CN102698980A - Method for softening and cleaning peripheral coagulum on ocean-effluent ceramic - Google Patents
Method for softening and cleaning peripheral coagulum on ocean-effluent ceramic Download PDFInfo
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Abstract
The invention relates to a method for softening and cleaning peripheral coagulum on an ocean-effluent ceramic. The method comprises the following mainly steps: 1) immersing the ocean-effluent ceramic in 3-5% of mass ratio of hydrochloric acid solution until the hydrochloric acid solution cannot be bubbled; and removing softened coagulum; and 2) immersing the ocean-effluent treated in the step 1) in mixed solution of 3-6% of mass ratio of EDTA-2Na and 1-4% of mass ratio of citric acid and removing the softened coagulum. According to the invention, the method can effectively remove the coagulum on the ocean-effluent ceramic.
Description
Technical field
The invention belongs to the historical relic's protection field, relate to the coagulative softening cleaning method of a kind of ocean water outlet ware week body particularly.
Background technology
Historical relics such as most of ocean water outlet ware, through the long term of seawater long period of soaking and calcareous thing such as marine organisms, ooze, the closely glued volume hard coagulation not of uniform size that forms.These coagulations are under the situation that extraneous humiture changes; Will inevitably produce the physical property squeeze and destroy to the historical relic bodies such as pottery, metal of parcel wherein; How under the prerequisite of guaranteeing historical relic safety, these historical relics complete extraction from coagulation is come out, become an extremely urgent scientific research difficult problem.
Therefore, carry out the coagulative softening cleaning research of ocean water outlet ware week body,, have general and profound significance for the protection and the preservation of the unearthed ware of archaeological excavation under water.
Inorganic Non-metallic Materials has excellent corrosion resisting performance usually.But because of reasons such as its chemical composition, crystalline state, structure and corrosive mediums, under any circumstance all corrosion resistant Inorganic Non-metallic Materials is non-existent.Inorganic Non-metallic Materials forms galvanic cell unlike metal is such when contacting with electrolyte solution except that graphite, thus its corrosion do not cause by electrochemical process, and cause owing to chemical action or physical action often.Except that hydrofluoric acid and high temperature phosphoric acid, the overall acid resistance of silicate material is stronger.In general, SiO
2Content is high more, and is corrosion-resistant more, and degree of crystallinity highly corrosion resistant ability more is strong more.Change curve according to glass solubility and pH value can know, pH＜5 o'clock are dominant mechanism with ion-exchange, and solubility is bigger; PH＞9 o'clock are dissolved as the master with matrix, and solubility is very big; 5＜pH＜9 o'clock are corroded the gentlyest, and solubility is very little.Simultaneously can know that according to the change curve of glass rate of dissolution and pH value the rate of dissolution of pH＜9 o'clock glass is all very low, pH＞9 o'clock, rate of dissolution is increased sharply.
Can know that according to ceramic erosion theory it in alkaline environment the matrix solubilizing reaction can take place, and reaction rate is very fast.Should in neutral environment, carry out when therefore, the ware material protection is handled as far as possible.Certainly because its acid corrosion-resistant relatively, and the rate of dissolution in weak acid environment very low-with neutral environment in speed close, therefore, in weak acid environment, protect processing also can not produce and damage the porcelain body.In a word, in the ware protection process, its processing procedure is answered " peaceful acid is alkali not ", in neutral weak acid environment, protects processing as far as possible.
About the research of ware surface deposits, aspect the removal of focus mostly at present in the land burial process formed calcareous, soil rust matter and organic matter deposition.Remove with diluted acid class cleaning agent (like oxalic acid, acetic acid, citric acid, watery hydrochloric acid etc.) for mineral-type deposition such as calcareous is many; Wherein how to remove with 10% hydrochloric acid or nitric acid for deposit of lime; Gypsum matter deposit is many to be removed with red fuming nitric acid (RFNA), and siliceous deposits is removed with 1% hydrofluoric acid.The scholar is also arranged with 5% sodium hexametaphosphate solution removal calcium deposition, relatively more in vogue in recent years with disodium ethylene diamine tetraacetate (EDTA disodium salt, EDTA-2Na) removal calcium deposition.And how to remove with reagent such as acetone, alcohol, gasoline and hydrogen peroxide solution for organic stains such as all kinds of greasy dirts.
