CN108642965B - Method for deacidifying paper by adopting electro-adsorption method - Google Patents
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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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Abstract
The application provides a method for deacidifying paper by an electric adsorption method, which comprises the following steps: s1, contacting the paper to be processed with a water absorption cushion layer, wherein the water absorption cushion layer contains water to wet the paper to be processed; and S2, placing the paper wetted in the step S1 and the water absorption cushion layer contacted with the paper between an inert anode plate and an inert cathode plate, wherein the surface of the inert anode plate is coated with a porous carbon material, and direct current is supplied for electric adsorption to obtain the paper after deacidification treatment. The electro-adsorption deacidification speed of the invention is much faster than that of the traditional aqueous solution method, only a few minutes are needed for one-time operation, the negative influence of the traditional soaking deacidification technology on paper is greatly reduced, and simultaneously, single paper, multiple paper and the whole book can be treated, and the pH value can be controlled more accurately. The method has the advantages of simplicity, convenience, reliability, greenness, safety and low cost, and can also avoid the problems of paper deformation, handwriting fading, ink penetration and the like possibly caused by a long-time wet state.
Description
Technical Field
The invention relates to the technical field of paper deacidification protection, in particular to a deacidification protection technology for paper cultural relics, files and books, and specifically relates to a method for deacidifying paper by an electro-adsorption method.
Background
The acidity of the literature paper is an important factor affecting the shelf life of the literature; scientists have been studying methods and apparatus for deacidifying and protecting paper since the discovery of self-destruction of paper in the nineteenth century. At present, the paper deacidification method commonly used in the world mainly comprises a gas phase deacidification method, an organic solvent deacidification method, an aqueous solution deacidification method and the like. Wherein, the aqueous solution deacidification method is simple, convenient and easy to implement, relatively environment-friendly and has more research in the industry.
An aqueous solution deacidification method is similar to the traditional alkaline water washing calligraphy of China, and is characterized in that pages are soaked in a prepared alkaline solution, and alkaline substances (such as calcium hydroxide and the like) and acid in paper are subjected to neutralization reaction, so that the aim of deacidification is fulfilled. The aqueous solution deacidification method has the advantages of environmental safety, convenient operation, economy and good deacidification effect.
However, this treatment also has disadvantages that must be overcome from another aspect. The deacidification treatment of the aqueous solution has a long time period, so that the aqueous solution soaks the paper and generates a neutralization reaction and then the subsequent wet paper needs a long time to dry, the paper is easily damaged in a long-time wet state, and the phenomena of expansion, wrinkle and the like occur during drying. If the soaking time is shortened, the alkaline deacidification agent is often only precipitated on the surface of the paper and cannot permeate into the paper. Moreover, the processing method can only process single sheets generally, and has small processing amount and low efficiency.
Disclosure of Invention
In view of this, the application provides a method for deacidifying paper by an electro-adsorption method, which has short treatment time, can simultaneously deacidify single page, multiple pages and the whole book, and has high efficiency, low cost, environmental protection and safety.
The application provides a method for deacidifying paper by an electric adsorption method, which comprises the following steps:
s1, contacting the paper to be processed with a water absorption cushion layer, wherein the water absorption cushion layer contains water to wet the paper to be processed;
and S2, placing the paper wetted in the step S1 and the water absorption cushion layer contacted with the paper between an inert anode plate and an inert cathode plate, wherein the surface of the inert anode plate is coated with a porous carbon material, and direct current is supplied for electric adsorption to obtain the paper after deacidification treatment.
Preferably, the pH value of the paper to be treated is 4.5-6.5.
Preferably, the water absorption cushion layer is made of a soft material which absorbs water and has certain strength.
Preferably, the water absorbing cushion layer is water-containing woven cloth, water-containing non-woven cloth or water-containing moisture-absorbing paper.
Preferably, the porous carbon material is one or more of activated carbon fiber, carbon aerogel and nano carbon tube.
Preferably, the porous carbon material has a BET of 500m2More than g.
Preferably, the surface of the inert anode plate is paved with activated carbon fiber cloth or activated carbon fiber felt; the thickness of the activated carbon fiber cloth or the activated carbon fiber felt is 1-5 mm.
Preferably, the direct current voltage is 0.6-1.6V, and more preferably the voltage is 0.8-1.5V; the time of the electrosorption does not exceed 15 minutes.
Preferably, the time of the electro-adsorption is 1 minute to 8 minutes.
