CN107602868A - A kind of abietyl epoxy foam insulation material and preparation method thereof - Google Patents
A kind of abietyl epoxy foam insulation material and preparation method thereof Download PDFInfo
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- CN107602868A CN107602868A CN201710913155.8A CN201710913155A CN107602868A CN 107602868 A CN107602868 A CN 107602868A CN 201710913155 A CN201710913155 A CN 201710913155A CN 107602868 A CN107602868 A CN 107602868A
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- abietyl
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Abstract
The invention discloses a kind of abietyl epoxy foam insulation material and preparation method thereof, abietyl epoxy foam insulation material is prepared by vegetable fat and rosin derivative reaction.The present invention is that raw material prepares abietyl epoxy foams by vegetable fat and rosin derivative, and overcome complex process in the prior art and it is not biodegradable the defects of, with raw material sources are wide, price is low, degradable, synthesis condition is gentle, preparation technology is simple, environmental pollution is small and meet the advantages such as sustainable development, the density of gained abietyl epoxy foam insulation material is 0.1~0.8g/cm3, compressive strength (σ 0.01) under 10% strained condition is 0.183~1.068MPa, and compressive strength (σ 0.50) under 50% strained condition is 2.548~15.351MPa, and thermal conductivity factor is 0.021~0.061W/mk.
Description
Technical field
The present invention relates to a kind of abietyl epoxy foam insulation material and preparation method thereof, belongs to cellular insulant neck
Domain.
Background technology
Epoxy foam due to it is light, heat endurance is good, high mechanical properties, dielectric constant are low, heat-proof quality it is excellent with
And the characteristics such as cost is low, it is widely used in the fields such as automobile, electronics embedding, aircraft product, packing case, ship outer casing.Tradition
Epoxy foam it is more prepared using oil radical derivative as raw material, the discarded object of this class A foam A is difficult to natural degradation, gives environment band
Seriously bear.Therefore, to prepare biodegradable epoxy foams using renewable resource as raw material significant.
Japan Patent JP2007161856 describes a kind of using epoxy resin, polyisocyanates, polyglycidyl ether, water
It is raw material etc. component, the method for preparing heat resistant type epoxy foam plastics.Report that the heat decomposition temperature of the epoxy foam plastics exists
In the range of 200~280 DEG C, density 0.05g/cm3During left and right, compressive strength is 0.08~0.12MPa.
The A of patent CN 102863747 disclose a kind of preparation method of High-temperature-reshigh-strength high-strength epoxy foam plastic, and it is formulated
For：Epoxy resin 50~80%, curing agent 10~40%, reinforcing agent 0~30%, foam stabiliser 0.5~5%, foaming agent 0.5
~4%, the epoxy foam being prepared disclosure satisfy that the application demand of hot environment.
The A of patent CN 101289570 describe a kind of preparation method of epoxy soybean oil resin based rigid cellular plastic, with
Epoxy soybean oil resin, vinyl monomer and foaming agent etc. are raw material, and it is 0.1~0.3g/cm that density, which is prepared,-3, compression is by force
Spend the thermosetting rigid foam for 0.3~3.5MPa.
The A of patent CN 106279605 disclose a kind of preparation method of polyurethane foam heat insulation material, with toluene diisocyanate
Acid esters, biobased polyether polyol, sorbeth and Sucrose polyethers etc. are raw material, and obtained polyurethane heat insulation material has strong
Degree height, light weight, heat conduction is low, dimensional stability is good, insulation effect is good, wear-and corrosion-resistant is good, also has efficient fire-retardant energy
Power.
The above-mentioned method for preparing epoxy foams has used petroleum-based feedstock, and complex process, equipment requirement are high.
The content of the invention
The present invention provides a kind of abietyl epoxy foam insulation material and preparation method thereof, is entirely different with prior art
The epoxy foam insulation material of design, the application are that raw material prepares abietyl epoxy foam by vegetable fat and rosin derivative
Material, and overcome complex process in the prior art and it is not biodegradable the defects of.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of preparation method of abietyl epoxy foam insulation material, by vegetable fat and rosin derivative reaction preparation
Into.
The present invention using rosin derivative and epoxidized vegetable oil fat as raw material, with source is wide, price is low, it is degradable,
Synthesis condition is gentle, environmental pollution is small, preparation technology is simple and the advantages that meeting sustainable development.The abietyl being prepared
Epoxy foam insulation material density is 0.120~0.361g/cm3, compressive strength (σ 0.01) is 0.183~1.068MPa, heat conduction
Coefficient is 0.021~0.061W/mk.
