technical effects of the invention are embodied in the following aspects:
1. the invention mainly carries out modification from the following two aspects, wherein the chemical modification is to introduce an organic silicon modifier in the prepolymer synthesis stage, and the whole molecular chain is nonpolar due to the wrapping of the side alkyl group, so the modified melamine rigid foam has hydrophobicity, and the water absorption of the modified melamine rigid foam is reduced to 7.6-10.5%; the main chain is regular silicon oxygen atoms which are arranged alternately, silicon oxygen bonds can rotate freely, alkyl groups of side chains are nonpolar groups, the size is small, a certain toughening effect is achieved on melamine resin, and the compressive strength of the modified melamine rigid foam reaches 339-356 kPa; the physical modification method is characterized in that carbon fibers are added in the preparation stage of the foaming liquid as a physical toughening and flame-retardant modifier, so that gas released by decomposition of a foaming agent in the foaming process is kept, the closed cell rate of the modified melamine rigid foam reaches 80-85%, and the limiting oxygen index reaches 38.5-39.5%. In addition, the carbon fiber contains a large amount of carbon elements, so that the flame retardant property is effectively improved in the foam combustion process.
2. The modification mechanism of the preparation method of the present invention is illustrated as follows: in the chemical modification process, the organosilicon is used as a modifier, and the whole molecular chain is nonpolar due to the encapsulation of the side alkyl group, so that the hydrophobic property is realized, and the water absorption of the prepared melamine foam is improved; the modified melamine resin contains a certain amount of Si-O-Si bonds, the strength is improved compared with that of the unmodified melamine resin, and when the melamine resin is foamed by a certain foaming process, the breakage and collapse of foam cells caused by too low resin strength in the initial foaming process can be effectively prevented, and the closed cell structure of hard melamine foam is increased; the organic silicon modifier is hydrolyzed, and the hydrolysis product is alcohol, so that the hydrolysis product is combined with hydroxymethyl of hydroxymethylated melamine to increase the distance of rigid groups and increase the flexibility of melamine resin molecules; in addition, the main chain is regular silicon oxygen atoms which are arranged alternately, silicon oxygen bonds can rotate freely, alkyl groups of the side chains are nonpolar groups, and the size is small, so that the molecular chain flexibility is good, and the flexibility of the melamine resin is improved to a certain extent. In the physical modification process, the carbon fibers effectively strengthen the support and weaken the deformation of the pores, so that the gas released by the decomposition of the foaming agent in the foaming process is kept, a closed pore structure is formed, the pores are stabilized, and the mechanical property of the foam material is well improved.
3. The raw material used in the preparation process is paraformaldehyde, and the melamine resin prepared from the paraformaldehyde has certain self-emulsifying capacity in prepolymerization, so that an emulsifier is not required to be added in the process of preparing the foaming liquid, the foaming liquid can be uniformly dispersed only by strong mechanical stirring, the number of large bubbles can be reduced, the surface tension of the foaming liquid is effectively reduced, the size distribution of the prepared melamine foam pores is more uniform, and the pore closing rate reaches 80-85%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by examples below. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention.
Example 1
The specific operation steps for preparing the modified melamine rigid foam with high closed cell rate and low water absorption are as follows:
(1) 353.5g of distilled water, 225.5g of paraformaldehyde and 300g of melamine are added into a 500ml three-neck flask, and stirred and reacted for 15min at 85 ℃ to obtain a clear melamine formaldehyde solution;
(2) adding 3.75g of hexamethylenetetramine and 9g of silane coupling agent (KH-550) into a melamine formaldehyde solution, and stirring at a constant speed at 85 ℃ for reaction for 3 hours; measuring the reaction end point by a cloud point method, adding 4.5g of sodium tetraborate, finishing the reaction, rapidly cooling to below 30 ℃ to obtain a modified melamine resin prepolymer with the viscosity of 0.54 Pa.s, and preserving at a constant temperature of 25 ℃ until the viscosity of the modified melamine resin prepolymer is 70 Pa.s;
(3) adding 4g of methyl silicone oil with the viscosity of 10cs, 10g of n-hexane and 1.8g of micron-sized carbon fibers into 200g of modified melamine resin prepolymer, adding 1.3g of hydrochloric acid with the concentration of 35-40% under the condition of high-speed stirring at 1300r/min, uniformly stirring, carrying out oven foaming at 100 ℃ for 35min, and curing to obtain modified melamine rigid foam with high closed cell rate and low water absorption rate;
the density of the prepared modified melamine rigid foam is 56kg/m3The sheet had a closed cell content of 85%, a water absorption of 7.6%, a compressive strength of 347kPa, a flexural strength of 0.43MPa and a limiting oxygen index of 39.5%.