Preferably, the water-absorbing cushion layer further contains a deacidification agent, and the deacidification agent is one or more selected from calcium oxide, calcium hydroxide, calcium carbonate, calcium bicarbonate, magnesium carbonate, magnesium bicarbonate and magnesium hydroxide.
The method for deacidifying the paper by the electro-adsorption method provided by the invention uses an aqueous solution as a carrier, wets the paper to be treated by contacting with a water absorption cushion layer, uses a porous carbon material as an electrode for capacitive deionization after wetting, and uses F in the paper under the drive of an external direct current electric field-、Cl-、SO4 2-、NO3 -And organic anions and the like move to the anode under the action of electrophoresis and are adsorbed by the porous carbon material electrode, and finally the aims of quickly deacidifying and decontaminating paper are fulfilled. The electro-adsorption deacidification speed of the invention is much faster than that of the traditional aqueous solution method, only a few minutes are needed for one-time operation, the negative effect of the traditional soaking deacidification technology on paper is greatly reduced, and simultaneously, single paper, multiple paper and the whole book can be treated, and the pH value can be controlled more accurately than that of any other deacidification method. The method not only keeps the advantages of simple, convenient and reliable deacidification of the traditional aqueous solution, greenness, safety and low cost, but also can avoid the problems of paper deformation, handwriting fading, ink permeation and the like possibly caused by a long-time wet state; meanwhile, the problems of high requirements, high cost, high risk, environmental pollution and the like of gas-phase and organic solvent liquid-phase deacidification equipment are solved, and the method can be widely popularized and applied.
Drawings
FIG. 1 is a graph comparing the condition of paper before and after deacidification in example 1;
FIG. 2 is a graph comparing the condition of the paper before and after deacidification in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
The invention provides a method for deacidifying paper by an electric adsorption method, which comprises the following steps:
s1, contacting the paper to be processed with a water absorption cushion layer, wherein the water absorption cushion layer contains water to wet the paper to be processed;
and S2, placing the paper wetted in the step S1 and the water absorption cushion layer contacted with the paper between an inert anode plate and an inert cathode plate, wherein the surface of the inert anode plate is coated with a porous carbon material, and direct current is supplied for electric adsorption to obtain the paper after deacidification treatment.
The method of the invention utilizes the porous carbon electrode electric adsorption method, can rapidly and accurately realize the deacidification and decontamination of paper cultural relics, files and books, and greatly reduces the negative effect of the traditional aqueous solution deacidification method on paper.
The invention mainly aims at deacidifying the paper in documents such as paper cultural relics, archives, books and the like, so that the paper is well protected and is convenient to store and research. Wherein the paper to be treated has a certain acidity and the pH value is generally less than 7. In the embodiment of the invention, the pH value of the paper to be treated is 4.5-6.5, preferably 5.0-6.5. Furthermore, the paper to be treated is generally light brown or yellowish brown and brittle.
The paper to be processed can be single page, multiple pages or the whole book; the thickness, area, printing method and the like of the paper are not particularly limited, and may be 16K, offset paper printing paper, and copperplate paper printing paper. Wherein, if the book is thick, the deacidification is not facilitated at the binding position.
The invention relates to a deacidification technology by taking an aqueous solution as a carrier, which can be used for flatly laying paper to be treated on a water absorption cushion layer, wherein the water absorption cushion layer contains water and can wet the paper to be treated. These mineral acids are ionic in the aqueous state of the paper (e.g. SO)4 2-、NO3 -、Cl-、CO3 2-Etc.) and is adsorbed by the paper fibers. Wherein, the substrate of the water absorption cushion layer is a layered substance with water absorption, and is generally a soft material which can absorb water and has certain strength, such as transverse tensile strength not less than 8.0N/m; the cushion layer material can be conventional woven cloth, non-woven cloth or moisture absorption paper. The cushion layer can be used repeatedly, and the area of the cushion layer is usually larger than that of paper; if the number of pages processed at one time is large, a thinner cushion layer needs to be selected.
In addition, the water absorption cushion layer preferably also contains a deacidification agent, so that the deacidification effect can be accelerated, and the treated paper has certain alkali residue. In the embodiment of the invention, the water-absorbing pad layer can be soaked in the electrolyte solution containing the deacidification agent for several minutes, such as 3 to 5 minutes, so that the water-absorbing pad layer contains a certain amount of the deacidification agent electrolyte solution. The deacidification agent can be one or more selected from calcium oxide, calcium hydroxide, calcium carbonate, calcium bicarbonate, magnesium carbonate, magnesium bicarbonate and magnesium hydroxide, and is preferably calcium hydroxide. In the embodiment of the present invention, the mass concentration of the deacidification agent in the solution is preferably 0.1 to 0.15%. The electrolyte solution of the deacidification agent is an aqueous solution containing the alkaline deacidification agent.