In order to further improve the mechanical property of resulting materials and heat-proof quality, above-mentioned abietyl epoxy foam insulation material
Preparation method, including following steps connected in order：
(1) by rosin derivative and epoxidized vegetable oil liposoluble in organic solvent, catalyst and foaming agent are added, mixing is equal
It is even；
(2) after the mixed system obtained by step (1) being removed into solvent, at 130~150 DEG C, after reacting 2~6h, cooling
To room temperature demoulding, abietyl epoxy foam insulation material is produced.
In step (1), rosin derivative is at least one of maleopimaric acid, rosin acrylic acid or fumaropimaric acid,
The mass concentration of rosin derivative raw material in organic solvent is 0.05~0.3g/mL.The thermal insulation of resulting materials can so be made
Can further it be lifted.
In step (1), the mass concentration of rosin derivative raw material in organic solvent is 0.1~0.2g/mL.It can so enter
One step improves the reactivity of rosin derivative and epoxidized vegetable oil fat.Step (1) can make material more by the use of organic solvent
Add uniform mixing.
Epoxy foams initial pyrolyzation temperature scope prepared by the application is at 350~360 DEG C, density 0.765g/
cm3When, compressive strength can reach 15.351MPa.
In step (1), epoxidized vegetable oil fat be epoxy castor oil, epoxidized soybean oil, epoxy palm oil, epoxy olive oil,
Epoxy corn oil, epoxy Chinese catalpa oil, at least one of epoxy peanut oil or epoxy castor oil, the quality dosage of epoxidized vegetable oil fat is pine
0.5~5 times of fragrant derivative material quality, the epoxide number scope of epoxidized vegetable oil fat is 3~7%.So can further it improve
The mechanical property and heat endurance of resulting materials.
The oily epoxy in vegetable oil lipid rapeseed oil, peanut oil, Semen setariae oil, soybean oil, palm oil, tung oil, castor oil or Chinese catalpa
Change process is to be prepared with reference to existing method, and epoxidized soybean oil is bought for Shanghai Jing Chun biochemical technologies limited company, so
It not only ensure that raw material is cheap and easy to get, and further ensure the degree of purity of raw material in technique.
Further preferably, the epoxide number scope of epoxidised vegetable grease is 4.2~6.2%.Resulting materials can so be made
Mechanical property must play more preferable guarantee.
In step (1), catalyst is at least one of 4-methylimidazole or N, N- dimethyl benzylamine, the quality of catalyst
Dosage is 0.001~0.05 times of rosin derivative material quality.It is preferred that the quality dosage of catalyst is rosin derivative raw material
0.005~0.02 times of quality.So can further catalytic reaction efficiency.
In step (1), organic solvent is at least one of absolute ethyl alcohol, methanol or acetone.So can further it improve
The reactivity of rosin derivative and epoxidized vegetable oil fat.
In step (1), foaming agent is at least one of calcium carbonate, magnesium carbonate or sodium acid carbonate, and the quality of foaming agent is used
Measure as 0.01~0.1 times of rosin derivative material quality.It is preferred that the quality dosage of foaming agent is rosin derivative material quality
0.02~0.07 times.Foaming effect can be so further ensured that, while ensures the mechanical performance and heat-proof quality of resulting materials.
As the abietyl epoxy foam insulation material prepared by the preparation method of above-mentioned abietyl epoxy foam insulation material
Density be 0.100~0.800g/cm3, for initial pyrolyzation temperature scope at 350~360 DEG C, compressive strength strains bar 10%
(σ 0.01) is 0.183~1.068MPa under part, compressive strength (σ 0.50) under 50% strained condition is 2.548~
15.351MPa, thermal conductivity factor are 0.021~0.061W/mk.
The NM technology of the present invention is with reference to prior art.
The present invention is that raw material prepares abietyl epoxy foams by vegetable fat and rosin derivative, and is overcome existing
Have in technology complex process and it is not biodegradable the defects of, have that raw material sources are wide, price is low, degradable, synthesis condition temperature
With, preparation technology is simple, environmental pollution is small and meets the advantages such as sustainable development, gained abietyl epoxy foam insulation material
Density be 0.100~0.800g/cm3, compressive strength (σ 0.01) under 10% strained condition is 0.183~1.068MPa, pressure
Contracting intensity (σ 0.50) under 50% strained condition is 2.548~15.351MPa, and thermal conductivity factor is 0.021~0.061W/mk.
