CN107936281A - A kind of NCC and graphene strengthen the preparation method of melamine foams jointly - Google Patents
A kind of NCC and graphene strengthen the preparation method of melamine foams jointly Download PDFInfo
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- CN107936281A CN107936281A CN201711246713.6A CN201711246713A CN107936281A CN 107936281 A CN107936281 A CN 107936281A CN 201711246713 A CN201711246713 A CN 201711246713A CN 107936281 A CN107936281 A CN 107936281A
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- 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
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C—CHEMISTRY; METALLURGY
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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
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
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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
- C08J9/0066—Use of inorganic compounding ingredients
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
- C08J2401/04—Oxycellulose; Hydrocellulose
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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Abstract
The present invention strengthens the preparation method of melamine foams for a kind of NCC and graphene jointly, using foaming after 10 ~ 20 μm of common modified cyanurotriamide resins of graphene oxide of NCC and particle diameter of 5 ~ 20nm of crystallite diameter, then the melamine foams that NCC and graphene strengthen jointly are made after hydrazine hydrate steam treatment foam.The NCC and graphene each serve as enhancing melamine foams frame strength as particulates reinforcements and bubble nucleating center and improve the effect of bubbling efficiency.Since graphene has thermal radiation property and hydrophobic character, the hydrophobicity performance of melamine foams can be improved while reducing the thermal conductivity factor of melamine foams, improving the heat-insulating capability of foam.
Description
Technical field
The present invention relates to a kind of preparation method for strengthening flexible melamine foams, more particularly, to a kind of NCC（Nano-cellulose
Crystal）Strengthen the preparation method of melamine foams jointly with graphene, belong to foam material field.
Background technology
Melamine foams are also known as melamino-formaldehyde foam, be one kind using melamine resin as primary raw material, it is foamed preparation and
Into novel flame-retardant perforated foams.Melamine foams density is low, has three-dimensional open pores structure and percent opening is higher than 85%, water suction
Property it is good, under unit volume can absorb 60 ~ 150 times of quality water, good flame resistance, thermal insulation is excellent, and sound absorption properties are good, and raw material sources are wide
It is general, it is cheap, machinability is good etc., therefore in every field such as noise-reducing building insulation, traffic, military affairs, electronics, daily use chemicals cleanings
All have great importance.Although melamine foams are widely used to the fields such as daily cleaning, building sound absorption, car body insulation,
Due to the shortcoming such as its intensity is relatively low, brittleness is larger, toughness is insufficient, dry linting rate is high, compressive strength is low, it is restricted its application.
The Chinese patent of Application No. 201410611034.4 provides a kind of modified melamine-formaldehyde of high-flexibility
Resin, by melamine, formaldehyde, isocyanuric acid ester, fatty acid amide, polyethylene glycol, alkylphenol polyoxyethylene ether, hydroxide
Sodium, alcohol and water synthesize the melmac for foaming after mixing according to a certain percentage.The invention is by regulating and controlling resin
Component, controls the copolycondensation of resin to change resin structure, reduces resin crosslink density, so as to strengthen foamy body, reduce
Toughness and brittleness, make its high resilience and increase its stability.Meanwhile extension melamine resin is realized by modification
Polymerization time and storage cycle.
The Chinese patent of Patent No. 201410611034.4 provides a kind of intrinsic flame-retardant modified melamino-formaldehyde bubble
Foam and its preparation method and application, using polyvinyl alcohol and KH550 modified melamine-formaldehyde resins, utilizes the soft of polyvinyl alcohol
Property segment and the characteristics of containing active amino and caking property of Silane coupling agent KH550, it is participated in the reaction of melamino-formaldehyde
In, so as to flexible PVA and KH550 chains are embedded between the rigid radical of melamino-formaldehyde to solve the easy embrittlement of foam
The problem of dusting, poor toughness.Melamino-formaldehyde foam prepared by the invention, with pliability is good, compressive strength is high, oxygen refers to
The advantages that number is more than 34%, and rebound degree is high.
The Chinese patent of Application No. 201610892337.7 provides a kind of the hard of the cellulose modified enhancing of nanocrystal
Matter melamine foams and preparation method thereof, highly concentrated nano crystalline fibers are made using nanocrystal cellulose and polyformaldehyde reaction
Reacted again with melamine after plain formaldehyde premixed solution, the cellulose modified expandability melamine resin of nanocrystal is made, through adding
Surfactant, curing agent, foaming agent etc. is added to obtain the hard melamine foams of the cellulose modified enhancing of nanocrystal after foaming.Should
The hard melamine foams of invention gained have compressive strength high, and uniform foam cell, fire resistance and heat endurance are good, preparation method letter
Just, the advantages that easily implementing.
