CN113914133B - Protection method of paper cultural relics containing transition metal - Google Patents
Protection method of paper cultural relics containing transition metal Download PDFInfo
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- CN113914133B CN113914133B CN202111145289.2A CN202111145289A CN113914133B CN 113914133 B CN113914133 B CN 113914133B CN 202111145289 A CN202111145289 A CN 202111145289A CN 113914133 B CN113914133 B CN 113914133B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/18—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00 of old paper as in books, documents, e.g. restoring
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M7/00—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock
- B41M7/0063—Preservation or restoration of currency, books or archival material, e.g. by deacidifying
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Abstract
The invention provides a method for protecting paper cultural relics containing transition metals, which comprises the step of contacting parts to be protected in the paper cultural relics with a solution containing a protecting agent, wherein the protecting agent is alkane substituted by at least one hydroxyl. The invention provides a protection method of paper cultural relics containing transition metal ions, wherein a protective agent is contacted with the paper cultural relics containing transition metal pigments, and the protective agent can be attached to the surface of paper for a long time, so that the degradation of hydrogen peroxide and hydroxyl radicals generated on the surface of the paper to damage the cellulose skeleton of the paper is avoided, the problems of the reduction of mechanical strength and polymerization degree of the paper, the serious color change of the paper and the like are effectively solved, and the long-term protection of the paper cultural relics is realized; in addition, the protective agent also has the advantages of simplicity, easy obtaining, no toxicity, no harm, economy, environmental protection and the like.
Description
Technical Field
The invention relates to the technical field of paper cultural relic protection, and relates to a protection method of paper cultural relics containing transition metals.
Background
Paper cultural relics such as calligraphy and painting serve as the witnesses of human history and civilization, are extremely precious wealth for human beings, and are non-renewable cultural resources. Paper is used as a carrier of cultural relics, is a two-dimensional material mainly composed of cellulose, and is assembled by polymer chains in a multi-scale mode.
At present, a great amount of paper cultural relics which are collected in various countries around the world are seriously degraded and discolored in the long-term storage process, for example, the use of iron container ink can cause serious corrosion to paper, perforation around the ink or the reduction of the mechanical property of the paper; in the case of the traditional Chinese painting using the rock green or rock green, the pigment causes yellowing and even embrittlement of the surrounding paper-based material to be damaged. It has been found that these paper damages are caused by Fenton-like oxidation of cellulose, and hydroxyl radicals generated by Fenton oxidation of transition metal substances such as iron and copper contained in the pigment are the most active molecules and are also one of the most aggressive chemical substances. Hydroxyl radicals can react with almost all biological macromolecules, organic or inorganic substances in a variety of different types and have very high reaction rate constants and electrophilicity with negative charges. Therefore, transition metal substances such as iron or copper contained in the pigment can accelerate the degradation of cellulose, resulting in the damage of paper.
In order to slow down the corrosion of ink, pigment and the like to paper,
and Cabrita et al apply nano calcium hydroxide/magnesium hydroxide, gallic acid, halide, phytin calcium as protective agents to prevent degradation of paper by iron-bladder ink. Potthast et al slow the corrosive degradation rate of pigments to paper by adding tetrabutylammonium bromide, benzotriazole, gelatin, and the like. However, these protective agents affect the color, pH or surface pigment state of the original paper to some extent, and at the same time, they cannot effectively remove free radicals and cannot perform long-term protection. Therefore, how to improve the long-term storage property of the paper containing the transition metal pigment is more and more interesting.
Disclosure of Invention
The invention provides a protection method of paper cultural relics containing transition metals, which is used for solving the problem that the paper cultural relics containing the transition metals cannot be effectively stored for a long time.
The invention provides a protection method of paper cultural relics containing transition metals, which comprises the following steps: and (3) contacting the part to be protected in the paper cultural relic with a solution containing a protecting agent, wherein the protecting agent is alkane substituted by at least one hydroxyl group.
Further, the transition metal is one or more of iron, copper, chromium, zinc, mercury and cadmium.
Further, the protective agent has a structure shown in formula 1:
wherein the number of carbon atoms of the protective agent is 4-5, and R 1 、R 2 Independently selected from linear alkyl of C1-C3.
Further, in the structure shown in formula 1, R 1 Is methyl, R 2 Is ethyl or propyl.
Further, in the structure shown in formula 1, R 1 And R 2 Are all ethyl groups.
Further, the protective agent has a structure shown in a formula 2,
wherein n =1 or 2.
