CN110314402A - A kind of recyclable device and recovery method of the interim curable type material of historical relic - Google Patents
A kind of recyclable device and recovery method of the interim curable type material of historical relic Download PDFInfo
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- CN110314402A CN110314402A CN201910498132.4A CN201910498132A CN110314402A CN 110314402 A CN110314402 A CN 110314402A CN 201910498132 A CN201910498132 A CN 201910498132A CN 110314402 A CN110314402 A CN 110314402A
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- curable type
- type material
- interim curable
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/18—Systems containing only non-condensed rings with a ring being at least seven-membered
- C07C2601/20—Systems containing only non-condensed rings with a ring being at least seven-membered the ring being twelve-membered
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides the recyclable device and recovery method of a kind of interim curable type material of historical relic, and the interim curable type material is the interim curable type material of volatility, and the recovery method by the material reinforced historical relic of the interim curable type the following steps are included: by being put into container；The evaporating dish that can cover the opening of the container is placed in the top of the container；The container is heated so that the interim curable type material sublimation；The evaporating dish is cooled down so that the interim curable type material after being distilled the evaporating dish bottom crystal.The present invention can carry out recycling and reusing to interim curable type material after carrying out historical relic's protection with interim curable type material.
Description
Technical field
The invention belongs to engage in archaeological studies and Techniques of Relics Protection field, and in particular, in the interim curable type material of use to historical relic
After being protected, recyclable device and recovery method that interim curable type material is recycled.
Background technique
The country ancient as one, China, most cultural representative value is exactly cultural sight.In archeological site, with
Excavate the progress of work, huge variation, the rings such as temperature, humidity, illumination, oxygen occur for environment moment locating for historical relic traces
The coupling of border factor, so that historical relic generates destruction because of dehydration, contraction, cracking and discoloration rapidly.During excavation
To historical relic traces apply controllably remove interim curable type protection materials, can effectively evade or reduce because environmental factor (temperature, humidity,
Illumination, oxygen etc.) damage of the mutation to historical relic, in favor of excavating the demand with subsequent protection transport.It is interim due to going out soil scene
Curable type material involvement level is insufficient, and certain precious fragile historical relic traces cannot timely be protected at the scene, text usually occurs
It is to lead to certain preciousnesses completely archaeological informations loss or fragility traces information the phenomenon that damage that object traces are unearthed once excavation
It extracts incomplete.At archaeological excavation scene, often there are many fragile historical relics or traces, and original state to be needed to extract, is carried to laboratory, so
Reinforcement protection is completed in the laboratory to satisfy the requirements afterwards.By fragile historical relic complete extraction in laboratory, this process is had become
A ring of most critical in fragile historical relic's protection work.
In recent years, a kind of revolutionary interim curable type material of volatility had been successfully applied to mentioning for scene of exploration historical relic
It takes, such as menthol and cyclododecane etc..Interim curable type technology has in time, effectively at archaeological excavation scene, utmostly protects
Deposit cash a function for historical relic original appearance, and can be convenient after historical relic safe transfer by the interim reversible removal of curable type material, and
The implementation of subsequent safeguard measure is not interfered, not only ensure that the safety of historical relic to be extracted but also has taken into account overall stability, is very
The historical relic's protection measure of important, efficient archaeological excavation scene.
Currently, it is literary to be unearthed using cyclododecane, menthol as the volatile organic solid of representative as archaeology excavation site
The interim curable type material of object has been widely used.But these are all so-called interim curable type materials, as the term suggests it is all wanted in the later period
Pass through volatilization removal.And with the generally use of this method, by interim curable type material in museum or historical relic's protection laboratory
The historical relic of reinforcing is more and more, although these interim curable type material toxicity are extremely low, but if not being controlled, in air concentration compared with
Still the problem of environment and health aspect can be brought when high；Simultaneously largely using these substances without being recycled in resource
It is very big waste.
Summary of the invention
In view of the foregoing, it is an object to provide recyclable device and the recycling of a kind of interim curable type material of historical relic
Method can carry out recycling and reusing to interim curable type material after carrying out historical relic's protection with interim curable type material.
