CN111732816A - Preparation process of light high-water-locking modified melamine foam plastic - Google Patents

Preparation process of light high-water-locking modified melamine foam plastic Download PDF

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CN111732816A
CN111732816A CN202010559380.8A CN202010559380A CN111732816A CN 111732816 A CN111732816 A CN 111732816A CN 202010559380 A CN202010559380 A CN 202010559380A CN 111732816 A CN111732816 A CN 111732816A
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water
locking
melamine foam
modified melamine
foam plastic
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蒋红卫
顾雪萍
徐绍林
俞宏建
蒋小弟
潘斌献
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Zhejiang Yadina New Material Technology Co ltd
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Zhejiang Yadina New Material Technology Co ltd
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-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 chemical blowing agent
    • C08J9/10Working-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 chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0095Mixtures of at least two compounding ingredients belonging to different one-dot groups
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08J2203/00Foams characterized by the expanding agent
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    • C08J2361/00Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/20Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08J2361/26Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
    • C08J2361/28Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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    • C08J2433/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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    • C08J2483/00Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/092Polycarboxylic acids

Abstract

The invention discloses a preparation process of a light high water-locking modified melamine foam plastic, which adds a small amount of high water-absorbing material polymerThe sodium acrylate is used for achieving the effect of high water absorption, and in order to further improve the high water absorption and high water locking performance of the material, citric acid and graphene oxide are added in the preparation process of the material; the citric acid is added, so that part of sodium polyacrylate can be converted into polyacrylic acid, and macromolecular chain entanglement is formed, and the water locking effect is improved; and the graphene oxide belongs to a typical two-dimensional polymer structure, and is added, so that the entanglement of macromolecular chains formed by sodium polyacrylate reaction is further promoted, and the water locking effect is remarkably promoted. The density of the light high-water-locking modified melamine foam plastic prepared by the invention is 15-20kg/m3The water absorption rate can reach 900-.