Brief description of the drawings
Fig. 1 is the electronic photo of the gained abietyl epoxy foams of embodiment 1；
Fig. 2 is the stereoscan photograph of the gained abietyl epoxy foams of embodiment 1；
Fig. 3 is the compression performance picture of the gained abietyl epoxy foams of embodiment 1；
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
Weigh 2g rosin acrylic acids and 3.4g epoxy castor oils (epoxide number 4.2, self-control, bibliography：Huang Xujuan, Liu
Crane, Shang Shibin, the Study on Preparation chemistry of forest product of epoxy dehydrated castor oils is waited with industrial, 2015,35 (4):It is 41-47) molten
In 20g acetone, 25 μ gN, N- dimethylbenzyl amine catalysts and 0.2g magnesium carbonate foaming agents are added, is well mixed.Pass through rotation
After evaporation removes acetone solvent, it is transferred in 130 DEG C of baking ovens, closing baking oven is cooled to room temperature demoulding after being incubated 6h, obtained pine
The density of perfume base epoxy foams is 0.208g/cm3, initial pyrolyzation temperature is 355 DEG C, and compressive strength strains bar 10%
(σ 0.01) is 0.482MPa under part, and compressive strength (σ 0.50) under 50% strained condition is 12.210MPa, and thermal conductivity factor is
0.043W/m·k。
Embodiment 2
Weighing 2g fumaropimaric acids and 2.72g epoxidized soybean oils, (epoxide number 5.4, the brilliant pure biochemical technology share in Shanghai have
Limit company) it is dissolved in 10g absolute ethyl alcohols, 47 μ g 4-methylimidazoles catalyst and 0.1g sodium acid carbonate foaming agents are added, mixing is equal
It is even.After removing alcohol solvent by rotary evaporation, it is transferred in 140 DEG C of baking ovens, closing baking oven is cooled to room temperature and taken off after insulation 4h
Film, the density of obtained abietyl epoxy foams is 0.462g/cm3, initial pyrolyzation temperature is 354 DEG C, compressive strength
(σ 0.01) is 0.620MPa under 10% strained condition, and compressive strength (σ 0.50) under 50% strained condition is 13.522MPa,
Thermal conductivity factor is 0.046W/mk.
Embodiment 3
Weigh 3g maleopimaric acids and 6g epoxidized soybean oils (epoxide number 6.2, the brilliant pure limited public affairs of biochemical technology share in Shanghai
Department) it is dissolved in 10g acetone, 90 μ g N, N- dimethylbenzyl amine catalysts and 0.3g sodium acid carbonate foaming agents are added, is well mixed.
After removing acetone solvent by rotary evaporation, it is transferred in 150 DEG C of baking ovens, closing baking oven is cooled to room temperature demoulding after being incubated 2h,
The density of obtained abietyl epoxy foams is 0.129g/cm3, initial pyrolyzation temperature is 358 DEG C, and compressive strength exists
(σ 0.01) is 0.425MPa under 10% strained condition, and compressive strength (σ 0.50) under 50% strained condition is 10.521MPa, is led
Hot coefficient is 0.021W/mk.
Embodiment 4
Weigh 5g fumaropimaric acids and 2.5g epoxy castor oils (epoxide number 4.5, self-control, bibliography：Ma Junhui epoxies
Tung oil study on the synthesis [J] Sichuan chemical industry, 1995,4:5-10) it is dissolved in 20g absolute ethyl alcohols, adds 25 μ g 4-methylimidazole amine
Catalyst and 0.1g calcium carbonate foaming agents, it is well mixed.After removing alcohol solvent by rotary evaporation, 135 DEG C of baking ovens are transferred to
In, closing baking oven is cooled to room temperature demoulding after being incubated 3h, and the density of obtained abietyl epoxy foams is 0.765g/cm3,
Initial pyrolyzation temperature is 350 DEG C, and compressive strength (σ 0.01) under 10% strained condition is 1.068MPa, and compressive strength exists
(σ 0.50) is 15.351MPa, thermal conductivity factor 0.033W/mk under 50% strained condition.
Embodiment 5
Weigh 5g rosin acrylic acids and 5g epoxies peanut oil (epoxide number 4.8, self-control, bibliography：Guo Zhifang, Yang Wen
Cloud tints, float research [J] the grains and grease of cry of certain animals plum chemical method catalysis peanut oil epoxidation techniques, 2016,29 (10):It is 35-37) molten
In 20g pyruvic alcohols, 30 μ g N, N- dimethylbenzyl amine catalysts and 0.75g sodium acid carbonate foaming agents are added, is well mixed.It is logical
After crossing rotary evaporation removing acetone solvent, it is transferred in 145 DEG C of baking ovens, closing baking oven is cooled to room temperature demoulding after being incubated 5h, obtains
The density of the abietyl epoxy foams arrived is 0.125g/cm3, initial pyrolyzation temperature is 352 DEG C, and compressive strength is 10%
(σ 0.01) is 0.573MPa under strained condition, and compressive strength (σ 0.50) under 50% strained condition is 11.858MPa, heat conduction system
Number is 0.032W/mk.
