CN108041779A - A kind of amber optimization method based on supercritical fluid technique - Google Patents
A kind of amber optimization method based on supercritical fluid technique Download PDFInfo
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- CN108041779A CN108041779A CN201711225193.0A CN201711225193A CN108041779A CN 108041779 A CN108041779 A CN 108041779A CN 201711225193 A CN201711225193 A CN 201711225193A CN 108041779 A CN108041779 A CN 108041779A
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- amber
- supercritical fluid
- optimization method
- method based
- supercritical
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000012530 fluid Substances 0.000 title claims abstract description 40
- 238000005457 optimization Methods 0.000 title claims abstract description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 35
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000013871 bee wax Nutrition 0.000 claims abstract description 30
- 239000012166 beeswax Substances 0.000 claims abstract description 30
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 17
- 239000004575 stone Substances 0.000 claims abstract description 11
- 238000001764 infiltration Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims abstract description 3
- 238000005498 polishing Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 5
- 230000008595 infiltration Effects 0.000 claims description 5
- 230000008961 swelling Effects 0.000 claims description 5
- 238000005422 blasting Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000004031 devitrification Methods 0.000 abstract description 6
- 238000005187 foaming Methods 0.000 abstract description 3
- 239000010437 gem Substances 0.000 abstract description 3
- 229910001751 gemstone Inorganic materials 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 229920002892 amber Polymers 0.000 description 76
- 238000013461 design Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 210000000497 foam cell Anatomy 0.000 description 3
- 239000008240 homogeneous mixture Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 241000580063 Ipomopsis rubra Species 0.000 description 1
- 241000218633 Pinidae Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A44—HABERDASHERY; JEWELLERY
- A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
- A44C27/00—Making jewellery or other personal adornments
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention belongs to the technical fields of gemstone treatment, disclose a kind of amber optimization method based on supercritical fluid technique.The method is：(1) amber original stone is pre-processed, the amber pre-processed；(2) amber of pretreatment being placed in autoclave, is emptied using carbon dioxide, enclosed high pressure reaction kettle is passed through high-pressure carbon dioxide, is warming up to 100 DEG C~180 DEG C, when pressure is 8~12MPa in autoclave, supercritical CO2It is formed, amber is in supercritical CO2Infiltration, pressure release are swollen in environment, cooling obtains beeswax.The method of the present invention is simple, efficiently, influence is had no on the chemical composition of amber in itself, greatly reduces the transparency of amber, significant effect；Used carbon dioxide non-toxic and safe, realizes environmentally protective foaming；And the method for the present invention reduces amber glass temperature, and formation bubble distribution is uniform, has good reflection to form milkiness devitrification effect to visible ray.
Description
Technical field
The invention belongs to the enhancement and treatment fields of jewel, and in particular to a kind of to change amber using supercritical fluid technique
The optimization method of amber opacity.
Technical background
Amber is that the resin of the Cretaceous period to Tertiary Period coniferale plant of new generation is formed after a series of geologic processes
A kind of natural organic petrochemical resins are a kind of precious and ancient organic gemstone.In recent years and because of its unique cultural connotation and
The propagation of capital, amber are subject to higher to pay close attention in recent years, and the trend that skyrockets is presented in price.Since the value of amber is high, demand
Greatly, less varieties, and be non-renewable resources, as the main object of enhancement and treatment tackling key problem.
And now very powerful and exceedingly arrogant commercial variety, beeswax, refer to translucent to opaque amber, opaqueness be by
Internal substantial amounts of micro-bubble causes the reflection and scattering process of incident light.Because its is rarity, buddhism culture and commercial speculation
Etc. under factors collective effect, the Chinese market high praise excessive to beeswax and the extreme consumption of consumer artificially cause beeswax original
Material price goes up.And the opacity of beeswax is as caused by internal micro-bubble to the diffusing scattering effect of light, in amber
Portion's ingredient is simultaneously irrelevant.
In face of growing market, a kind of side that clear amber can be changed into effectively to opaque beeswax is looked for
Method is necessary, realizes the transformation of amber transparency, makes full use of natural resources so as to meet Jewelry Market to greatest extent
It needs.
The content of the invention
In view of the shortage of existing amber optimizing research and for overcome the deficiencies in the prior art, the object of the present invention is to provide
A kind of amber optimization method based on supercritical fluid technique.
