CN108752943A - A kind of preparation method of epoxy resin-matrix ambroin - Google Patents
A kind of preparation method of epoxy resin-matrix ambroin Download PDFInfo
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- CN108752943A CN108752943A CN201810505046.7A CN201810505046A CN108752943A CN 108752943 A CN108752943 A CN 108752943A CN 201810505046 A CN201810505046 A CN 201810505046A CN 108752943 A CN108752943 A CN 108752943A
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- Prior art keywords
- amber
- resin
- ambroin
- mixed system
- matrix
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 53
- 239000011159 matrix material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229940106691 bisphenol a Drugs 0.000 claims abstract description 20
- 229920006387 Vinylite Polymers 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 14
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 5
- HZEOUPCNUWSUFL-UHFFFAOYSA-N 4,5,5-trimethyl-4-pentan-3-yl-1H-imidazole Chemical class C(C)C(C1(N=CNC1(C)C)C)CC HZEOUPCNUWSUFL-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 238000004382 potting Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000006188 syrup Substances 0.000 description 4
- 235000020357 syrup Nutrition 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 230000002547 anomalous effect Effects 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000000386 microscopy Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 230000003749 cleanliness Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- ZYUVGYBAPZYKSA-UHFFFAOYSA-N 5-(3-hydroxybutan-2-yl)-4-methylbenzene-1,3-diol Chemical compound CC(O)C(C)C1=CC(O)=CC(O)=C1C ZYUVGYBAPZYKSA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- NHADDZMCASKINP-HTRCEHHLSA-N decarboxydihydrocitrinin Natural products C1=C(O)C(C)=C2[C@H](C)[C@@H](C)OCC2=C1O NHADDZMCASKINP-HTRCEHHLSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L93/00—Compositions of natural resins; Compositions of derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to a kind of preparation methods of epoxy resin-matrix ambroin, belong to ambroin technical field.The present invention cleans amber particle, ball milling powdering；Temperature be 35 ~ 45 DEG C under the conditions of, by trimethylolpropane be added in bisphenol-A epoxy vinylite and be uniformly mixed obtain resin mixed system A；High-temperature curing agent is added to be uniformly mixed in mixed system A and obtains resin mixed system B；Amber powder is added to be uniformly mixed in resin mixed system B and obtains resin-amber mixed system, it is subsequently placed in centrifuge and 8000 ~ 10000rmp centrifugation 1 ~ 2h discharge bubbles is set, resin-amber mixed system is placed under inert atmosphere or vacuum condition again, is fired when being at the uniform velocity warming up to 250 ~ 300 DEG C（Anaerobic）2 ~ 4h keeps inert atmosphere or vacuum condition furnace cooling up to epoxy resin-matrix ambroin.The present invention prepares epoxy resin-matrix ambroin using natural amber, bisphenol-A epoxy vinylite as raw material, appearance and context of detection with natural amber no significant difference.
Description
Technical field
The present invention relates to a kind of preparation methods of epoxy resin-matrix ambroin, belong to ambroin technical field.
Background technology
Natural amber is constantly subjected to liking for people with its distinctive external effect with inherent value, also there is utilization in the market
Epoxy resin makes some artificial amber products.Artificial amber is shape by the macromolecule resin package inner matter of the high grade of transparency
At having many advantages, such as true nature, glittering and translucent.But due in the manufacturing process of artificial amber, especially in large-sized artificial
In the preparation process of amber, when pouring into a mould potting syrup, inner matter moves under the impact of potting syrup, and product figure is made to lose
Very, and interiors of products is caused bubble and slight crack occur.
The patent document of Patent No. 201210287603.5 discloses a kind of artificial amber preparation method, and providing one has
The transparent bounding box of host cavity；Inner matter is bonded in by shadowless glue on the internal chamber wall of the host cavity, and is shone by ultraviolet light
Penetrating makes the shadowless glue cure；Potting syrup is poured into the host cavity, and makes its solidification.Above-mentioned artificial amber preparation side
In method, inner matter is bonded in by shadowless glue on the internal chamber wall of host cavity, and shadowless glue is made to cure under ultraviolet irradiation,
To which when being poured into a mould, inner matter position under the impact of potting syrup is still kept fixed, and meets the design requirement of product.