Foregoing invention gives some and is used for the thinking that melamine foams are modified, and melamine is modified by increasing enhancing phase particle
The performance of foam, such as compressive strength, pulverization rate, fire resistance, have certain enhancing effect.But for using two-phase
Strengthen the melamine foams of Particles dispersed enhancing and improve the hydrophobicity, thermal insulation, fire resistance of melamine foams on this basis still
Do not refer to, therefore be based on the demand, it is proposed that the technical solution in the present invention.
The content of the invention
The purpose of the present invention overcomes the shortcomings of the prior art, there is provided a kind of NCC and graphene strengthen melamine bubble jointly
The preparation method of foam, is used as particulates reinforcements and bubble shape by the way that NCC crystallites and graphene are added in melamine foams skeleton
Core center, is improving bubbling efficiency at the same time, is improving the intensity of foam framework, has achieveed the purpose that melamine foams strengthen.Due to
Graphene has thermal radiation property, can reduce the thermal conductivity factors of melamine foams to improve its heat-insulating capability.Meanwhile graphene
Add the hydrophobicity performance for also improving melamine foams.
It is to achieve the object of the present invention the technical solution of use：
A kind of NCC and graphene strengthen the preparation method of melamine foams jointly, it is characterised in that the preparation method include with
The step of lower order：
（1）Graphene powder is dispersed in water to form graphene aqueous solution；
（2）NCC microcrystalline dispersions are formed and NCC aqueous solutions in water；
（3）By step（1）In graphene aqueous solution and paraformaldehyde be added in reaction kettle, and control temperature of reaction kettle 80
~ 110 DEG C, 10 ~ 30min of ultrasonic vibration, graphene is set to be uniformly dispersed to obtain the paraformaldehyde solution of graphene-containing in the solution, its
The concentration of middle paraformaldehyde is 50 ~ 60%；
（4）To step（3）In melamine is added in obtained mixed solution, and kettle temperature is controlled at 50 ~ 85 DEG C, adjusts solution
PH is 8 ~ 9, and mechanical agitation 1.5 ~ 3h of isothermal reaction is carried out with 200 ~ 600rpm rotating speeds, and measures mixed liquor in reaction kettle in real time and glue
When degree to viscosity be 800 ~ 1000mPa s, ice-water bath cooling reaction kettle is used to stop reaction, wherein melamine and poly first
The ratio of aldehyde is 1:1.8~2.8；
（5）By step（2）Obtained NCC aqueous solutions add step（4）In obtained mixed solution, and 1500 ~ 3000rpm turn
Speed is lower to carry out mechanical mixture, NCC is uniformly dispersed；
（6）Regulating step（5）Obtained mixed solution pH is 8 ~ 9, and kettle temperature is adjusted to 60 ~ 90 DEG C, with 1500 ~ 3000rpm
Rotating speed stirring isothermal reaction to solution viscosity is 1200 ~ 1400mPa s, and modified cyanurotriamide resin is made；
（7）To step（6）In the surfactant of volume fraction 2 ~ 5%, the curing of volume fraction 3 ~ 6% are added in obtained resin
Agent, the foaming agent of volume fraction 5 ~ 8%, the enhancing of expandability processed changes after 25 ~ 50s of mechanical agitation under 2500 ~ 3000rpm rotating speeds
Property melmac；
（8）By step（7）In the enhancing modified cyanurotriamide resin of expandability pour into mould, and in microwave foaming machine
Enhancing foam is made in foaming；
（9）By step（8）In obtained foam after 60 ~ 90 DEG C of 12 ~ 24h of hydrazine hydrate steam treatment, in 100 ~ 150 DEG C of air gas
Obtained NCC and graphene strengthen melamine foams jointly after atmosphere dries 1 ~ 5h.
Further, the step（1）In graphene powder be graphene oxide powder, diameier is 10 ~ 20 μm；
The NCC crystallite dimensions are diameter 5-20 nm, and the concentration of length 150-350nm, NCC solution is 0.1 ~ 0.5%.
The step（2）In NCC crystallite dimensions be diameter 5-20 nm, the concentration of length 150-350nm, NCC solution is
0.1~0.5%。
The advantageous effects of the present invention are：
In the present invention enhancing melamine foams, prepared enhancing melamine foams skeleton knot are prepared by adding NCC and graphene
Structure is strengthened, and foam cell uniformity is high, and mechanical property is also highly improved.Meanwhile the addition for strengthening phase graphene also improves
The heat-proof qualities of melamine foams.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after the present invention has been read, various equivalences of the those skilled in the art to the present invention
The modification of form falls within the application appended claims and is limited.