Further, the protecting agent has a structure shown in formula 3:
wherein R is 1 、R 2 Independently selected from H and C1-C2 straight chain alkyl.
Further, in the structure shown in formula 3, R 1 And R 2 Are all H.
Further, in the structure shown in formula 3, R 1 And R 2 Are all methyl.
Further, in the structure shown in formula 3, R 1 And R 2 Are all ethyl groups.
Further, the protective agent has a structure shown in formula 4:
wherein R is 1 、R 2 Independently selected from H or methyl.
Further, in the structure shown in formula 4, R 1 And R 2 Are all H.
Further, in the structure shown in formula 4, R 1 And R 2 Are all methyl.
Further, in the solution containing the protective agent, the mass ratio of the protective agent to the solvent is 1.
Further, the solution containing the protective agent also comprises a water-based protective agent, wherein the water-based protective agent is one or two of calcium magnesium phytate and magnesium hydroxide.
Further, the mass of the protective agent is 0.5% -8.0% of the total mass of the solution.
Further, the part to be protected in the paper cultural relic is contacted with the solution containing the protective agent in a manner of one or more of soaking, smearing and spraying.
The invention provides a protection method of paper cultural relics containing transition metal ions, wherein a protective agent is contacted with the paper cultural relics containing transition metal pigments, and the protective agent can be attached to the surface of paper for a long time, so that the degradation of hydrogen peroxide and hydroxyl radicals generated on the surface of the paper to damage the cellulose skeleton of the paper is avoided, the problems of the reduction of mechanical strength and polymerization degree of the paper, the serious color change of the paper and the like are effectively solved, and the long-term protection of the paper cultural relics is realized; in addition, the protective agent also has the advantages of simplicity, easy obtaining, no toxicity, no harm, economy, environmental protection and the like.
Drawings
FIG. 1 is a scanning electron microscope image of the papers of the protected group and the unprotected group provided in example 1 of the present invention after reacting for 2 hours, 12 hours and 48 hours in Fenton-like reagent;
FIG. 2a is a graph showing the effect of the paper of the protective group provided in example 1 of the present invention after 48 hours of reaction in Fenton-like reagent;
FIG. 2b is a graph showing the effect of the unprotected group of paper sheets provided in example 1 of the present invention after 48 hours of reaction in Fenton-like reagent;
FIG. 3 is a graph of the reduced carbonyl content of the sheets of the protected group and the unprotected group provided in example 1 of the present invention at different reaction times;
FIG. 4 is a graph of the carboxyl content of the protected group and unprotected group of paper sheets at different reaction times provided in example 1 of the present invention;
FIG. 5 is a graph of the change of infrared spectra of the protected group and the unprotected group of paper sheets at different reaction times, which are provided by example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example used 2, 5-hexanediol as the alcohol protectant, specifically, 80mL of ultrapure water and 20mmol of 2, 5-hexanediol, in which the concentration of 2, 5-hexanediol was 2.95wt%, were mixed to give a protectant solution. A1.6 g paper sample containing the transition metal pigment is soaked in a protective agent solution, and simultaneously 1.6mmol of anhydrous copper sulfate and 16mmol of hydrogen peroxide are added to simulate a Fenton-like reaction system for degrading the paper cultural relic containing the transition metal pigment. The reaction system was placed in an oven at 90 ℃ for 2, 6, 12, 24, and 48 hours, respectively, to fully simulate the oxidative degradation process that occurs over long periods of time for paper cultural relics containing transition metal pigments. And (3) taking out the paper sample after each reaction stage is finished, washing the paper sample with ultrapure water and naturally airing the paper sample, and finding that the paper has no obvious color change or damage after the reaction.
In order to better embody the protection effect of the invention, an unprotected group is set as a control experiment group at the same time, and specifically, 1.6g of paper is soaked in 80mL of ultrapure water, and simultaneously 1.6mmol of anhydrous copper sulfate and 16mmol of hydrogen peroxide are added to simulate a Fenton-like reaction system for degrading paper cultural relics containing transition metal pigments. The reaction system was placed in an oven at 90 ℃ for 2, 6, 12, 24, and 48 hours, respectively, to fully simulate the oxidative degradation process that occurs over long periods of time for paper cultural relics containing transition metal pigments. After each reaction stage, the paper sample was taken out, washed with ultrapure water and air-dried naturally.