There is the scholar once to use Modern Analytical Instrument such as chromatography of ions, X fluorescence power spectrum, X-ray diffractometer, ESEM, microscope, conductivity meter; Quantitative analysis to the constituent analysis of the marine sediment of water outlet porcelain body and parcel, CT scan, classification, salt content; Show that the coagulation that wraps up porcelain has two kinds; A kind of for the calcium carbonate being main deposit, a kind of in addition main sulfate with gypsum matter, iron.So far, the analysis and research of the coagulated material that adheres to for cultural artifact surface in the shipwreck rarely have report, to the removal research of coagulated material as yet not system carry out.
Summary of the invention
The object of the present invention is to provide the coagulative softening cleaning method of a kind of ocean water outlet ware week body.
Be the realization above-mentioned purpose, the coagulative softening cleaning method of ocean water outlet ware week body provided by the invention, key step has:
1) ocean water outlet ware being put into mass ratio is till the hydrochloric acid solution of 3-5% is dipped to hydrochloric acid solution and does not emit bubble, and removes softening coagulation;
2) to put into mass ratio be that the mixed solution of 3-6%EDTA-2Na and 1-4% citric acid soaks to the ocean water outlet ware after step 1 is handled, and remove the coagulation that has softened; Wherein, the mass ratio of mixed solution is preferably 5%EDTA-2Na and 3% citric acid.
Described softening cleaning method, wherein, repeating step 1 to 2.
Described softening cleaning method wherein, is removed organic dirt on the ocean water outlet ware surface after step 2 is handled with hydrogen peroxide solution; Wherein, the mass ratio of hydrogen peroxide solution is 3-5%.
Softening cleaning way of the present invention can effectively be removed the coagulation on the ocean water outlet ware.
Description of drawings
Fig. 1 is the coagulative thing phase composition of HGJ-BG1 XRD analysis result in the specific embodiment of the invention.
Fig. 2 is the coagulative industry CT scanned photograph of HGJ-BG1 in the specific embodiment of the invention, demonstrates one of them lamella.
Fig. 3 is the coagulative XRD analysis result of HGJ-BG2 in the specific embodiment of the invention,
The specific embodiment
In March, 2007-May, in November, 2008-December, China archaeological work person under water salvages magnificent light reef I shipwreck in the marine site, Xisha, excavates the water outlet historical relic and exceedes ten thousand.China's light reef water outlet historical relic is main with ware, totally one ten thousand of water outlet wares, and wherein complete relatively has seven over thousands of.Also have ironware, the wooden deck of boat and a small amount of bronze mirror relic.Ware is in the majority with bluish white glaze, blue or green glaze, also has some sauce enamal organs.Type mainly contains bowl, dish, dish, bottle, kettle, powder box, jar, alms bowl, army and holds etc.The decoration technique of implements has delineation, press back etc.; Main decorative pattern twines branch flower, folding branch flower etc. and happy character (like " Ji ", " very lucky " etc.).In addition, in the end of some implements, foot, find to have the Mo Shuti note.The pottery place of production is mainly the common cave in Fujian and Jing Dezhen, Jiangxi.These wares the time on behalf of Southern Song Dynasty's middle and advanced stage, surplus modern 800 year.For the manufacturing process of research China Southern Song Dynasty porcelain in period, type style, decorative technique, export situation etc. provide important data in kind; The discovery of these water outlet historical relics, witness the history that good contact arranged and promote development of world civilization with surrounding countries in China Southern Song Dynasty period.
Yet after several centuries had been buried in the seabed, these historical relics Zhou Tijun covered coagulation in various degree, takes scientific and effective cleaning process, to protecting the huge ceramic historical relic of this lot number amount, makes it can preserve displaying for a long time and just seems particularly important.