The purpose of the present invention is achieved through the following technical solutions：
A kind of amber optimization method based on supercritical fluid technique, comprises the following steps：
(1) amber original stone is pre-processed, the amber pre-processed；
(2) amber of pretreatment is placed in autoclave, is emptied using carbon dioxide, enclosed high pressure reaction kettle leads to
Enter high-pressure carbon dioxide, be warming up to 100 DEG C~180 DEG C, when pressure is 8~12MPa in autoclave, supercritical CO2Shape
Into amber is in supercritical CO2Infiltration, pressure release are swollen in environment, cooling obtains treated amber, that is, beeswax.
The time that infiltration is swollen described in step (2) is 3~12h.
Pretreatment refers to amber original stone carrying out polishing peeling described in step (1), cuts, and cleans, drying, obtains pre- place
The amber of reason；The pretreatment is processed by shot blasting after further including polishing, in particular to cutting.The temperature of the drying is 25 DEG C
~50 DEG C.
Amber minimum dimension >=the 2mm pre-processed described in step (1), minimum dimension is preferably 2~50mm, more preferably
2~10mm；
The amber of the pretreatment is preferably sheet or bulk；
The thickness of the amber of the sheet is 2~50mm, is preferably 2~10mm；
Amber described in step (1) is preferably the amber in Baltic Sea area.
The supercritical fluid of the present invention refers to that temperature is higher than the critical-temperature of fluid, while pressure is higher than its critical pressure
Power.Supercritical CO is used in the present invention2, purity 99.9%, super critical condition is that temperature is more than 31.1 DEG C, and pressure is higher than
7.4MPa。
Compared with prior art, the invention has the advantages that：
(1) compared with existing amber optimize technique, the present invention, as medium, does not change amber in itself using carbon dioxide
Chemical constitution property, be not introduced into other organic principles, it is notable to amber appearance transparence modified effect, it is seen that the percent of pass of light
Greatly reduce；
(2) present invention utilizes swelling osmotic effect of the supercritical carbon dioxide to polymer, reduces amber glass temperature,
It is uniform to form bubble distribution, has good reflection to form milkiness devitrification effect to visible ray；
(3) in processing procedure of the present invention using non-toxic inexpensive, environmental-friendly carbon dioxide as medium, use is intermittent
Foaming adjusting process shortens the amber optimization time, and treatment process is simple and efficient, and equipment is simple, and energy consumption is few.
Description of the drawings
Fig. 1 is the supercritical reaction apparatus schematic diagram of Examples 1 to 3；
Fig. 2 is design sketch of the amber before and after treatment with supercritical fluid；Wherein (A) is clear amber at supercritical fluid
The design sketch under front-reflection light is managed, (B) is design sketch of the clear amber before treatment with supercritical fluid under transmitted light, and (C) is
The design sketch of the beeswax that bright amber is formed after treatment with supercritical fluid under reflected light, (D) are clear ambers in shooting flow
The design sketch of the beeswax formed after body processing in transmitted light；
Fig. 3 is ultraviolet-visible spectrogram of the amber of embodiment 1 before and after treatment with supercritical fluid；Wherein clear amber pair
Before answering treatment with supercritical fluid, after beeswax corresponds to treatment with supercritical fluid；
Fig. 4 is the infrared spectrogram of beeswax, natural amber and natural beeswax prepared by embodiment 2；
Fig. 5 is the SEM figures of its section of beeswax prepared by embodiment 3.
Specific embodiment
The present invention is described in further detail with reference to embodiment and attached drawing, but embodiments of the present invention are unlimited
In this.Amber used is selected from Ukraine area in the present invention, belongs to typical Baltic amber.CO used2Medium
Purity is up to more than 99.9%.
The optimization method of Examples 1 to 3 uses device (i.e. supercritical reaction apparatus) schematic diagram as shown in Figure 1, described
Device includes autoclave, heating unit (aluminum alloy heating furnace) and CO2Gas bomb (carbon dioxide steel cylinder), the high pressure are anti-
Kettle is answered to be placed in heating unit, the top of autoclave is equipped with through hole, passes through gas pipeline (high-pressure metal pipe) and CO2Gas storage
Bottle connects, and is disposed with valve 2, pressure gauge, booster pump, valve 1 on gas pipeline, valve 1 is close to CO2Gas bomb；It is described
Device further includes relief valve, and relief valve is connected by efferent duct with the through hole at the top of autoclave；The heating unit with can
The connection of high accuracy temperature control instrument is programmed, height is further controlled by the heating condition that may be programmed high accuracy temperature control instrument control refrigerating/heating apparatus
The temperature in reaction kettle is pressed, the booster pump is connected with air compressor.The optimization method uses device to include another pressure
Power table, the pressure gauge measure the pressure in autoclave, which is arranged on the through hole of autoclave.