Example 2
The specific operation steps for preparing the modified melamine rigid foam with high closed cell rate and low water absorption are as follows:
(1) 353.5g of distilled water, 225.5g of paraformaldehyde and 300g of melamine are added into a 500ml three-neck flask, and a clear melamine formaldehyde solution is obtained after stirring and reacting for 15min at 85 ℃;
(2) adding 3.75g of hexamethylenetetramine and 12g of methyl trialkoxy silane into a melamine formaldehyde solution, stirring at a constant speed, and reacting for 2.5h at 85 ℃; measuring the reaction end point by a cloud point method, adding 4.5g of sodium tetraborate, rapidly cooling to below 30 ℃ to obtain a modified melamine resin prepolymer with the viscosity of 0.48 Pa.s, and preserving at a constant temperature of 25 ℃ until the viscosity of the modified melamine resin prepolymer is 70 Pa.s;
(3) adding 4g of methyl silicone oil with the viscosity of 10cs, 10g of n-hexane and 1.2g of micron-sized carbon fibers into 200g of modified melamine resin prepolymer, adding 1.3g of hydrochloric acid with the concentration of 35-40% under the condition of high-speed stirring at 1300r/min, uniformly stirring, carrying out oven foaming at 100 ℃ for 35min, and curing to obtain modified melamine rigid foam with high closed cell rate and low water absorption rate;
the density of the prepared modified melamine rigid foam is 53kg/m3The closed cell content was 83%, the water absorption was 9%, the compressive strength was 339kPa, the flexural strength was 0.41MPa, and the limiting oxygen index was 38.5%.
Example 3
The specific operation steps for preparing the modified melamine rigid foam with high closed cell rate and low water absorption are as follows:
(1) 353.5g of distilled water, 225.5g of paraformaldehyde and 300g of melamine are added into a 500ml three-neck flask, and a clear melamine formaldehyde solution is obtained after stirring and reacting for 15min at 85 ℃;
(2) adding 3.75g of hexamethylenetetramine into a melamine formaldehyde solution, adding 15g of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring at 85 ℃ for reacting for 3 hours; measuring the reaction end point by a cloud point method, adding 4.5g of sodium tetraborate, rapidly cooling to below 30 ℃ to obtain a modified melamine foam prepolymer with the viscosity of 0.51 Pa.s, and preserving at a constant temperature of 25 ℃ until the viscosity of the modified melamine resin prepolymer is 75 Pa.s;
(3) adding 4g of methyl silicone oil with the viscosity of 10cs, 10g of n-hexane and 0.15g of micron-sized carbon fibers into 200g of modified melamine resin prepolymer, adding 1.3g of hydrochloric acid with the concentration of 35-40% under the condition of high-speed stirring at 1300r/min, uniformly stirring, carrying out oven foaming at 100 ℃ for 35min, and curing to obtain modified melamine rigid foam with high closed cell rate and low water absorption rate;
the density of the prepared modified melamine rigid foam is 57kg/m3The closed cell content was 79.5%, the water absorption was 10.1%, the compressive strength was 356kPa, the flexural strength was 0.37MPa, and the limiting oxygen index was 39%.
Example 4
The specific operation steps for preparing the modified melamine rigid foam with high closed cell rate and low water absorption are as follows:
(1) 353.5g of distilled water, 225.5g of paraformaldehyde and 300g of melamine are added into a 500ml three-neck flask, and a clear melamine formaldehyde solution is obtained after stirring and reacting for 15min at 85 ℃;
(2) adding 3.75g of hexamethylenetetramine into a melamine formaldehyde solution, adding 12g of silane coupling agent (KH-550), heating to 85 ℃, and stirring for reacting for 2.5 h; measuring the reaction end point by a cloud point method, adding 4.5g of sodium tetraborate, rapidly cooling to below 30 ℃ to obtain a modified melamine resin prepolymer with the viscosity of 0.56 Pa.s, and preserving at a constant temperature of 25 ℃ until the viscosity of the modified melamine resin prepolymer is 75 Pa.s;
(3) adding 4g of methyl silicone oil with the viscosity of 10cs, 10g of n-hexane and 1.8g of micron-sized carbon fibers into 200g of modified melamine resin prepolymer, adding 1.3g of hydrochloric acid with the concentration of 35-40% under the condition of high-speed stirring at 1300r/min, uniformly stirring, carrying out oven foaming at 100 ℃ for 35min, and curing to obtain modified melamine rigid foam with high closed cell rate and low water absorption rate;
the density of the prepared modified melamine rigid foam is 51kg/m3The sheet had a closed cell content of 82%, a water absorption of 9.3%, a compressive strength of 347kPa, a flexural strength of 0.39MPa and a limiting oxygen index of 39.5%.