But the artificial amber in the invention and natural amber are only used for the decoration of low side without something in common.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of epoxy resin-matrix ambroin, the present invention
Prepare epoxy resin-matrix ambroin as raw material using natural amber, bisphenol-A epoxy vinylite, appearance and context of detection with
The equal no significant difference of natural amber, cleanliness is very high, gloss is fine, and shape is unrestricted, and cheap, is easily processed into all kinds of
Craftwork.
A kind of preparation method of epoxy resin-matrix ambroin, the specific steps are：
（1）Amber particle is cleaned, ball milling powdering；
（2）Under the conditions of temperature is 35 ~ 45 DEG C, trimethylolpropane is added in bisphenol-A epoxy vinylite and is mixed
Uniformly obtain resin mixed system A；
（3）High-temperature curing agent is added to step（2）It is uniformly mixed in mixed system A and obtains resin mixed system B；
（4）By step（1）Gained amber powder is added to step（3）It is uniformly mixed in gained resin mixed system B and obtains resin-
Amber mixed system is subsequently placed in rotating speed and is that 8000 ~ 10000rmp centrifuges 1 ~ 2h is discharged bubble, then by resin-amber
Mixed system, which is placed under inert atmosphere or vacuum condition, is at the uniform velocity warming up to 250 ~ 300 DEG C, carries out anaerobic and fires 2 ~ 4h, keeps inertia
Atmosphere or vacuum condition furnace cooling are up to epoxy resin-matrix ambroin；
The step（3）High temperature curing agent be methylnadic anhydride and diethyl tetramethyl imidazoles using arbitrary mass ratio into
The mixed mixture of row；
The amber powder, bisphenol-A epoxy vinylite, high-temperature curing agent mass ratio be (2 ~ 5):1:(0.8 ~ 1.5), it is double
The mass ratio of phenol A epoxy vingl ester resins and trimethylolpropane is 1:(0.03~0.1)；
Preferably, bisphenol-A epoxy vinylite is bisphenol-A epoxy vinylite 907；
Preferably, step（4）In the rate that at the uniform velocity heats up be 2 ~ 5 DEG C/min.
Beneficial effects of the present invention：
（1）The present invention prepares epoxy resin-matrix ambroin, epoxy using natural amber, bisphenol-A epoxy vinylite as raw material
Bubble-free, free from admixture in resin base ambroin, cleanliness is very high, glossiness is fine and shape is unrestricted；
（2）The method of the present invention prepares color, density, refractive index and the Ultraluminescence testing result of epoxy resin-matrix ambroin
With the equal no significant difference of natural amber；
（3）The method of the present invention ambroin is prepared simply, and operation is easy, and of low cost, composite stable structure is specious,
It is nontoxic, there is very high value, is suitable for industrial production.
Specific implementation mode
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1：A kind of preparation method of epoxy resin-matrix ambroin, the specific steps are：
（1）Amber particle is cleaned, ball milling 20h obtains amber powder；
（2）Under the conditions of temperature is 35 DEG C, trimethylolpropane is added in bisphenol-A epoxy vinylite and is uniformly mixed
Obtain resin mixed system A；Wherein the mass ratio of bisphenol-A epoxy vinylite and trimethylolpropane is 1:0.03；
（3）High-temperature curing agent is added to step（2）It is uniformly mixed in mixed system A and obtains resin mixed system B；Its high temperature
It according to mass ratio is 1 that curing agent, which is methylnadic anhydride and diethyl tetramethyl imidazoles,:The mixing that 1 ratio is mixed
Object；
（4）By step（1）Gained amber powder is added to step（3）It is uniformly mixed in gained resin mixed system B and obtains resin-
Amber mixed system, is subsequently placed in centrifuge, and centrifugation 2h is discharged bubble under the conditions of 8000rmp, then by resin-amber mixed system
It is placed in atmosphere furnace and passes to nitrogen, 2 DEG C/min keeps the temperature 4h after being warming up to 250 DEG C, keep inert atmosphere（Nitrogen）Under the conditions of with furnace cooling
But up to epoxy resin-matrix ambroin；The wherein mass ratio of amber powder, bisphenol-A epoxy vinylite, high-temperature curing agent
It is 2:1:0.8；
Refractive index, density, color and the Ultraluminescence of the present embodiment epoxy resin-matrix ambroin, polariscope and amplification microscopy
Survey that the results are shown in Table 1, as known from Table 1, natural amber is brown color, refractive index 1.540, and density is set as 1, and Ultraluminescence is shone
Aobvious blue, polariscope are detected as anomalous extinction and interference colours, amplify in sem observation natural amber that there are a large amount of cracks and impurity；Ring
Epoxy resin-based ambroin is brown color, refractive index 1.496, relative density（Relative to natural amber）It is 1.05, it is ultraviolet glimmering
The aobvious blue of light irradiation, polariscope are detected as all light, amplify and contain trace impurity in sem observation epoxy resin-matrix ambroin.