Description

Preparation process of light high-water-locking modified melamine foam plastic
Technical Field
The invention belongs to the technical field of melamine products, and particularly relates to a preparation process of a light high-water-locking modified melamine foam plastic.
Background
The melamine foam plastic has excellent sound absorption performance, flame retardant performance, heat insulation performance, insulativity, heat and humidity resistance stability, safety, sanitation, secondary processing performance and the like, and is a novel foam plastic with a low-density three-dimensional grid structure, which is prepared by taking melamine as a main raw material and has the aperture ratio of up to 99.9%. The melamine foam plastic has wide application prospect in the fields of construction, traffic, vehicle manufacturing, acoustic engineering, electronic information, object surface cleaning and decontamination and the like.
In recent years, melamine foam is widely used in the field of daily necessities, for example, melamine foam has excellent flame retardant property and replaces polyurethane foam to prepare a seat cushion, but the research focus of the existing melamine foam is low water absorption, for example, chinese invention patent CN10658927A discloses a melamine foam prepolymer with high closed cell rate and a preparation method thereof, the patent discloses a melamine foam added with boron modifier, in the foaming process of melamine resin, the boron modified melamine prepolymer can rapidly react, a polymer with high crosslinking density is rapidly formed around the cells formed by a foaming agent, and the foamed cells are stabilized and maintained, so that melamine foam with high closed cell rate is prepared, and the closed cell rate reaches more than 95%. The research on the modified melamine foam plastic with high water absorption and high water locking is less, and in order to expand the application range of the modified melamine foam plastic, a preparation process of the light modified melamine foam plastic with high water locking is needed to be developed.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation process of a light high-water-locking modified melamine foam plastic.
The technical scheme of the invention is as follows:
a preparation process of a light high-water-locking modified melamine foam plastic comprises the following steps:
(1) adding melamine into formaldehyde solution, regulating pH value to 9-10 by triethanolamine, heating to 80-90 deg.C, reacting for 50-60min to obtain melamine formaldehyde resin, adding polyvinyl butyral, citric acid and polyether modified polysiloxane copolymer while stirring, introducing nitrogen, slowly adding sodium polyacrylate solution, reacting for 60-90min, adding concentrated hydrochloric acid to regulate pH value to neutrality, and dehydrating; obtaining modified melamine resin;
(2) uniformly mixing and stirring the modified melamine resin obtained in the step (1), a surfactant and a foaming agent to obtain a first material for later use;
(3) mixing and stirring isooctyl mercaptopropionate and a liquid curing agent uniformly to obtain a second material for later use;
(4) continuously stirring the first material obtained in the step (2) for 2-3h, preheating to 45-50 ℃, then adding the second material obtained in the step (3), and continuously stirring for 30-40min to obtain a mixture;
(5) and (4) transferring the mixture obtained in the step (4) to a microwave heating furnace for microwave foaming to generate the melamine foam plastic.
Preferably, in the step (1), the sodium polyacrylate solution is composed of sodium polyacrylate, graphene oxide and deionized water.
Further preferably, in the step (1), the mass ratio of the sodium polyacrylate, the graphene oxide and the deionized water is 0.5-1.2: 0.1-0.3: 100.
preferably, the mass concentration of the formaldehyde solution is 35-40%, and the mass ratio of melamine, formaldehyde, polyvinyl butyral, citric acid, polyether modified polysiloxane copolymer, sodium polyacrylate solution, surfactant, foaming agent, isooctyl mercaptopropionate and liquid curing agent is 1: 0.35-0.45: 0.2-0.3: 0.03-0.04: 0.05-0.1: 0.008-0.015: 0.8-1.2: 0.1-0.2: 0.7-0.8: 0.05-0.1.
Preferably, in the step (2), the surfactant is sodium dodecyl sulfate.
Preferably, in the step (2), the blowing agent is a mixture of azobisisobutyronitrile and polyphenyl polymethylene polyisocyanate. More preferably, the mass ratio of the two is 1: 1.
preferably, in the step (5), the microwave frequency of the microwave foaming furnace is 2000-2500MHz, the power is 350-450W, and the microwave foaming time is 5-8 min.
The invention has the advantages that: according to the preparation process of the light high-water-locking modified melamine foam plastic, a small amount of high-water-absorption material sodium polyacrylate is added into the traditional light melamine foam plastic, so that the high-water-absorption effect is achieved, and in order to further improve the high-water-absorption and high-water-locking performance of the material, citric acid and graphene oxide are added in the preparation process of the material; the citric acid is added, so that part of sodium polyacrylate can be converted into polyacrylic acid, and macromolecular chain entanglement is formed, and the water locking effect is improved; and the graphene oxide belongs to a typical two-dimensional polymer structure, and is added, so that the entanglement of macromolecular chains formed by sodium polyacrylate reaction is further promoted, and the water locking effect is remarkably promoted. The density of the light high-water-locking modified melamine foam plastic prepared by the invention is 15-20kg/m3The water absorption rate can reach 900-.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified. The reagents used in the following examples, unless otherwise specified, were purchased from conventional biochemical reagent stores.
Example 1
A preparation process of a light high-water-locking modified melamine foam plastic comprises the following steps:
(1) adding melamine into a formaldehyde solution, adjusting the pH value to 9.5 by using triethanolamine, heating to 88 ℃ for reaction for 55min to generate melamine formaldehyde resin, adding polyvinyl butyral, citric acid and polyether modified polysiloxane copolymer while stirring, introducing nitrogen, slowly adding a sodium polyacrylate solution, continuing to react for 70min, adding concentrated hydrochloric acid to adjust the pH value to be neutral, and dehydrating; obtaining modified melamine resin;
(2) uniformly mixing and stirring the modified melamine resin obtained in the step (1), a surfactant and a foaming agent to obtain a first material for later use;
(3) mixing and stirring isooctyl mercaptopropionate and a liquid curing agent uniformly to obtain a second material for later use;
(4) continuously stirring the first material obtained in the step (2) for 2.5h, preheating to 48 ℃, then adding the second material obtained in the step (3), and continuously stirring for 35min to obtain a mixture;
(5) and (4) transferring the mixture obtained in the step (4) to a microwave heating furnace for microwave foaming to generate the melamine foam plastic.