Embodiment 1
A kind of NCC and graphene strengthen the preparation method of melamine foams jointly, it is characterised in that the preparation method include with
Lower sequential steps：
（1）Graphene powder is dispersed in water to form graphene aqueous solution；
（2）NCC microcrystalline dispersions are formed and NCC aqueous solutions in water；
（3）By step（1）In graphene aqueous solution and paraformaldehyde be added in reaction kettle, and control temperature of reaction kettle 80
DEG C, ultrasonic vibration 20min, makes graphene be uniformly dispersed to obtain the paraformaldehyde solution of graphene-containing, wherein poly in the solution
The concentration of formaldehyde is 50%；
（4）To step（3）In melamine is added in obtained mixed solution, and kettle temperature is controlled at 65 DEG C, adjusts pH value of solution
For 8.5, mechanical agitation isothermal reaction 1.5h is carried out with 350rpm rotating speeds, and measures viscosity of mixed liquid in reaction kettle in real time, to viscous
Spend for 900mPa s when, using ice-water bath cooling reaction kettle stop reaction, wherein the ratio of melamine and paraformaldehyde be 1:
2；
（5）By step（2）Obtained NCC aqueous solutions add step（4）In obtained mixed solution, and under 1500rpm rotating speeds
Mechanical mixture is carried out, NCC is uniformly dispersed；
（6）Regulating step（5）Obtained mixed solution pH is 8, and kettle temperature is adjusted to 75 DEG C, is stirred with 1600rpm rotating speeds permanent
Temperature reaction to solution viscosity is 1200mPa s, and modified cyanurotriamide resin is made；
（7）To step（6）In add the surfactant of volume fraction 2% in obtained resin, the curing agent of volume fraction 3%,
The foaming agent of volume fraction 8%, under 2500rpm rotating speeds after mechanical agitation 30s expandability processed enhancing modified cyanurotriamide tree
Fat；
（8）By step（7）In the enhancing modified cyanurotriamide resin of expandability pour into mould, and in microwave foaming machine
Enhancing foam is made in foaming；
（9）By step（8）In obtained foam after 70 DEG C of hydrazine hydrate steam treatment 20h, after 120 DEG C of air atmospheres dry 5h
NCC and graphene is made strengthens melamine foams jointly.
Further, the step（1）In graphene powder be graphene oxide powder, diameier is 10 μm；Institute
The NCC crystallite dimensions stated are 10 nm of diameter, and the concentration of length 150nm, NCC solution is 0.3%.
The thermal conductivity factor that obtained NCC and graphene strengthen melamine foams jointly is 30mW/mK, and hydrophobic rate is 95%,
It is 300N to collapse intensity, which possesses excellent heat-proof quality and hydrophobicity, collapses that intensity is big, and anti-compression properties are good.
Embodiment 2
A kind of NCC and graphene strengthen the preparation method of melamine foams jointly, it is characterised in that the preparation method include with
Lower sequential steps：
（1）Graphene powder is dispersed in water to form graphene aqueous solution；
（2）NCC microcrystalline dispersions are formed and NCC aqueous solutions in water；
（3）By step（1）In graphene aqueous solution and paraformaldehyde be added in reaction kettle, and control temperature of reaction kettle to exist
110 DEG C, ultrasonic vibration 15min, graphene is set to be uniformly dispersed to obtain the paraformaldehyde solution of graphene-containing in the solution, wherein more
The concentration of polyformaldehyde is 50%；
（4）To step（3）In melamine is added in obtained mixed solution, and kettle temperature is controlled at 50 ~ 85 DEG C, adjusts solution
PH is 9, and mechanical agitation isothermal reaction 2h is carried out with 400rpm rotating speeds, and measures viscosity of mixed liquid in reaction kettle in real time, to viscosity
For 1000mPa s when, using ice-water bath cooling reaction kettle stop reaction, wherein the ratio of melamine and paraformaldehyde be 1:
2.5；
（5）By step（2）Obtained NCC aqueous solutions add step（4）In obtained mixed solution, and under 2000rpm rotating speeds
Mechanical mixture is carried out, NCC is uniformly dispersed；
（6）Regulating step（5）Obtained mixed solution pH is 8, and kettle temperature is adjusted to 70 DEG C, is stirred with 2500rpm rotating speeds permanent
Temperature reaction to solution viscosity is 1300mPa s, and modified cyanurotriamide resin is made；
（7）To step（6）In add the surfactant of volume fraction 3% in obtained resin, the curing agent of volume fraction 4%,
The foaming agent of volume fraction 6%, under 3000rpm rotating speeds after mechanical agitation 30s expandability processed enhancing modified cyanurotriamide tree
Fat；
（8）By step（7）In the enhancing modified cyanurotriamide resin of expandability pour into mould, and in microwave foaming machine
Enhancing foam is made in foaming；
（9）By step（8）In obtained foam after 85 DEG C of hydrazine hydrate steam treatment 14h, after 110 DEG C of air atmospheres dry 2h
NCC and graphene is made strengthens melamine foams jointly.