Embodiment 2：A kind of preparation method of epoxy resin-matrix ambroin, the specific steps are：
（1）Amber particle is cleaned, ball milling 10h obtains amber powder；
（2）Under the conditions of temperature is 40 DEG C, trimethylolpropane is added in bisphenol-A epoxy vinylite and is uniformly mixed
Obtain resin mixed system A；Wherein the mass ratio of bisphenol-A epoxy vinylite and trimethylolpropane is 1:0.08；
（3）High-temperature curing agent is added to step（2）It is uniformly mixed in mixed system A and obtains resin mixed system B；Its high temperature
It according to mass ratio is 1 that curing agent, which is methylnadic anhydride and diethyl tetramethyl imidazoles,:The mixing that 2 ratio is mixed
Object；
（4）By step（1）Gained amber powder is added to step（3）It is uniformly mixed in gained resin mixed system B and obtains resin-
Amber mixed system, is subsequently placed in centrifuge, and centrifugation 1.5h is discharged bubble under the conditions of 9000rmp, then by resin-amber mixture
System is placed in atmosphere furnace and passes to helium, and 3 DEG C/min keeps the temperature 3h after being warming up to 280 DEG C, keep inert atmosphere（Helium）Under the conditions of with stove
Cooling epoxy resin-matrix ambroin to obtain the final product；The wherein quality of amber powder, bisphenol-A epoxy vinylite, high-temperature curing agent
Than being 5:1:1.5；
Refractive index, density, color and the Ultraluminescence of the present embodiment epoxy resin-matrix ambroin, polariscope and amplification microscopy
Survey that the results are shown in Table 1, as known from Table 1, natural amber is brown color, refractive index 1.540, and density is set as 1, and Ultraluminescence is shone
Aobvious blue is penetrated, polariscope is detected as anomalous extinction and interference colours, amplifies in sem observation natural amber that there are a large amount of cracks and impurity；
Epoxy resin-matrix ambroin is brown color, refractive index 1.517, relative density（Relative to natural amber）It is 1.07, it is ultraviolet
The aobvious blue of fluorescent lamp, polariscope are detected as all light, amplify and contain trace impurity in sem observation epoxy resin-matrix ambroin.
Embodiment 3：A kind of preparation method of epoxy resin-matrix ambroin, the specific steps are：
（1）Amber particle is cleaned, ball milling 15h obtains amber powder；
（2）Under the conditions of temperature is 45 DEG C, trimethylolpropane is added in bisphenol-A epoxy vinylite and is uniformly mixed
Obtain resin mixed system A；Wherein the mass ratio of bisphenol-A epoxy vinylite and trimethylolpropane is 1:0.1；
（3）High-temperature curing agent is added to step（2）It is uniformly mixed in mixed system A and obtains resin mixed system B；Its high temperature
It according to mass ratio is 2 that curing agent, which is methylnadic anhydride and diethyl tetramethyl imidazoles,:The mixing that 1 ratio is mixed
Object；
（4）By step（1）Gained amber powder is added to step（3）It is uniformly mixed in gained resin mixed system B and obtains resin-
Amber mixed system, is subsequently placed in centrifuge, and centrifugation 1h is discharged bubble under the conditions of 10000rmp, then by resin-amber mixture
System is placed in vacuum drying oven, and 5 DEG C/min keeps vacuum condition to fire 2h after being warming up to 300 DEG C, furnace cooling is closed up to epoxy resin-matrix
At amber；Wherein amber powder, bisphenol-A epoxy vinylite, high-temperature curing agent mass ratio be 3.5:1:1；
Refractive index, density, color and the Ultraluminescence of the present embodiment epoxy resin-matrix ambroin, polariscope and amplification microscopy
The results are shown in Table 1 for survey,
1 epoxy resin-matrix ambroin of table and natural amber testing result
As known from Table 1, natural amber is brown color, refractive index 1.540, and density is set as 1, the aobvious blue of Ultraluminescence irradiation, partially
Light microscopic is detected as anomalous extinction and interference colours, amplifies in sem observation natural amber that there are a large amount of cracks and impurity；Epoxy resin-matrix
Ambroin is brown color, refractive index 1.535, relative density（Relative to natural amber）It is 1.08, Ultraluminescence irradiation is aobvious
Blue, polariscope are detected as all light, amplify and contain trace impurity in sem observation epoxy resin-matrix ambroin.