In the step (1), the sodium polyacrylate solution consists of sodium polyacrylate, graphene oxide and deionized water; the mass ratio of the sodium polyacrylate, the graphene oxide and the deionized water is 0.8: 0.25: 100.
the mass concentration of the formaldehyde solution is 37%, and the mass ratio of melamine, formaldehyde, polyvinyl butyral, citric acid, polyether modified polysiloxane copolymer, sodium polyacrylate solution, surfactant, foaming agent, isooctyl mercaptopropionate and liquid curing agent is 1: 0.42: 0.25: 0.035: 0.08: 0.012: 1.1: 0.18: 0.75: 0.07.
in the step (2), the surfactant is sodium dodecyl sulfate.
In the step (2), the foaming agent is a mixture of azodiisobutyronitrile and polyphenyl polymethylene polyisocyanate; the mass ratio of the two is 1: 1.
in the step (5), the microwave frequency of the microwave foaming furnace is 2280MHz, the power is 420W, and the microwave foaming time is 7 min.
Example 2
A preparation process of a light high-water-locking modified melamine foam plastic comprises the following steps:
(1) adding melamine into a formaldehyde solution, adjusting the pH value to 10 by using triethanolamine, heating to 80 ℃ for reaction for 60min to generate melamine formaldehyde resin, adding polyvinyl butyral, citric acid and polyether modified polysiloxane copolymer while stirring, introducing nitrogen, slowly adding a sodium polyacrylate solution, continuing the reaction for 60min, adding concentrated hydrochloric acid to adjust the pH value to be neutral, and dehydrating; obtaining modified melamine resin;
(2) uniformly mixing and stirring the modified melamine resin obtained in the step (1), a surfactant and a foaming agent to obtain a first material for later use;
(3) mixing and stirring isooctyl mercaptopropionate and a liquid curing agent uniformly to obtain a second material for later use;
(4) continuously stirring the first material obtained in the step (2) for 3 hours, preheating to 45 ℃, then adding the second material obtained in the step (3), and continuously stirring for 40min to obtain a mixture;
(5) and (4) transferring the mixture obtained in the step (4) to a microwave heating furnace for microwave foaming to generate the melamine foam plastic.
In the step (1), the sodium polyacrylate solution consists of sodium polyacrylate, graphene oxide and deionized water; the mass ratio of the sodium polyacrylate, the graphene oxide and the deionized water is 0.5: 0.3: 100.
the mass concentration of the formaldehyde solution is 35%, and the mass ratio of melamine, formaldehyde, polyvinyl butyral, citric acid, polyether modified polysiloxane copolymer, sodium polyacrylate solution, surfactant, foaming agent, isooctyl mercaptopropionate and liquid curing agent is 1: 0.45: 0.2: 0.04: 0.05: 0.015: 0.8: 0.1: 0.8: 0.05.
in the step (2), the surfactant is sodium dodecyl sulfate.
In the step (2), the foaming agent is a mixture of azodiisobutyronitrile and polyphenyl polymethylene polyisocyanate; the mass ratio of the two is 1: 1.2.
in the step (5), the microwave frequency of the microwave foaming furnace is 2000MHz, the power is 450W, and the microwave foaming time is 5 min.
Example 3
A preparation process of a light high-water-locking modified melamine foam plastic comprises the following steps:
(1) adding melamine into a formaldehyde solution, adjusting the pH value to 9 by using triethanolamine, heating to 90 ℃ for reaction for 50min to generate melamine formaldehyde resin, adding polyvinyl butyral, citric acid and polyether modified polysiloxane copolymer while stirring, introducing nitrogen, slowly adding a sodium polyacrylate solution, continuing the reaction for 90min, adding concentrated hydrochloric acid to adjust the pH value to be neutral, and dehydrating; obtaining modified melamine resin;
(2) uniformly mixing and stirring the modified melamine resin obtained in the step (1), a surfactant and a foaming agent to obtain a first material for later use;
(3) mixing and stirring isooctyl mercaptopropionate and a liquid curing agent uniformly to obtain a second material for later use;
(4) continuously stirring the first material obtained in the step (2) for 2 hours, preheating to 50 ℃, then adding the second material obtained in the step (3), and continuously stirring for 30min to obtain a mixture;
(5) and (4) transferring the mixture obtained in the step (4) to a microwave heating furnace for microwave foaming to generate the melamine foam plastic.
In the step (1), the sodium polyacrylate solution consists of sodium polyacrylate, graphene oxide and deionized water; the mass ratio of the sodium polyacrylate, the graphene oxide and the deionized water is 1.2: 0.1: 100.
the mass concentration of the formaldehyde solution is 35-40%, and the mass ratio of melamine, formaldehyde, polyvinyl butyral, citric acid, polyether modified polysiloxane copolymer, sodium polyacrylate solution, surfactant, foaming agent, isooctyl mercaptopropionate and liquid curing agent is 1: 0.35: 0.3: 0.03: 0.1: 0.008: 1.2: 0.2: 0.7: 0.1.
in the step (2), the surfactant is sodium dodecyl sulfate.
In the step (2), the foaming agent is a mixture of azodiisobutyronitrile and polyphenyl polymethylene polyisocyanate; the mass ratio of the two is 1.2: 1.
in the step (5), the microwave frequency of the microwave foaming furnace is 2500MHz, the power is 350W, and the microwave foaming time is 8 min.
Comparative example 1
The citric acid in example 1 was removed and the rest of the formulation and preparation method were unchanged.
Comparative example 2
The graphene oxide in example 1 was removed, and the rest of the formulation and preparation method were unchanged.
The following physical property tests were performed on the lightweight high water-locking modified melamine foams prepared in examples 1 to 3 and comparative examples 1 to 2, and the following test results were obtained, and the specific test data are shown in table 1.
1. And (3) testing mechanical properties: testing the compression performance according to GBT 8813-2008;
2. and (3) testing the density: weighing a sample of dry foam having a size of 300mm × 300mm × 500mm with an analytical balance to an accuracy of 0.001g, and then calculating a foam density;
3. and (3) water absorption measurement: testing according to GBT 8810-2005;
4. testing the water retention: the above-mentioned water-saturated sample was taken out and weighed every 24 hours under an environment of 25 ℃ to calculate the water retentivity (ratio of the mass of water held in the water-absorbent material to the original mass of the foam).
TABLE 1 results of physical Properties test of modified Melamine foams
Density (kg/m)3 Compressive Strength (kPa) Water absorption% Water retention (72 h)%
Example 1 18 31.2 1127 843
Example 2 17 30.7 1054 795
Example 3 18 31.5 1172 871
Comparative example 1 18 30.9 1069 767
Comparative example 2 18 29.6 1015 541
As can be seen from the test data in Table 1, the melamine foam prepared by the invention has the remarkable characteristics of low density, high water absorption and high water locking.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (8)