The observation result of observing the paper by using a scanning electron microscope is shown in fig. 1, the cellulose on the surface of the paper of the protected group is better maintained in the original shape (fig. 1 d-f) along with the prolonging of time, the fibers of the paper of the unprotected group are degraded by the oxidation of hydroxyl radical to form cavities and even break (fig. 1 a-c), in fig. 1, a and d are electron microscope images of the paper after 2h reaction, b and e are electron microscope images of the paper after 12h reaction, and c and f are electron microscope images of the paper after 48h reaction.
Taking out the paper sample after 48h of reaction, observing the colors of the paper of the protected group and the unprotected group as shown in figures 2a-2b, and respectively testing the polymerization degree, the content of reduced carbonyl and the content of carboxyl on the paper, wherein the process operation is as follows, and the test results are shown in table 1:
polymerization degree: the degree of polymerization of the paper was measured according to ISO 5351 using the copper ethylenediamine solution viscometry. Weighing a proper amount of paper samples to be detected in a certain amount of copper ethylenediamine solution, fully oscillating and dissolving, measuring the viscosity of the paper samples by using a viscometer under the condition of standard temperature, and calculating the polymerization degree of the paper samples according to the method specified by ISO 5351. Each set of samples was tested 3 times and the final polymerization results averaged.
Reducing the content of carbonyl: 0.5mL of 2,3, 5-triphenyltetrazolium chloride solution with the concentration of 0.5 percent and 0.5mL of KOH solution with the concentration of 0.5mol/L are mixed, and 2-10mg of paper samples are added into the solution. The reaction mixture was heated in an open 10mL tube in a water bath at 80 ℃ for 6 minutes. Then 8ml of methanol were added after the reaction suspension had cooled to room temperature. Finally, the absorbance of the liquid at 482nm was measured using an ultraviolet spectrophotometer, and a standard curve was constructed with glucose solutions of different concentrations. The results of the reduced carbonyl content are the average of 3 determinations.
Carboxyl group content: 150mg of paper was added to 50mL of H 2 And (4) in O. Then 5mL of NaCl solution with a concentration of 0.01mol/L was added to increase the conductivity. After stirring for 1 hour, 0.1mol/L HCl solution was added to adjust the pH to 2.5. Finally, 0.04mol/L NaOH solution was added at a rate of 0.1mL/min until the pH of the solution rose to 11, while the conductivity of the solution was measured on a conductivity meter. And calculating the carboxyl content of the paper sample according to the conductivity titration curve.
TABLE 1 color Difference, degree of polymerization, reduced carbonyl and carboxyl content of protected and unprotected paper
| Protection group (48 h) | Unprotected group (48 h) | |
| Chromatic aberration | FIG. 2a | FIG. 2b |
| Degree of polymerization | 792 | 316 |
| Content of reduced carbonyl group (. Mu. Mol/g) | 338.1 | 1942.6 |
| Carboxyl group content (. Mu. Mol/g) | 117.2 | 594.7 |
Experiments on the polymerization degree, the content of reduced carbonyl and the content of carboxyl show that the polymerization degree of paper added with the 2, 5-hexanediol compound only decreases from 1022 to 792 after reaction for 48 hours, and the content of the reduced carbonyl and the content of the carboxyl are respectively 338.1 mu mol/g and 117.2 mu mol/g; the polymerization degree of the paper without the 2,5-hexanediol alcohol compound is sharply reduced from 1022 to 316, and the content of the reduced carbonyl group and the content of the carboxyl group are 1942.6 mu mol/g and 594.7 mu mol/g respectively, so that the effective protection of the paper containing the transition metal pigment by the 2,5-hexanediol is shown.
FIG. 3 is a graph of the reduced carbonyl content of the protected group and unprotected group of paper sheets at different reaction times as provided in example 1 of the present invention; FIG. 4 is a graph showing the carboxyl content of the papers of the protected group and the unprotected group under different reaction times, as shown in FIGS. 3-4, the contents of reduced carbonyl group and carboxyl group change substantially in the same manner as in Table 1, i.e. the contents of reduced carbonyl group and carboxyl group of the papers of the protected group are much lower than those of the papers of the unprotected group, and the contents of reduced carbonyl group and carboxyl group do not change much with the extension of the reaction time; FIG. 5 is a graph showing the change of infrared spectra of the protected group and the unprotected group of paper sheets at different reaction times in example 1 of the present invention, as shown in FIG. 5, wherein a is the unprotected group, b is the protected group, and the unprotected group of paper sheets is 1720cm -1 The peak intensity of carbonyl group increases continuously with the reaction time, and is 897cm -1 The peak intensity of the glycosidic bond decreased with the reaction time, while the paper of the protective group was at 1720cm -1 And 897cm -1 No obvious change is shown, and the 2, 5-hexanediol effectively inhibits the generation of the carbonyl group and the breakage of the glycosidic bond of the paper cellulose.