Claims (10)
- A kind of 1. preparation method of abietyl epoxy foam insulation material, it is characterised in that：By vegetable fat and rosin derivative Reaction is prepared.
- 2. the preparation method of abietyl epoxy foam insulation material as claimed in claim 1, it is characterised in that：Including order The following steps to connect：(1) by rosin derivative and epoxidized vegetable oil liposoluble in organic solvent, catalyst and foaming agent are added, is well mixed；(2) after the mixed system obtained by step (1) being removed into solvent, at 130~150 DEG C, after reacting 2~6h, it is cooled to room Warm demoulding, produce abietyl epoxy foam insulation material.
- 3. the preparation method of abietyl epoxy foam insulation material as claimed in claim 2, it is characterised in that：Step (1) In, rosin derivative is at least one of maleopimaric acid, rosin acrylic acid or fumaropimaric acid, and rosin derivative raw material exists Mass concentration in organic solvent is 0.05~0.3g/mL.
- 4. the preparation method of abietyl epoxy foam insulation material as claimed in claim 3, it is characterised in that：Step (1) In, the mass concentration of rosin derivative raw material in organic solvent is 0.1~0.2g/mL.
- 5. the preparation method of the abietyl epoxy foam insulation material as described in claims 2-4 any one, its feature exist In：In step (1), epoxidized vegetable oil fat is epoxy castor oil, epoxidized soybean oil, epoxy palm oil, epoxy olive oil, epoxy jade Rice bran oil, epoxy Chinese catalpa oil, at least one of epoxy peanut oil or epoxy castor oil, the quality dosage of epoxidized vegetable oil fat is rosin derivative 0.5~5 times of raw material quality, the epoxide number scope of epoxidized vegetable oil fat is 3~7%.
- 6. the preparation method of abietyl epoxy foam insulation material as claimed in claim 5, it is characterised in that：Epoxidation is planted The epoxide number scope of thing grease is 4.2~6.2%.
- 7. the preparation method of the abietyl epoxy foam insulation material as described in claims 2-4 any one, its feature exist In：In step (1), catalyst is at least one of 4-methylimidazole or N, N- dimethyl benzylamine, the quality dosage of catalyst For 0.001~0.05 times of rosin derivative material quality.
- 8. the preparation method of the abietyl epoxy foam insulation material as described in claims 2-4 any one, its feature exist In：In step (1), organic solvent is at least one of absolute ethyl alcohol, methanol or acetone.
- 9. the preparation method of the abietyl epoxy foam insulation material as described in claims 2-4 any one, its feature exist In：In step (1), foaming agent is at least one of calcium carbonate, magnesium carbonate or sodium acid carbonate, and the quality dosage of foaming agent is pine 0.01~0.1 times of fragrant derivative material quality.
- 10. as prepared by the preparation method of the abietyl epoxy foam insulation material described in claims 1-9 any one Abietyl epoxy foam insulation material, it is characterised in that：The density of abietyl epoxy foam insulation material be 0.100~ 0.800g/cm3, initial pyrolyzation temperature scope is in 350~360 DEG C, compressive strength (σ 0.01) under 10% strained condition 0.183~1.068MPa, compressive strength (σ 0.50) under 50% strained condition is 2.548~15.351MPa, and thermal conductivity factor is 0.021~0.061W/mk.
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| CN201710913155.8A CN107602868B (en) | 2017-09-30 | 2017-09-30 | Rosin-based epoxy foam thermal insulation material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710913155.8A CN107602868B (en) | 2017-09-30 | 2017-09-30 | Rosin-based epoxy foam thermal insulation material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423334A (en) * | 2019-08-08 | 2019-11-08 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of full biology base vitrimer |
| CN112225712A (en) * | 2020-09-24 | 2021-01-15 | 仲恺农业工程学院 | Epoxidized soybean oil propylene pimaric acid ester and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423334A (en) * | 2019-08-08 | 2019-11-08 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of full biology base vitrimer |
| CN110423334B (en) * | 2019-08-08 | 2022-01-11 | 中国林业科学研究院林产化学工业研究所 | Preparation method of total-organism-based vitrimer |
| CN112225712A (en) * | 2020-09-24 | 2021-01-15 | 仲恺农业工程学院 | Epoxidized soybean oil propylene pimaric acid ester and preparation method and application thereof |
| CN112225712B (en) * | 2020-09-24 | 2023-02-03 | 仲恺农业工程学院 | Epoxidized soybean oil propylene pimaric acid ester and preparation method and application thereof |
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