After the paper to be treated is wetted quickly, the paper to be treated and the cushion layer are clamped between two flat electrodes together, and a direct current power supply is switched on to form a closed loop. Wherein, the anode plate is an inert electrode plate, and the surface is paved with porous carbon material. The porous carbon material has good conductivity, large specific surface area (BET) and high chemical stability, and when placed in an electrostatic field, a strong double electric layer (the thickness is generally 1 nm-10 nm) is generated at the interface of a carbon electrode and a solution, so that a large amount of ions can be adsorbed. Under the drive of an external direct current electric field, the acidic ions can be separated from the paper and move towards the anode direction (electrophoresis), so that the acidic ions are adsorbed and stored in the double electric layers on the surface of the porous carbon material electrode. Along with the gradual increase of the ions adsorbed by the electrodes, various acid radical ions in the paper are gradually reduced, and the aim of deacidification can be quickly achieved.
The embodiment of the invention can be used for flatly paving the water-absorbed cushion layer on the plate-shaped inert anode plate paved with the porous carbon material, and then flatly paving the single-page paper to be treated on the cushion layer; if multiple layers of paper or the entire book are to be treated, a single paper layer is to be stacked. Then, the inert cathode plate is pressed on and the two plates are clamped. In the present invention, the inert cathode plate and the inert cathode plate are preferably graphite electrode plates (inert graphite). In an embodiment of the present invention, the porous carbon material may be one or more of activated carbon fiber, carbon aerogel and nano carbon tube, and is preferably activated carbon fiber. Preferably, the BET of the porous carbon material is 500m2More than g, e.g. 600 to 1000m2The concentration/g, even higher, is determined by the corresponding commercial products. Specifically, the surface of the inert anode plate is paved with a layer with the thickness of 1 mm-5 mm, preferably 1.5-4 mmThe activated carbon fiber cloth or the activated carbon fiber felt.
In the embodiment of the invention, the two polar plates are electrified with direct current, the voltage is 0.6V-1.6V, and a closed loop is formed, namely the acid removal process is started, and the acid removal process can be properly adjusted according to the thickness and the number of the paper. The time for removing acid by the electro-adsorption (also called as a capacitive deionization method or a capacitive method) is generally not more than 15 minutes, preferably 1 to 8 minutes, and more preferably 2 to 5 minutes; can be adjusted according to the acidification degree of the paper, the number of layers treated at one time and the final requirement on the pH value.
The method has the advantages that the voltage required by deacidification of the paper by the capacitance or capacitance adsorption method is lower, the operation is easier, and the method is safer. In particular in terms of safety: because the voltage is low, only the electro-adsorption process is needed, the electrode plate has no electrolytic reaction and the like, the temperature of the electrode plate is lower, and the safety of the processed paper document is ensured. In addition, the deacidification time can also be shortened. Meanwhile, the porous carbon electrode can be easily desorbed and can be repeatedly used. More important points are: the capacitor or the electric adsorption can reserve space for the subsequent paper deacidification-cleaning-reinforcement (even sterilization) integration, and has wider application prospect.
After the deacidification treatment is completed, the power supply is cut off, the cushion layer is taken off, and the paper is naturally aired or dried by other methods.
The existing paper deacidification methods used in the world have major defects, and the traditional aqueous solution method is no exception. The paper soaked for a long time is often deformed and wrinkled after being dried, and the single sheet needs to be disassembled for treatment, because the whole book needs a longer time to be soaked completely, and the sticking among the paper is inevitable and difficult to treat. The technology of the invention is suitable for processing single, multiple and whole volumes of paper cultural relics, files and books, and can control the pH value more accurately than other deacidification methods. Because the paper is only in a wet state and is tightly pressed between the electrode plates, the electrode plates press the paper like an electric iron, and separate secondary pressing treatment is not needed, the efficiency is greatly improved, and the problems of paper shrinkage, deformation, sticking in the whole book, low efficiency and the like caused by the traditional aqueous solution deacidification method can be reduced to the maximum extent. In conclusion, the deacidification technology has the remarkable advantages of good effect, high efficiency, low cost, good controllability, safety, environmental protection and the like.