Claims (3)
1. a kind of preparation method of epoxy resin-matrix ambroin, which is characterized in that the specific steps are：
（1）Amber particle is cleaned, ball milling powdering；
（2）Under the conditions of temperature is 35 ~ 45 DEG C, trimethylolpropane is added in bisphenol-A epoxy vinylite and is mixed
Uniformly obtain resin mixed system A；
（3）High-temperature curing agent is added to step（2）It is uniformly mixed in mixed system A and obtains resin mixed system B；
（4）By step（1）Gained amber powder is added to step（3）It is uniformly mixed in gained resin mixed system B and obtains resin-
Amber mixed system, is subsequently placed in centrifuge, and 8000 ~ 10000rmp of setting centrifuges 1 ~ 2h to be discharged bubble, then by resin-amber
Amber mixed system, which is placed under inert atmosphere or vacuum condition, is at the uniform velocity warming up to 250 ~ 300 DEG C, carries out anaerobic and fires 2 ~ 4h, keeps lazy
Furnace cooling is up to epoxy resin-matrix ambroin under property atmosphere or vacuum condition.
2. the preparation method of epoxy resin-matrix ambroin according to claim 1, it is characterised in that：Step（3）High temperature
Curing agent is the mixture of methylnadic anhydride and diethyl tetramethyl imidazoles.
3. the preparation method of epoxy resin-matrix ambroin according to claim 1, it is characterised in that：Amber powder, bisphenol-A
Epoxy vingl ester resin, high-temperature curing agent mass ratio be (2 ~ 5):1:(0.8 ~ 1.5), bisphenol-A epoxy vinylite and three
The mass ratio of hydroxymethyl-propane is 1:(0.03~0.1).
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| CN201810505046.7A CN108752943A (en) | 2018-05-24 | 2018-05-24 | A kind of preparation method of epoxy resin-matrix ambroin |
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| CN201810505046.7A CN108752943A (en) | 2018-05-24 | 2018-05-24 | A kind of preparation method of epoxy resin-matrix ambroin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1603362A (en) * | 2003-09-29 | 2005-04-06 | 颜长硕 | Artificial amber and its making process |
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| CN102863332A (en) * | 2012-09-27 | 2013-01-09 | 昆明理工大学 | Organic amber and preparation method thereof |
| CN103059515A (en) * | 2012-12-20 | 2013-04-24 | 桂林电器科学研究院 | Vinyl ester resin modified epoxy pouring sealant and preparation method thereof |
| CN103554839A (en) * | 2013-11-07 | 2014-02-05 | 哈尔滨工业大学 | Motor retaining ring made from carbon fiber composite material |
| CN103819877A (en) * | 2014-03-20 | 2014-05-28 | 哈尔滨工业大学 | Hybrid fiber composite material motor guard ring |
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2018
- 2018-05-24 CN CN201810505046.7A patent/CN108752943A/en active Pending
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|---|---|---|---|---|
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| CN102863332A (en) * | 2012-09-27 | 2013-01-09 | 昆明理工大学 | Organic amber and preparation method thereof |
| CN103059515A (en) * | 2012-12-20 | 2013-04-24 | 桂林电器科学研究院 | Vinyl ester resin modified epoxy pouring sealant and preparation method thereof |
| CN103554839A (en) * | 2013-11-07 | 2014-02-05 | 哈尔滨工业大学 | Motor retaining ring made from carbon fiber composite material |
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Application publication date: 20181106 |
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