On the one hand, the present invention provides a kind of recovery method of the interim curable type material of historical relic, the interim curable type material is
The interim curable type material of volatility, the recovery method the following steps are included:
It will be put into container by the material reinforced historical relic of the interim curable type；
The evaporating dish that can cover the opening of the container is placed in the top of the container；
The container is heated so that the interim curable type material sublimation；
The evaporating dish is cooled down so that the interim curable type material after being distilled the evaporating dish bottom crystal.
According to the present invention it is possible to which substance to be recycled is put into container, it is placed with evaporating dish above container, heats container,
Make above-mentioned substance sublimates to be recycled and bear crystal in evaporating dish bottom, to realize the recycling of the interim curable type material of historical relic.
It is also possible in the present invention, the interim curable type material of volatility is volatility organic solid, is selected from ring 12
At least one of alkane, menthol and its derivative, amphene and its complex material.
On the other hand, it is based on above-mentioned recovery method, the present invention also provides a kind of recycling of the interim curable type material of historical relic dresses
It sets, the interim curable type material is the interim curable type material of volatility, comprising:
It accommodates by the container of the material reinforced historical relic of the interim curable type；
The heating part so that the interim curable type material sublimation is heated to the container；
With the interim curable type material after distillation so that the cooling end of its crystallization.
It is also possible in the present invention, the container is filter flask, and the cooling end is to be inserted into the filter flask and circulate
There is the test tube of water, is tightly connected between the test tube and the filter flask.
It is also possible in the present invention, the useful pipe in feeding water of insertion in the test tube.
Also, the interim curable type material is to wave the present invention also provides a kind of recyclable device of the interim curable type material of historical relic
The interim curable type material of hair property, comprising:
It is aspirated to accommodating by the interim curable type material of volatility in the space of the material reinforced historical relic of the interim curable type
Suction section；
The cooling end for receiving the interim curable type material aspirated and crystallizing it.
It is also possible in the present invention, the cooling end is the glass trial jar for having double-layer inner containers structure, and outer layer circulation has
Water, internal layer accommodate the interim curable type material of volatility aspirated by the suction section.
It is also possible in the present invention, further includes being connected to the outer layer for feeding the pipe of water.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the recyclable device of the interim curable type material of novel historical relic of an implementation form of the invention；
Fig. 2 is the structural schematic diagram of the recyclable device of the interim curable type material of novel historical relic of another implementation form of the present invention；
Appended drawing reference:
1, filter flask；
2, test tube；
3,4, plug with holes；
5,6, bend pipe；
7, cotton；
8, sample；
9, room；
10, the historical relic being reinforced；
11, lift pump；
12, glass trial jar；
13, outer layer；
14, internal layer；
15, plug with holes；
16, bend pipe；
17, cotton；
18, water inlet pipe；
19, outlet pipe；
20,21, glass tube.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
For using after interim curable type material curable type interim for historical relic, the recycling problem of interim curable type material is of the invention
Develop the recovery method and recyclable device of a kind of dedicated interim curable type material of historical relic's protection.
The recovery method and recyclable device are suitable for cyclododecane, menthol, menthanol lactic acid ester, amphene and its compounding material
The interim curable type materials of volatiles such as material.Below by taking cyclododecane, menthol, menthanol lactic acid ester as an example, recovery method is illustrated.
Cyclododecane molecular formula is C12H24, boiling point: 118 DEG C, fusing point: 59~61 DEG C, vapour pressure: 0.0 ± 0.2 mmHg,
With extremely strong chemical inertness.
Menthol molecular formula is C10H20O, boiling point: 212 DEG C, fusing point: 41~43 DEG C, vapour pressure: 0.8 mm Hg is slightly soluble in
Water.Organic compound, colorless needle crystals or granular are dissolved in most organic solvents.
Menthanol lactic acid ester molecular formula is C13H24O3, boiling point: 80~85 DEG C, fusing point: 40 DEG C, vapour pressure: 8.58E-
05mmHg, white solid.
In order to realize the recycling purpose of above-mentioned interim curable type material, the recovery method of the interim curable type material of historical relic of the invention
Include the following steps:
It will be put into container by the material reinforced historical relic of interim curable type；
The evaporating dish that can cover the opening of container is placed in the top of container；
Container is heated so that interim curable type material sublimation；
Evaporating dish is cooled down so that interim curable type material after being distilled evaporating dish bottom crystal.