Example 2
This example used 2, 4-pentanediol as an alcohol protectant, specifically, 80mL of ultrapure water and 20mmol of 2, 4-pentanediol, in which the concentration of 2, 4-pentanediol was 2.60wt%, were mixed to a protectant solution. A paper sample of 1.6g containing the transition metal pigment is soaked in a protective agent solution, and simultaneously 1.6mmol of anhydrous copper sulfate and 16mmol of hydrogen peroxide are added to simulate a Fenton-like reaction system for degrading the paper cultural relics containing the transition metal pigment. The reaction system was placed in an oven at 90 ℃ for 2, 6, 12, 24, and 48 hours, respectively, to fully simulate the oxidative degradation process that occurs over long periods of time for paper cultural relics containing transition metal pigments. And (3) taking out the paper sample after each reaction stage is finished, washing the paper sample with ultrapure water, and naturally airing the paper sample, wherein the paper has no obvious color change or damage after the reaction.
The degree of polymerization, the content of reduced carbonyl groups and the content of carboxyl groups of the papers of the protected group and the unprotected group were measured in the same manner as in example 1, and the results are shown in Table 2.
TABLE 2 degree of polymerization, reduced carbonyl and carboxyl content of protected and unprotected paper
| Protection group (48 h) | Unprotected group (48 h) | |
| Degree of polymerization | 799 | 316 |
| Content of reduced carbonyl group (. Mu. Mol/g) | 402.2 | 1942.6 |
| Carboxyl group content (. Mu. Mol/g) | 125.2 | 594.7 |
Experiments on the polymerization degree, the content of reduced carbonyl group and the content of carboxyl group are carried out to conclude that the polymerization degree of the paper added with the 2, 4-pentanediol alcohol compound is only reduced to 799 from 1022 after the reaction for 48 hours, and the content of the reduced carbonyl group and the content of the carboxyl group are respectively 402.2 mu mol/g and 125.2 mu mol/g, so that the effective protection of the paper containing the transition metal pigment by the 2, 4-pentanediol is shown.
Example 3
This example used 2-butanol as an alcohol protectant, specifically, 80mL of ultrapure water and 20mmol of 2-butanol, in which the concentration of 2-butanol was 3.75wt%, were mixed to obtain a protectant solution. A1.6 g paper sample containing the transition metal pigment is soaked in a protective agent solution, and simultaneously 1.6mmol of anhydrous copper sulfate and 16mmol of hydrogen peroxide are added to simulate a Fenton-like reaction system for degrading the paper cultural relic containing the transition metal pigment. The reaction system was placed in an oven at 90 ℃ for 2, 6, 12, 24 and 48 hours, respectively, to fully simulate the oxidative degradation process of paper cultural relics containing transition metal pigments over a long period of time. And (3) taking out the paper sample after each reaction stage is finished, washing the paper sample with ultrapure water and naturally airing the paper sample, and finding that the paper has no obvious color change or damage after the reaction.
The degree of polymerization, the content of reduced carbonyl groups and the content of carboxyl groups of the papers of the protected group and the unprotected group were measured in the same manner as in example 1, and the results are shown in Table 3.
TABLE 3 degree of polymerization, reduced carbonyl and carboxyl content of the protected versus unprotected paper
| Protection group (48 h) | Unprotected group (48 h) | |
| Degree of polymerization | 766 | 316 |
| Content of reduced carbonyl group (. Mu. Mol/g) | 381.3 | 1942.6 |
| Carboxyl group content (. Mu. Mol/g) | 117.4 | 594.7 |
Experiments on the polymerization degree, the reduced carbonyl content and the carboxyl content show that the polymerization degree of the paper added with the 2-butanol alcohol compound is only reduced from 1022 to 766 after 48 hours of reaction, and the reduced carbonyl content and the carboxyl content are 381.3 mu mol/g and 117.4 mu mol/g respectively, so that the effective protection of the paper containing the transition metal pigment by the 2-butanol is shown.