Example 5
The specific operation steps for preparing the modified melamine rigid foam with high closed cell rate and low water absorption are as follows:
(1) 353.5g of distilled water, 225.5g of paraformaldehyde and 300g of melamine are added into a 500ml three-neck flask, and a clear melamine formaldehyde solution is obtained after stirring and reacting for 15min at 85 ℃;
(2) adding 3.75g of hexamethylenetetramine into a melamine formaldehyde solution, adding 9g of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring at 85 ℃ for reacting for 2.5 hours; measuring the reaction end point by a cloud point method, adding 4.5g of sodium tetraborate, rapidly cooling to below 30 ℃ to obtain a modified melamine resin prepolymer with the viscosity of 0.43 Pa.s, and preserving at a constant temperature of 25 ℃ until the viscosity of the modified melamine resin prepolymer is 75 Pa.s;
(3) adding 4g of methyl silicone oil with the viscosity of 10cs, 10g of n-hexane and 1.3g of micron-sized carbon fibers into 200g of modified melamine resin prepolymer, adding 1.3g of hydrochloric acid with the concentration of 35-40% under the condition of high-speed stirring at 1300r/min, uniformly stirring, carrying out oven foaming at 100 ℃ for 35min, and curing to obtain modified melamine rigid foam with high closed cell rate and low water absorption rate;
the density of the prepared modified melamine rigid foam is 53kg/m3The closed cell content was 80%, the water absorption was 10.5%, the compressive strength was 352kPa, the flexural strength was 0.36MPa, and the limiting oxygen index was 38.5%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. Modification with high closed pore rate and low water absorptionA melamine rigid foam characterized by: the density of the modified melamine rigid foam is less than 60kg/m3The bending strength is 0.36-0.43 MPa;
in the preparation process of the modified melamine rigid foam, the organosilicon is used as a modifier, so that the water absorption of the modified melamine rigid foam is reduced to 7.6-10.5%, and the compressive strength reaches 339-356 kPa; the carbon fiber is used as a physical toughening and flame-retardant modifier, so that the closed-cell rate of the modified melamine rigid foam reaches 80-85%, and the limiting oxygen index reaches 38.5-39.5%.
2. The method for preparing the modified melamine rigid foam with high closed cell rate and low water absorption according to claim 1, which is characterized by comprising the following steps:
(1) adding 222.5g of paraformaldehyde and 353.6g of distilled water into 300g of melamine, and dissolving for 10-20min at the temperature of 80-85 ℃ under stirring to obtain a clear melamine formaldehyde solution;
(2) adding 3.75g of a pH value regulator hexamethylene tetramine and 6-21g of an organic silicon modifier into a melamine formaldehyde solution, and reacting for 2-3h under the condition of constant stirring at the temperature of 80-85 ℃; adding 4.5g of retarder sodium tetraborate, and rapidly cooling to below 30 ℃ to obtain a chemically modified melamine resin prepolymer;
the organic silicon modifier is an alkoxy silane modifier;
(3) adding 3-5g of dimethyl silicone oil, 6-10g of foaming agent n-hexane and 0.05-2g of micron-sized carbon fibers into 200g of chemically modified melamine resin prepolymer, and stirring at a high speed for 2-3min to obtain a melamine resin prepolymer, wherein the viscosity of the modified melamine resin prepolymer is 70-75 Pa.s;
(4) and adding 0.8-1.4g of curing agent hydrochloric acid into the melamine resin prepolymer, stirring at a high speed for 1-2min, carrying out oven foaming at 100 ℃ for 30-40min, and curing to obtain the hard melamine foam material with high closed cell rate and low water absorption.
3. The method according to claim 2, wherein in the step (2), the alkoxysilane-based modifier is one of a silane coupling agent KH-550, methyltrialkoxysilane, and 3- (2, 3-glycidoxy) propyltrimethoxysilane.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007009127A1 (en) * | 2006-03-09 | 2007-09-13 | Basf Ag | Open-cell aminoplastics foam for thermal and acoustic insulation in building, vehicle or aircraft, low temperature insulation, insulating shock-absorbing packaging material, cleaning sponge or hygiene product contains fibrous filler |
| CN103391964A (en) * | 2011-02-24 | 2013-11-13 | 巴斯夫欧洲公司 | Melamine resin foam having particulate filler |
| CN109181215A (en) * | 2018-08-10 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of the hard melamine foams of the high rate of closed hole of low-density |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007009127A1 (en) * | 2006-03-09 | 2007-09-13 | Basf Ag | Open-cell aminoplastics foam for thermal and acoustic insulation in building, vehicle or aircraft, low temperature insulation, insulating shock-absorbing packaging material, cleaning sponge or hygiene product contains fibrous filler |
| CN103391964A (en) * | 2011-02-24 | 2013-11-13 | 巴斯夫欧洲公司 | Melamine resin foam having particulate filler |
| US20130337255A1 (en) * | 2011-02-24 | 2013-12-19 | Basf Se | Melamine resin foam with particulate filling material |
| CN109181215A (en) * | 2018-08-10 | 2019-01-11 | 合肥工业大学 | A kind of preparation method of the hard melamine foams of the high rate of closed hole of low-density |
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