Said vesse can be beaker.That is, by being put into beaker by the material reinforced historical relic sample of interim curable type, on beaker
Side puts evaporating dish, heats beaker.Beaker bottom is especially heated, makes interim curable type material sublimation to be recycled and in evaporating dish
Bottom condenses out white crystal.There is white crystal situation in observation evaporating dish bottom, is recycled.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1:
The interim curable type material recovery of cyclododecane in loess.
The loess after 50g is reinforced is weighed, is placed in the beaker of 500ML, beaker is placed on hot plate, setting temperature is
60 DEG C, the evaporating dish that can cover beaker mouth is put above beaker, then suitable ice cube is put on evaporating dish.Observe evaporating dish
Bottom white crystal crystalline state, until bottom not until there is crystallization.White cyclododecane crystal after removing distillation claims
Weight calculates the rate of recovery.
By above recovery processing, the rate of recovery for finally calculating cyclododecane in loess is 84.7%, illustrates this with this
The recycling to interim curable type material cyclododecane may be implemented in invention.
Embodiment 2
The interim curable type material recovery of menthol in loess.
The loess after 50g is reinforced is weighed, is placed in the beaker of 500ML, beaker is placed on hot plate, setting temperature is
40 DEG C, the evaporating dish that can cover beaker mouth is put above beaker, then suitable ice cube is put on evaporating dish.Observe evaporating dish
Bottom white crystal crystalline state, until bottom not until there is crystallization.White peppermint alcohol crystals after removing distillation claim
Weight calculates the rate of recovery.
By above recovery processing, the rate of recovery for finally calculating menthol in loess is 74.3%, illustrates this hair with this
The bright recycling that may be implemented to interim curable type material menthol.
Embodiment 3
Menthanol lactic acid ester temperature pier material recovery in loess.
The loess after 50g is reinforced is weighed, is placed in the beaker of 500ML, beaker is placed on hot plate, setting temperature is
40 DEG C, the evaporating dish that can cover beaker mouth is put above beaker, then suitable ice cube is put on evaporating dish.Observe evaporating dish
Bottom white crystal crystalline state, until bottom not until there is crystallization.White menthanol lactic acid ester after removing distillation is brilliant
Body, weighing calculate the rate of recovery.
By above recovery processing, the rate of recovery for finally calculating menthanol lactic acid ester in loess is 87.2%, is said with this
The recycling to interim curable type material menthanol lactic acid ester may be implemented in the bright present invention.
Embodiment 4
Menthol temperature pier material recovery on blank sheet of paper.
Weigh 10g menthol, take and solidified on a blank sheet of paper, then its blank sheet of paper, it is to be solidified completely after, carry out blank sheet of paper on it is thin
The recycling of lotus alcohol places blank sheet of paper in 500ML beaker, beaker is placed on hot plate, burning can be covered by putting above beaker
The evaporating dish of rim of a cup, then suitable ice cube is put on evaporating dish, it is arranged 40 DEG C of temperature, observation evaporating dish bottom white crystal crystallization
State calculates the rate of recovery until bottom not until there is crystallization.
By being recycled above, the rate of recovery for finally calculating menthol on blank sheet of paper is 54.9%, illustrates the present invention with this
The recycling to interim curable type material menthol may be implemented.
Embodiment 5
Menthol temperature pier material recovery on silk.
Weigh 10g menthol, take a pull spring silk fabric, then solidified on its silk, it is to be solidified completely after, carry out silk on it is thin
The recycling of lotus alcohol places silk in 500ML beaker, beaker is placed on hot plate, burning can be covered by putting above beaker
The evaporating dish of rim of a cup, then suitable ice cube is put on evaporating dish, it is arranged 40 DEG C of temperature, observation evaporating dish bottom white crystal crystallization
State calculates the rate of recovery until bottom not until there is crystallization.
By being recycled above, the rate of recovery for finally calculating menthol on silk is 64.2%, illustrates the present invention with this
The recycling to interim curable type material menthol may be implemented.
On the other hand, according to the recovery method of above-mentioned interim curable type material, in order to promote the recovery method in real life
The recyclable device of novel interim curable type material has also been devised in application in terms of middle historical relic's protection, the present invention.