Embodiment 1
A kind of amber optimization method based on supercritical fluid technique, comprises the following steps：
(1) the Baltic amber original stone from the Ukraine place of production is chosen, by amber original stone polishing peeling, cutting, warp
The clear amber thin slice that the smooth thickness in surface is 3mm is obtained after the polishing of 5000 mesh sand paper, cleaning after 50 DEG C of low temperature dryings；
(2) choose 3~4 pieces of clear amber thin slices to be laid in autoclave, closed reactor opens valve (valve 1
With 2) be passed through small flow CO2It purges reaction kettle 1min to replace air in kettle totally, closes relief valve, open booster pump to high pressure
High-pressure carbon dioxide is filled in reaction kettle to 6MPa, closes valve 1, rise autoclave temperature is pressed to 130 DEG C in reaction kettle
Power control is 12MPa, and supercritical carbon dioxide fluid is formed in reaction kettle, when swelling infiltration 5 is small, makes CO2Amber is infiltrated through to gather
It closes in object and forms homogeneous mixture；
(3) and then opening pressure reduction control valve (relief valve) makes in autoclave pressure moment rapidly be depressurized to gauge pressure as 0,
Release CO2Supercriticality, treat that reaction kettle is cooled to less than 50 DEG C, take out after sample can obtain treatment with supercritical fluid
Amber, that is, beeswax, beeswax uniform foam cell, devitrification.
Design sketch of the amber before and after treatment with supercritical fluid be as indicated with 2 in the present embodiment；Wherein (A) is clear amber
The design sketch of (i.e. natural amber) under treatment with supercritical fluid front-reflection light, (B) are clear ambers (i.e. natural amber) super
Design sketch under critical fluids before processing transmitted light, (C) are clear amber (i.e. natural amber) shapes after treatment with supercritical fluid
Into beeswax design sketch under reflected light, (D) is that clear amber (i.e. natural amber) is formed after treatment with supercritical fluid
The design sketch of beeswax in transmitted light.
Ultraviolet-visible spectrogram of the amber before and after treatment with supercritical fluid is as shown in figure 3, clear amber in the present embodiment
Before (i.e. natural amber) corresponding treatment with supercritical fluid, after beeswax corresponds to treatment with supercritical fluid.
The density of beeswax (after supercritical fluid foaming) manufactured in the present embodiment is 0.79g/cm3, to visible light transmittance
Only 0.06%, there is good reflection performance to visible ray, devitrification effect is presented, clear amber is successfully modified by the present invention to be become not
Transparent beeswax kind.
Embodiment 2
A kind of amber optimization method based on supercritical fluid technique, comprises the following steps：
(1) the Baltic amber original stone from the Ukraine place of production is chosen, by amber original stone polishing peeling, cutting, warp
The clear amber thin slice that the smooth thickness in surface is 3mm is obtained after the polishing of 5000 mesh sand paper, cleaning after 50 DEG C of low temperature dryings；
(2) choose 3~4 pieces of clear amber thin slices to be laid in autoclave, closed reactor is opened valve, is passed through
Small flow CO2It purges reaction kettle 1min to replace air in kettle totally, closes relief valve, open booster pump into autoclave
High-pressure carbon dioxide is filled with to 6MPa, closes valve 1, for rise autoclave temperature to 120 DEG C, regulation and control relief valve makes reaction kettle
Middle pressure control is 10MPa, and supercritical carbon dioxide fluid is formed in reaction kettle, when swelling infiltration 3 is small, makes CO2Infiltrate through amber
Homogeneous mixture is formed in amber polymer；
(3) and then opening pressure reduction control valve (relief valve) makes pressure moment in autoclave rapidly be depressurized to gauge pressure as 0
(atmospheric pressure) releases CO2Supercriticality, treat that reaction kettle is cooled to less than 50 DEG C, take out sample can obtain it is overcritical
Fluid treated amber, that is, beeswax, beeswax uniform foam cell, devitrification.
The beeswax of the present embodiment is 8.94% to visible light transmittance.
Beeswax manufactured in the present embodiment, the infrared spectrogram of natural amber and natural beeswax are as shown in Figure 4.