Further, the step（2）In NCC crystallite dimensions be 20 nm of diameter, length 350nm, NCC solution it is dense
Spend for 0.5%.
The thermal conductivity factor that obtained NCC and graphene strengthen melamine foams jointly is 29mW/mK, and hydrophobic rate is 96%,
The advantages that it is 310N to collapse intensity, possesses excellent heat-proof quality and hydrophobicity, and resistance to compression is good.
Two embodiments of the invention are above are only, but the design concept of the present invention is not limited thereto, all utilizations
This design carries out the present invention change of unsubstantiality, should all belong to the behavior for invading the scope of protection of the invention.In every case it is not
Depart from the content of technical solution of the present invention, the technical spirit according to the present invention is made above example any type of simple
Modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (2)
1. a kind of NCC and graphene strengthen the preparation method of melamine foams jointly, it is characterised in that the preparation method includes
The step of following order：
Graphene powder is dispersed in water to form graphene aqueous solution；
NCC microcrystalline dispersions are formed and NCC aqueous solutions in water；
By step（1）In graphene aqueous solution and paraformaldehyde be added in reaction kettle, and control temperature of reaction kettle 80 ~
110 DEG C, 10 ~ 30min of ultrasonic vibration, graphene is set to be uniformly dispersed to obtain the paraformaldehyde solution of graphene-containing in the solution, its
The concentration of middle paraformaldehyde is 50 ~ 60%；
To step（3）In melamine is added in obtained mixed solution, and kettle temperature is controlled at 50 ~ 85 DEG C, adjusts pH value of solution
For 8 ~ 9, mechanical agitation 1.5 ~ 3h of isothermal reaction is carried out with 200 ~ 600rpm rotating speeds, and measures mixed liquor in reaction kettle in real time and glues
When degree to viscosity be 800 ~ 1000mPa s, ice-water bath cooling reaction kettle is used to stop reaction, wherein melamine and poly first
The ratio of aldehyde is 1:1.8~2.8；
By step（2）Obtained NCC aqueous solutions add step（4）In obtained mixed solution, and in 1500 ~ 3000rpm rotating speeds
Lower carry out mechanical mixture, makes NCC be uniformly dispersed；
Regulating step（5）Obtained mixed solution pH is 8 ~ 9, and kettle temperature is adjusted to 60 ~ 90 DEG C, with 1500 ~ 3000rpm rotating speeds
It is 1200 ~ 1400mPa s to stir isothermal reaction to solution viscosity, and modified cyanurotriamide resin is made；
To step（6）In add the surfactant of volume fraction 2 ~ 5% in obtained resin, the curing agent of volume fraction 3 ~ 6%,
The foaming agent of volume fraction 5 ~ 8%, the enhancing of expandability processed is modified three after 25 ~ 50s of mechanical agitation under 2500 ~ 3000rpm rotating speeds
Cymel；Wherein surfactant is Tween-80, trimethyl ammonium chloride, neopelex, sodium glycerinate, list
One or more in 1-isobutyl-3,5-dimethylhexylphosphoric acid potassium, fatty alcohol polyoxy ether ammonium sulfate；Foaming agent is sodium acid carbonate or n-hexane；
Curing agent is formic acid, the one or more in acetic acid, ethanedioic acid, chloracetic acid, hydrochloric acid；
By step（7）In the enhancing modified cyanurotriamide resin of expandability pour into mould, and sent out in microwave foaming machine
It is brewed to strengthen foam；
By step（8）In obtained foam after 60 ~ 90 DEG C of 12 ~ 24h of hydrazine hydrate steam treatment, in 100 ~ 150 DEG C of air atmospheres
NCC and graphene is made after dry 1 ~ 5h strengthens melamine foams jointly.
2. preparation method according to claim 1, it is characterised in that the graphene is graphene oxide, diameier
For 10 ~ 20 μm；The NCC crystallite dimensions are diameter 5-20nm, the concentration of length 150-350nm, NCC solution for 0.1 ~
0.5%。
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106380783A (en) * | 2016-10-12 | 2017-02-08 | 江南大学 | Nanometer crystalline cellulose modification enhanced hard melamine foam and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106380783A (en) * | 2016-10-12 | 2017-02-08 | 江南大学 | Nanometer crystalline cellulose modification enhanced hard melamine foam and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 何欢等: ""三聚氰胺甲醛树脂硬质泡沫体的研究"", 《应用化工》 * |
| 陈中华等: "氧化石墨烯/密胺树脂导电复合材料的制备与性能研究"", 《功能材料》 * |
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