Fig. 1 is the structural schematic diagram of the interim curable type material recuperating machines of novel historical relic of an implementation form of the invention.Herein
The recyclable device of the interim curable type material of object is a kind of recyclable device of simplicity, can be used for time of interim curable type material in laboratory
It receives.The recyclable device includes: to accommodate by the container of the material reinforced historical relic of interim curable type；Container is heated so that interim solid
The heating part of type material sublimation；With the interim curable type material after distillation so that the cooling end of its crystallization.
Specifically, as shown in Figure 1, said vesse, which can be, accommodates the sample 8(after being protected i.e. by interim curable type material
The sample of reinforcing) filter flask 1.Cooling end can be in insertion filter flask 1 and circulation has the test tube 2 of water.The test tube 2 and suction strainer
It is tightly connected between bottle 1, such as plug 3 with holes is installed at the mouthpiece of filter flask 1, test tube 2 is inserted in the hole of the plug
In.
Further, constantly circulation has water in test tube 2.In this embodiment, by be inserted in test tube 2 for
The circulation for sending the pipe of water to realize water in test tube 2.The pipe can be two bend pipes 5,6, such as 90 ° of bend pipes.Wherein one it is curved
The connection water source of pipe 5 is another to send out the water in test tube 2 with bend pipe 6 to supply water into test tube 2, to keep the water in test tube 2
Constantly flowing.Plug 4 with holes is installed, bend pipe 5,6 is inserted in the hole of the plug at the nozzle of test tube 2.
In addition, the mouthpiece vicinity in filter flask 1 is additionally provided with opening, the glass for being plugged with cotton 7 is installed in the opening
Pipe 21, the pressure that the effect of cotton 7 is to maintain filter flask 1 are constant.
That is, sample is placed in filter flask in the present invention, test tube and 90 ° of bend pipes plug with holes are installed
Get up, then is installed together with plug with holes with filter flask.90 ° of bend pipes are connected into water flow, are allowed to constantly have water flow trying
It is flowed in pipe, heating filter flask bottom makes the material sublimation to be recycled in it, and temperature setting is at 40 DEG C or so, then, gradually exists
It will appear white crystal on test tube outer wall inside filter flask, finished wait condense, take out test tube, scraped on test tube outer wall with spoon
Interim curable type material, that is, realize the recycling of interim curable type material.
In view of the practical problem that historical relic storage is placed, a kind of recyclable device of implementation form has also been devised.Fig. 2 is this hair
The structural schematic diagram of the recyclable device of the interim curable type material of historical relic of bright another kind implementation form.The recyclable device of this implementation form
It can be used for the recycling of the interim curable type material of historical relic's protection later period in real life, comprising: added by interim curable type material to accommodating
Solid historical relic space in the suction section aspirated of the interim curable type material of volatility；Receive the interim curable type material aspirated
And the cooling end for crystallizing it.
Specifically, as shown in Fig. 2, above-mentioned accommodate can be storage by the space of the material reinforced historical relic of interim curable type and have
The room 9 for the historical relic 10 being reinforced.Suction section can be for being aspirated to the interim curable type material of volatility in room 9
Lift pump 11.Cooling end can be the glass trial jar 12 for having double-layer inner containers structure, and ectonexine is separated by glass wall.Glass trial jar
Circulation has water in 12 outer layer 13, accommodates the interim curable type of volatility aspirated by lift pump 11 in the internal layer 14 of glass trial jar 12
Material.The interim curable type material of the volatility condenses into crystal when touching the glass wall of above-mentioned separation ectonexine and is attached to this
On wall.
Furthermore, also as shown in Fig. 2, the top of glass trial jar 12 has opening, which is equipped with holes
Plug 15.Lift pump 11 can be connected to the internal layer 14 of glass trial jar 12 by bend pipe 16.The bend pipe 16 can be inserted into the hole of plug 15
In be connected to internal layer 14.A glass tube 20 is also inserted in another hole of the plug 15, the lower end of the glass tube 20 is connected to interior
Layer 14, upper end is blocked with cotton 17, to keep the pressure of glass trial jar 12 constant.The outer layer 13 of above-mentioned glass trial jar 12 is equipped with
Two through hole, the two through-holes are respectively communicated with the pipe for feeding water, i.e., connection water source into 12 outside 13 of glass trial jar to supply
The water inlet pipe 18 of water supply and the outlet pipe 19 for sending out the water in glass trial jar 12.The position of outlet pipe 19 is higher than water inlet pipe 18,
As shown in Fig. 2, the top for being closely located to glass trial jar 12 of outlet pipe 19.To guarantee the outer layer 13 1 of entire glass trial jar 12
The straight state passed through in water flow, so that the internal layer 14 of glass trial jar 12 is surrounded by water flow always.