Embodiment 3
A kind of amber optimization method based on supercritical fluid technique, comprises the following steps：
(1) the Baltic amber original stone from the Ukraine place of production is chosen, by amber original stone polishing peeling, cutting, warp
The clear amber thin slice that the smooth thickness in surface is 3mm is obtained after the polishing of 5000 mesh sand paper, cleaning after 50 DEG C of low temperature dryings；
(2) choose 3~4 pieces of clear amber thin slices to be laid in autoclave, closed reactor is opened valve, is passed through
Small flow CO2It purges reaction kettle 1min to replace air in kettle totally, closes relief valve, open booster pump into autoclave
High-pressure carbon dioxide is filled with to 6MPa, closes valve 1, for rise autoclave temperature to 160 DEG C, regulation and control relief valve makes reaction kettle
Middle pressure control is 10MPa, and supercritical carbon dioxide fluid is formed in reaction kettle, when swelling infiltration 5 is small, makes CO2Infiltrate through amber
Homogeneous mixture is formed in amber polymer；
(3) and then opening pressure reduction control valve (relief valve) makes pressure moment in autoclave rapidly be depressurized to gauge pressure as 0
(atmospheric pressure) releases CO2Supercriticality, treat that reaction kettle is cooled to less than 50 DEG C, take out sample can obtain it is overcritical
Fluid treated amber, that is, beeswax, beeswax uniform foam cell, devitrification.
Beeswax manufactured in the present embodiment is 3.23% to visible light transmittance.
The SEM figures of beeswax section manufactured in the present embodiment are as shown in Figure 5.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from the embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of amber optimization method based on supercritical fluid technique, it is characterised in that：Comprise the following steps：
(1) amber original stone is pre-processed, the amber pre-processed；
(2) amber of pretreatment is placed in autoclave, is emptied using carbon dioxide, enclosed high pressure reaction kettle is passed through height
Carbon dioxide is pressed, is warming up to 100 DEG C~180 DEG C, when pressure is 8~12MPa in autoclave, supercritical CO2It is formed, amber
Amber is in supercritical CO2Infiltration, pressure release are swollen in environment, cooling obtains treated amber, that is, beeswax.
2. the amber optimization method based on supercritical fluid technique according to claim 1, it is characterised in that：In step (2)
The time of the swelling infiltration is 3~12h.
3. the amber optimization method based on supercritical fluid technique according to claim 1, it is characterised in that：In step (1)
Amber minimum dimension >=2mm of the pretreatment.
4. the amber optimization method based on supercritical fluid technique according to claim 3, it is characterised in that：In step (1)
The amber minimum dimension of the pretreatment is 2~50mm.
5. the amber optimization method based on supercritical fluid technique according to claim 1, it is characterised in that：In step (1)
The pretreatment refers to amber original stone carrying out polishing peeling, cut, and cleans, drying, obtains the amber of pretreatment.
6. the amber optimization method based on supercritical fluid technique according to claim 5, it is characterised in that：The drying
Temperature is 25 DEG C~50 DEG C.
7. the amber optimization method based on supercritical fluid technique according to claim 1, it is characterised in that：The pretreatment
It is processed by shot blasting after further including polishing, in particular to cutting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711225193.0A CN108041779B (en) | 2017-11-29 | 2017-11-29 | Amber optimization method based on supercritical fluid technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711225193.0A CN108041779B (en) | 2017-11-29 | 2017-11-29 | Amber optimization method based on supercritical fluid technology |
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| Publication Number | Publication Date |
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| CN108041779A true CN108041779A (en) | 2018-05-18 |
| CN108041779B CN108041779B (en) | 2019-12-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110934889A (en) * | 2019-12-30 | 2020-03-31 | 嘉兴怡萃生物科技有限公司 | Efficient and comprehensive extraction method of effective components in amber |
| CN115569628A (en) * | 2022-08-17 | 2023-01-06 | 广州大学 | Supercritical carbon dioxide swelling asphalt system and operation method |
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| CN105835285A (en) * | 2016-04-05 | 2016-08-10 | 昆明理工大学 | Preparation method for reconstructed amber |
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2017
- 2017-11-29 CN CN201711225193.0A patent/CN108041779B/en not_active Expired - Fee Related
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| CN101003174A (en) * | 2006-12-28 | 2007-07-25 | 中北大学 | Forming machine for extruding assistant high molecular material in supercritical fluid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110934889A (en) * | 2019-12-30 | 2020-03-31 | 嘉兴怡萃生物科技有限公司 | Efficient and comprehensive extraction method of effective components in amber |
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| CN115569628B (en) * | 2022-08-17 | 2024-05-24 | 广州大学 | Supercritical carbon dioxide swelling asphalt system and operation method |
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