It is example that the present invention goes out the coagulative softening cleaning of ceramic water week body for I number with magnificent light reef, and method of the present invention is described in detail.
1, laboratory sample
Test used coagulation sample and all take from museum, Hainan Province.
2, laboratory apparatus and sample preparation
1) industry CT method
Industry CT, English INDUSTRIAL COMPUTED TOMO-GRAPHY by name, literal translating is " industrial computer X ray tomographic machine ".The CT check and analysis are detected as as the laboratory in mathematics institute of Capital Normal University to be carried out, and two sample profiles of detection are similar to the ellipsoid shape, and length is about 250MM, and the axial radii maximum is about 45MM-50MM.
After the comparison of overtesting and reconstructed image, confirm that parameter is following: scanning voltage is 440KV, and electric current 9MA, SOD are 730MM, and ODD is 230MM (SOD representes the distance of radiographic source scanning samples, and ODD representes the distance of scanning samples to detector).
The probe unit that linear array is surveyed is 0.083MM, and the highest resolution ratio can reach about 0.06MM, and the unit of planar array detector is 0.127MM, and highest resolution is about 0.1MM.
Use line detector to carry out Single Slice Mode repeatedly, layering computed tomography, the tired then three-dimensional result that builds up.The resolution ratio of rebuilding is about 0.4MM.For sample number into spectrum BG1 (porcelain piece), carried out 125 layers of scanning altogether, consuming time 2 hours 30 minutes, final reconstructed results was 512 * 512 * 125.For sample number into spectrum BG2 (ironware piece), carry out 53 layers of scanning altogether, 1 hour consuming time.Final reconstructed results is 512 * 512 * 52.
2) x-ray fluorescence analyzer: day island proper Tianjin EDX-800HS x-ray fluorescence analyzer, rhodium target (Rh), voltage Ti-U 50kV; Na-Sc 15kV, test environment are vacuum, testing time 200s.
3) X-ray diffractometer: Japanese RINT2000X x ray diffractometer x of science, copper target, slit DS=SS=1 °, RS=0.15mm; Voltage 40kV, electric current 40mA.Check and analysis are accomplished in Chinese culture legacy research institute water outlet historical relic's protection science and technology laboratory.
Go out ceramic water and generally all be wrapped in the coagulation, the existing ooze of coagulation material of parcel also is mingled with iron rust.XRF (XRF) analysis result shows that the BG1 main component is (seeing table 1) such as iron, calcium, sulphur, silicon; X-ray diffraction (XRD) analysis result shows sulfate, carbonate and the oxidation corrosion that main coagulative thing phase composition is an iron among the BG1, also contains in addition (as shown in Figure 1) such as calcium carbonate, silica.BG1 is carried out ion chromatography (IC) show that cation wherein mainly is Ca
2+, Na
+, anion mainly is Cl
-, SO
4 2-, see table 2.After BG1 carried out industry CT scanning, find to cascade by six layers of porcelain altogether in this coagulation, layer and layer between the space in be filled with iron rust and ooze class material, as shown in Figure 2.
The surface can be attached with some calcium carbonates, gypsum matter, siliceous or ooze matter deposit usually after most of ware water outlet, has both influenced the outward appearance of historical relic, has covered the cultural information on implements surfaces again, like the surperficial texturing of porcelain, stroke flower, decalcomania etc.Mostly China light reef I water outlet ware surface is calcium carbonate, gypsum matter deposit.In the museum 95% porcelain from water outlet till now also without any surface cleaning processing, the thick 3-4mm that reaches of the deposit of part ware wherein.Some then by the rimstone gluing together.The white deposits on two implements surface have wherein been carried out XRF analysis (seeing table 3), and the result shows that it contains components such as calcium, sodium, magnesium, chlorine, sulphur, is main with calcium deposition mainly.