1. A preparation process of a light high-water-locking modified melamine foam plastic is characterized by comprising the following steps:
(1) adding melamine into formaldehyde solution, regulating pH value to 9-10 by triethanolamine, heating to 80-90 deg.C, reacting for 50-60min to obtain melamine formaldehyde resin, adding polyvinyl butyral, citric acid and polyether modified polysiloxane copolymer while stirring, introducing nitrogen, slowly adding sodium polyacrylate solution, reacting for 60-90min, adding concentrated hydrochloric acid to regulate pH value to neutrality, and dehydrating; obtaining modified melamine resin;
(2) uniformly mixing and stirring the modified melamine resin obtained in the step (1), a surfactant and a foaming agent to obtain a first material for later use;
(3) mixing and stirring isooctyl mercaptopropionate and a liquid curing agent uniformly to obtain a second material for later use;
(4) continuously stirring the first material obtained in the step (2) for 2-3h, preheating to 45-50 ℃, then adding the second material obtained in the step (3), and continuously stirring for 30-40min to obtain a mixture;
(5) and (4) transferring the mixture obtained in the step (4) to a microwave heating furnace for microwave foaming to generate the melamine foam plastic.
2. The preparation process of the light high water-locking modified melamine foam plastic as claimed in claim 1, wherein in step (1), the sodium polyacrylate solution is composed of sodium polyacrylate, graphene oxide and deionized water.
3. The preparation process of the light high-water-locking modified melamine foam plastic as claimed in claim 2, wherein in the step (1), the mass ratio of the sodium polyacrylate, the graphene oxide and the deionized water is 0.5-1.2: 0.1-0.3: 100.
4. the preparation process of the light high water-locking modified melamine foam plastic as claimed in claim 1, wherein the mass concentration of the formaldehyde solution is 35-40%, and the mass ratio of melamine, formaldehyde, polyvinyl butyral, citric acid, polyether modified polysiloxane copolymer, sodium polyacrylate solution, surfactant, foaming agent, isooctyl mercaptopropionate and liquid curing agent is 1: 0.35-0.45: 0.2-0.3: 0.03-0.04: 0.05-0.1: 0.008-0.015: 0.8-1.2: 0.1-0.2: 0.7-0.8: 0.05-0.1.
5. The process for preparing the light weight high water-locking modified melamine foam according to claim 1, wherein in step (2), the surfactant is sodium dodecyl sulfate.
6. The process for preparing a lightweight, high water-locking modified melamine foam according to claim 1, wherein in step (2), said blowing agent is a mixture of azobisisobutyronitrile and polyphenyl polymethylene polyisocyanate.
7. The process for preparing a lightweight high water-locking modified melamine foam according to claim 6, wherein the mass ratio of azobisisobutyronitrile to polyphenyl polymethylene polyisocyanate is 1: 1.
8. the process for preparing the light melamine foam with high water-locking property as claimed in claim 1, wherein in the step (5), the microwave frequency of the microwave foaming furnace is 2000-2500MHz, the power is 350-450W, and the microwave foaming time is 5-8 min.
CN202010559380.8A 2020-06-18 2020-06-18 Preparation process of light high-water-locking modified melamine foam plastic Pending CN111732816A (en)

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