Example 4
This example used glycerol as an alcohol protectant, specifically, 80mL of ultrapure water and 20mmol of glycerol were mixed into a protectant solution, wherein the glycerol concentration was 2.25wt%. A paper sample of 1.6g containing the transition metal pigment is soaked in a protective agent solution, and simultaneously 1.6mmol of anhydrous copper sulfate and 16mmol of hydrogen peroxide are added to simulate a Fenton-like reaction system for degrading the paper cultural relics containing the transition metal pigment. The reaction system was placed in an oven at 90 ℃ for 2, 6, 12, 24, and 48 hours, respectively, to fully simulate the oxidative degradation process that occurs over long periods of time for paper cultural relics containing transition metal pigments. And (3) taking out the paper sample after each reaction stage is finished, washing the paper sample with ultrapure water and naturally airing the paper sample, and finding that the paper has no obvious color change or damage after the reaction.
The degree of polymerization, the content of reduced carbonyl groups and the content of carboxyl groups of the papers of the protected group and the unprotected group were measured in the same manner as in example 1, and the results are shown in Table 4.
TABLE 4 degree of polymerization, reduced carbonyl and carboxyl content of the protected versus unprotected paper
| Protection group (48 h) | Unprotected group (48 h) | |
| Degree of polymerization | 748 | 316 |
| Content of reduced carbonyl group (. Mu. Mol/g) | 391.6 | 1942.6 |
| Carboxyl group content (. Mu. Mol/g) | 124.2 | 594.7 |
Experiments on the polymerization degree, the reduced carbonyl content and the carboxyl content show that the polymerization degree of the paper added with the glycerol alcohol compound is only reduced from 1022 to 748 after reaction for 48 hours, and the reduced carbonyl content and the carboxyl content are 391.6 mu mol/g and 124.2 mu mol/g respectively, so that the effective protection of the paper containing the transition metal pigment by the glycerol is shown.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A method for protecting a paper cultural relic containing a transition metal, which is characterized by comprising the following steps: contacting a part to be protected in the paper cultural relic with a solution containing a protective agent, wherein the protective agent is alkane substituted by at least one hydroxyl;
the transition metal is one or more of iron, copper, chromium, zinc, mercury and cadmium;
the protective agent has a structure represented by formula 1:
wherein the number of carbon atoms of the protective agent is 4-5, and R 1 、R 2 Independently selected from linear alkyl of C1-C3;
or the protective agent has a structure shown in a formula 2,
wherein n =1 or 2;
alternatively, the protecting agent has a structure represented by formula 3:
wherein R is 1 、R 2 Independently selected from H, straight chain alkyl of C1-C2;
alternatively, the protecting agent has a structure represented by formula 4:
wherein R is 1 、R 2 Independently selected from H or methyl.
2. The method according to claim 1, wherein in the solution containing the protective agent, the mass ratio of the protective agent to the solvent is 1.
3. The method according to claim 1, wherein the solution containing the protective agent further comprises a water-based protective agent, and the water-based protective agent is one or two of magnesium calcium phytate and magnesium hydroxide.
4. The method according to claim 1, characterized in that the mass of the protective agent is 0.5-8.0% of the total mass of the solution.
5. The method of claim 1, wherein the portion of the paper relic to be protected is contacted with the solution containing the protective agent by one or more of soaking, painting and spraying.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4318963A (en) * | 1980-01-21 | 1982-03-09 | Smith Richard D | Treatment of cellulosic materials |
| CN104652172A (en) * | 2015-02-04 | 2015-05-27 | 广州乾程化工科技发展有限公司 | Paper historical relic deacidifying and reinforcing protective material and preparation method thereof |
| CN108442175A (en) * | 2018-04-20 | 2018-08-24 | 中国人民大学 | A kind of paper material acid stripping method based on nano calcium hydroxide |
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| WO2003060234A1 (en) * | 2002-01-15 | 2003-07-24 | Consorzio Interuniversitario Per Lo Sviluppo Dei Sistemi A Grande Interfase C.S.G.I. | Basic suspension, its preparation and process for paper deacidification |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4318963A (en) * | 1980-01-21 | 1982-03-09 | Smith Richard D | Treatment of cellulosic materials |
| CN104652172A (en) * | 2015-02-04 | 2015-05-27 | 广州乾程化工科技发展有限公司 | Paper historical relic deacidifying and reinforcing protective material and preparation method thereof |
| CN108442175A (en) * | 2018-04-20 | 2018-08-24 | 中国人民大学 | A kind of paper material acid stripping method based on nano calcium hydroxide |
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