That is, in this embodiment, the menthol in historical relic after being reinforced for a long time in a room can occur
It volatilizees, so that being filled with the taste of menthol in the air in room, although small toxicity, smell is larger, to health
It has a certain impact.And the recyclable device of interim curable type material suitable for large-scale room of this implementation form is used, in room
One lift pump is installed, principle is similar to the smoke exhaust ventilator of family, is connected by bend pipe, makes to volatilize in room at one jiao of top
Gas sucks in a large-scale glass trial jar, and double-layer inner containers form is presented in this glass trial jar, and there are two through-holes for outer layer, for connecting
Water receiving stream is passed through with guaranteeing that the outer layer hollow space of entire bottle is constantly in water flow, so that internal layer is surrounded by water flow always.
A glass tube is inserted at the plug above glass trial jar, then upper end is blocked with cotton, keeps the pressure of glass trial jar constant.
Gradually, as menthol gas is sucked out, it will appear white crystal in glass trial jar, when white crystal is more, Ke Yiqu
Lower glass trial jar realizes the recycling for menthol gas in house with the peppermint alcohol crystals on spoon scraping inner wall.
Industrial applicability:
The recyclable device and recovery method of the interim curable type material of historical relic of the invention can be used in historical relic's protection, to interim curable type material
The recycling and reusing of material.
Under the objective for not departing from essential characteristic of the invention, the present invention can be presented as diversified forms, therefore in the present invention
Implementation form be to be illustrative rather than definitive thereof, limited since the scope of the present invention is defined by the claims rather than by specification,
And all changes fallen in the full scope of equivalents of the range that claim defines or the range that it is defined be understood to include
In detail in the claims.
Claims (8)
1. a kind of recovery method of the interim curable type material of historical relic, the interim curable type material is the interim curable type material of volatility,
Be characterized in that, the recovery method the following steps are included:
It will be put into container by the material reinforced historical relic of the interim curable type；
The evaporating dish that can cover the opening of the container is placed in the top of the container；
The container is heated so that the interim curable type material sublimation；
The evaporating dish is cooled down so that the interim curable type material after being distilled the evaporating dish bottom crystal.
2. the recovery method of the interim curable type material of historical relic according to claim 1, which is characterized in that the volatility is interim
Curable type material is volatility organic solid, in cyclododecane, menthol and its derivative, amphene and its complex material extremely
Few one kind.
3. a kind of recyclable device of the interim curable type material of historical relic, the interim curable type material is the interim curable type material of volatility,
It is characterized in that, comprising:
It accommodates by the container of the material reinforced historical relic of the interim curable type；
The heating part so that the interim curable type material sublimation is heated to the container；
With the interim curable type material after distillation so that the cooling end of its crystallization.
4. the recyclable device of the interim curable type material of historical relic according to claim 3, which is characterized in that the container is suction strainer
Bottle, the cooling end is in the insertion filter flask and circulation has the test tube of water, seals between the test tube and the filter flask
Connection.
5. the recyclable device of the interim curable type material of historical relic according to claim 4, which is characterized in that insertion in the test tube
There is the pipe for feeding water.
6. a kind of recyclable device of the interim curable type material of historical relic, the interim curable type material is the interim curable type material of volatility,
It is characterized in that, comprising:
It is aspirated to accommodating by the interim curable type material of volatility in the space of the material reinforced historical relic of the interim curable type
Suction section；
The cooling end for receiving the interim curable type material aspirated and crystallizing it.
7. the recyclable device of the interim curable type material of historical relic according to claim 6, which is characterized in that the cooling end is tool
The glass trial jar of standby double-layer inner containers structure, outer layer circulation have water, and it is interim that internal layer accommodates the volatility aspirated by the suction section
Curable type material.
8. the recyclable device of the interim curable type material of historical relic according to claim 7, which is characterized in that further include with it is described outer
The pipe for being used to feed water of layer connection.
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| CN112812544A (en) * | 2021-02-04 | 2021-05-18 | 浙江大学 | In-situ solid multi-coated extraction material and extraction recovery method for underwater fragile cultural relics |
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