In addition, also there are marine sediments such as more shell, coral in many implements surfaces.Owing to have small amounts of iron matter historical relic in the shipwreck, thus some ware surface also exist iron rust matter deposit or with iron cultural relic by using adhesion mutually, even around some porcelain by iron rust or iron cultural relic by using parcel.
Coagulation can produce the physical property squeeze and destroy to the historical relic bodies such as pottery that wherein wrap up under the situation that extraneous humiture changes, be necessary historical relic is extracted from coagula.At first, choose coagulation BG1 plurality of small blocks and soak the decomposition experiment with different chemical reagent.With the oven dry of each coagulation fritter and weigh, weight is as shown in table 4 before the experiment.Immersion reagent is respectively 8% hydrochloric acid (HCl), nitric acid (HNO
3), calgon and EDTA disodium salt.All soaks all are made into 200ml, soak and change new soln after 24 hours.The immersion dissolving is reclaimed coagulation fritter residue and is weighed after seven days.
Soak to finish the back and use filtration method to extract each coagulation fritter residue, and the residue that will clean, dry weighs, residue weight is as shown in table 5.
China light reef coagulation BG1 decomposes experiment and shows; Owing to contain the oxide of sulfate, carbonate and the iron of more iron among the magnificent light reef BG1; It is all undesirable in 8% hydrochloric acid, resolution in the nitric acid, and the solute effect in calgon and EDTA disodium salt is better.Be embodied in: just produced great amount of bubbles in first day with the immersion of EDTA disodium salt, react more obvious; Soak then visible a little bubble with calgon and produce, explain dissolving has also taken place, but comparatively slow; And with not producing bubble in the soak of hydrochloric acid, nitric acid dissolve basically, explain basically not react.Soak with the EDTA disodium salt that the sample major part powders after five days, and less with hydrochloric acid, the variation of nitric acid dissolve sample, react very slow.Coagulative weight has then further proved this conclusion before and after soaking: the dissolution rate of sample in EDTA disodium salt solution and sodium hexametaphosphate solution reaches 55.26% and 54.16% respectively; And the dissolution rate in hydrochloric acid (HCl) solution and nitric acid (HNO3) solution has only 25.31% and 16.07%.Therefore show that through soaking dissolution experiment the solute effect of magnificent light reef BG1 in the EDTA disodium salt is best.
Simultaneously, choose mentioned reagent light reef to China coagulation BG2 and carried out similar dissolution experiment.Selected coagulation fritter weight is seen table 6.
Extract each coagulation fritter residue soak finishing the same filtration method that uses in back, and the residue that will clean, dry weighs, residue weight is as shown in table 7.
China light reef coagulation BG2 decomposes experiment and shows that (XRD analysis shows that magnificent light reef coagulation BG2 mainly is made up of calcium carbonate and silica owing to contain more carbonate among the magnificent light reef coagulation BG2; Contain a small amount of calcium sulfate and ferrous disulfide simultaneously; As shown in Figure 3), the hydrochloric acid 8%, the resolution in the nitric acid are all more satisfactory, and dissolution velocity is very fast; And the solute effect in calgon and EDTA disodium salt is relatively poor, and dissolution velocity is slower.Be embodied in: just produced great amount of bubbles in first day with nitric acid, salt soak, reaction clearly.Soak after three days, the coagulation in this two solution all thoroughly decomposes, and has become fine particle, shows that the coagulation solute effect is remarkable.Also there are some difference in salpeter solution and hydrochloric acid solution, show as, and soak after three days, have loseed black particle in the salpeter solution, all are khaki and white particle (being siliceous grains of sand composition) basically.Carbonate has not only been dissolved in this explanation, salpeter solution, has also dissolved black content (mainly should be organic matter) simultaneously, reflects, and the solute effect of salpeter solution is superior to hydrochloric acid.Soak then visible a little bubble with EDTA disodium salt, calgon and produce, explain dissolving has also taken place, but comparatively slow.Soak with the EDTA disodium salt that sample partly powders after five days, and less with the variation of calgon dissolved samples, react very slow.Weight before and after China light reef coagulation BG2 soaks has been supported this conclusion equally: sample is at hydrochloric acid (HCl) solution and nitric acid (HNO
3) dissolution rate in the solution reaches 59.96% and 75.54% respectively; And the dissolution rate in EDTA disodium salt solution and sodium hexametaphosphate solution has only 52.71% and 13.43%.Therefore show that through soaking dissolution experiment the solute effect of BG2 in dilute nitric acid solution is best.
More than experiment shows that for the carbonate coagulation, the diluted acid effect is very good; For coagulations such as Sulfates, molysite classes, the solute effect of diluted acid is all undesirable, but the effect of EDTA disodium salt is better.Based on this, EDTA-2Na has been carried out composite research.Choose magnificent light reef coagulation plurality of small blocks, soak with the composite reagent of different EDTA-2Na and decompose experiment, soak the reagent quality ratio and be respectively:
1) 3-6%EDTA-2Na+1-4% citric acid;
2) 3-6%EDTA-2Na+1-4% oxalic acid;
3) 3-6%EDTA-2Na+1-4% hydrogen peroxide solution.
The soak of all mixing all is made into 200ml.The coagulation fritter that experiment is chosen is weighed after oven dry, and its weight is seen table 8.Soak to dissolve and finish back recovery dissolution residual substance, weigh after cleaning, drying, residue weight is listed in table 9.
Composite reagent effect of EDTA-2Na such as table 10, combine experiment shows that the effect of EDTA-2Na+ citric acid is best, the effect of EDTA-2Na+ oxalic acid secondly, the effect of EDTA-2Na+ hydrogen peroxide solution is the poorest.
1) utilize Sulfates in softening No. 1 shipwreck of magnificent light reef of EDTA-2Na reagent, molysite class coagulation effect better, the best results of its composite reagent 5%EDTA-2Na+3% citric acid can select to use this composite reagent in the actual mechanical process;
2) utilize rare nitric acid decomposing carbonate class of 8% coagulative fastest, best results.Consider that rare nitric acid possibly produce slight damage to ceramic body, can select the lower watery hydrochloric acid of concentration (3-5%) in the actual mechanical process;
3) because coagulation kind more complicated in the shipwreck, the ceramic cultural artifact surface that is unearthed in the same environment possibly existingly be main deposit with carbonate, and having with the sulfate of calcium sulfate, iron etc. again is master's deposit.In the softening actual mechanical process of coagulation, follow following program:
1. putting into 3～5% hydrochloric acid solution to implements soaks 0.5～1.5 hour (this operation can be removed most of carbonate deposition rapidly; But the time is unsuitable long; Just should stop this step operation when emitting bubble immediately when soak is not obvious), remove with instruments such as scalpel, hairbrush afterwards and softened the part coagulation.
2. change implements over to and soak 5～7 days (this operation can be removed the sulfate of calcium sulfate, iron etc.) in the 5%EDTA-2Na+3% citric acid solution, remove softening part coagulation with instruments such as scalpel, hairbrush afterwards.
3. the organic dirt for the device table is remaining, then considers to remove with 3～5% hydrogen peroxide solution wiping.
4. if satisfactory for result, then get into next step operation-desalination, otherwise repeat above process according to circumstances, or consider to select for use appropriate reagent to operate with the paper pulp application method to the subregion.
Table 1: coagulative XRF analysis result (W%) in the magnificent light reef I shipwreck
| Numbering | SiO 2 | Fe 2O 3 | CaO | SO 3 | MnO |
| HGJ-BG1 | 1.49 | 81.79 | 4.89 | 11.74 | 0.09 |
Table 2: coagulative ion chromatography result (μ g/g) in the magnificent light reef I shipwreck
| Numbering | Cl - | SO 4 2- | Na + | K + | Mg 2+ | Ca 2+ |
| HGJ-BG1 | 1829.03 | 10437.38 | 3180.91 | 178.93 | 666 | ＞2485.09 |
Table 3: the XRF analysis result (W%) of ware surface deposits in the magnificent light reef I shipwreck
| Numbering | K 2O | Fe 2O 3 | CaO | MgO | Na 2O | SO 3 | P 2O 5 | Cl |
| HGJ-QB6-JJW | 0.502 | 0.328 | 47.371 | 12.086 | 29.948 | 2.420 | 7.315 | |
| HGJ-QB7-JJW | 1.310 | 48.742 | 18.968 | 6.936 | 2.275 | 11.973 |
Table 4: the parallel appearance of magnificent light reef I coagulation BG1 dissolving piece weight
| Sample | HGJ-HCl | HGJ-HNO 3 | HGJ-EDTA-2Na | HGJ-(NaPO 3) 6 |
| Weight (g) | 0.818 | 0.841 | 0.891 | 0.855 |
Table 5: each parallel appearance piece dissolving back of magnificent light reef I coagulation BG1 is residual heavy
| Sample | HGJ-HCl | HGJ-HNO 3 | HGJ-EDTA-2Na | HGJ-(NaPO 3) 6 |
| Weight (g) | 0.611 | 0.706 | 0.398 | 0.392 |
| Dissolution rate (%) | 25.31 | 16.07 | 55.26 | 54.16 |
Table 6: the parallel appearance of magnificent light reef I coagulation BG2 dissolving piece weight
| Sample | HGJ-HCl | HGJ-HNO 3 | HGJ-EDTA-2Na | HGJ-(NaPO 3) 6 |
| Weight (g) | 13.014 | 15.40973 | 16.299 | 11.643 |
Table 7: each parallel appearance piece dissolving back of magnificent light reef I coagulation BG2 is residual heavy
| Sample | HGJ-HCl | HGJ-HNO 3 | HGJ-EDTA-2Na | HGJ-(NaPO 3) 6 |
| Weight (g) | 5.210 | 3.768 | 7.708 | 10.079 |
| Dissolution rate (%) | 59.96 | 75.54 | 52.71 | 13.43 |
Table 8: the parallel appearance of magnificent light reef I coagulation dissolving piece weight
| Sample | EDTA-2Na+ oxalic acid | The EDTA-2Na+ citric acid | The EDTA-2Na+ hydrogen peroxide solution |
| Weight (g) | 1.030 | 0.846 | 1.090 |
Each parallel appearance piece dissolving back of the magnificent light reef of table 9 I coagulation BG1 is residual heavy
| Sample | EDTA-2Na+ oxalic acid | The EDTA-2Na+ citric acid | The EDTA-2Na+ hydrogen peroxide solution |
| Weight (g) | 0.179 | 0.013 | 0.446 |
| Dissolution rate (%) | 82.55 | 98.43 | 59.04 |
Table 10:EDTA-2Na combine experiment effect
Claims (5)
1. the coagulative softening cleaning method of ocean water outlet ware week body, key step has:
1) ocean water outlet ware being put into mass ratio is till the hydrochloric acid solution of 3-5% is dipped to hydrochloric acid solution and does not emit bubble, and removes softening coagulation;
2) to put into mass ratio be that the mixed solution of 3-6%EDTA-2Na and 1-4% citric acid soaks to the ocean water outlet ware after step 1 is handled, and remove the coagulation that has softened.
2. softening cleaning method according to claim 1, wherein, the mixed solution of step 2 is mass ratio 5%EDTA-2Na and 3% citric acid.
3. softening cleaning method according to claim 1, wherein, repeating step 1 to 2.
4. softening cleaning method according to claim 1 wherein, is removed organic dirt on the ocean water outlet ware surface after step 2 is handled with hydrogen peroxide solution.
5. softening cleaning method according to claim 4, wherein, the mass ratio of hydrogen peroxide solution is 3-5%.
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| CN104030734A (en) * | 2014-06-18 | 2014-09-10 | 中山大学 | Stripping method of emersed ceramic surface condensate |
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