For further understanding of the present application, the process for deacidifying paper by an electro-adsorption method provided herein is specifically described below with reference to examples.
In the following embodiments, the non-woven fabric mats are all commercially available common chemical fiber non-woven fabrics, and the area of the non-woven fabric mats is slightly larger than the page to be treated.
Example 1
Soaking a non-woven fabric cushion layer in deionized water, and then spreading the soaked cushion layer on an anode plate, wherein the anode plate is made of flat graphite, and activated carbon fiber cloth (the thickness is 1.5mm, BET: 1000 m) is spread on the flat graphite2/g)；
Laying the single-page paper to be processed (one page of pages of' Jiu Bai Han Shi Annotation in English printed by Beijing Business print library in 1978; 16K, offset paper printing) on the cushion layer, pressing the flat graphite cathode plate, and clamping the two electrode plates;
connecting the two polar plates with a voltage-stabilizing direct current, wherein the voltage is 1.5V, and the electric adsorption time is 5 minutes; then the power supply is cut off, the cushion layer is taken off, and the paper is naturally dried. Comparison of the conditions before and after deacidification of the paper sheets see table 1 and figure 1, and figure 1 is a comparison of the conditions of the paper sheets before and after deacidification of example 1. In fig. 1, the right side is the paper before deacidification and the left side is the paper after deacidification.
Table 1 comparative table of analytical indexes before and after deacidification of paper in example 1
Remarking: the pH value is obtained by obtaining a cold extraction solution according to the method of China national standard GB/T1545-2008 'determination of acidity or alkalinity of paper, paperboard and pulp water extraction solution', and is obtained by adopting a precision test paper with the pH value of 5.5-9.0 of Shanghai Saneisi reagent company Limited; the following examples are the same.
Example 2
Soaking the non-woven fabric cushion layer in deionized water,then the soaked cushion layer is spread on an anode plate, the anode plate is made of flat graphite, and activated carbon fiber cloth (thickness 1.5mm, BET: 1000 m) is spread on the flat graphite2/g)；
Laying the single-page paper to be treated (one page of pages of 'abstract summary of the religion' printed by Shanghai New knowledge publisher in 1957; 16K, offset paper printing) on the cushion layer, pressing the flat graphite cathode plate, and clamping the two electrode plates;
connecting the two polar plates with a voltage-stabilizing direct current, wherein the voltage is 1.5V, and the electric adsorption time is 5 minutes; then the power supply is cut off, the cushion layer is taken off, and the paper is naturally dried. Comparison of the conditions before and after deacidification of the paper sheets see table 2 and figure 2, and figure 2 is a comparison of the conditions of the paper sheets before and after deacidification of example 2. In fig. 2, the right side is the paper before deacidification and the left side is the paper after deacidification.
Table 2 example 2 comparative table of analysis indexes before and after deacidification of paper
Example 3
Soaking a non-woven fabric cushion layer in deionized water, and then spreading the soaked cushion layer on an anode plate, wherein the anode plate is made of flat graphite, and activated carbon fiber cloth (the thickness is 1.5mm, BET: 1000 m) is spread on the flat graphite2/g)；
Laying the multi-page paper to be processed (three pages of 'Jiu Bai Han Shi Annotation in English' printed by Beijing Business print library in 1978; 16K, offset paper printing) on the cushion layer, pressing the flat graphite cathode plate, and clamping the two electrode plates;
connecting the two polar plates with a voltage-stabilizing direct current, wherein the voltage is 1.5V, and the electric adsorption time is 8 minutes; then the power supply is cut off, the cushion layer is taken off, and the paper is naturally dried. See table 3 for a comparison of the conditions before and after deacidification of the paper.
Table 3 comparative table of analysis indexes before and after deacidification of paper in example 3
Example 4
Soaking a non-woven fabric cushion layer in deionized water, and then spreading the soaked cushion layer on an anode plate, wherein the anode plate is made of flat graphite, and activated carbon fiber cloth (the thickness is 1.5mm, BET: 1000 m) is spread on the flat graphite2/g)；
Spreading a plurality of sheets of paper to be treated (three pages of a 'abstract summary of amendments' printed by Shanghai New knowledge publisher in 1957; 16K, offset paper printing) on the cushion layer, pressing a flat graphite cathode plate, and clamping two electrode plates;
connecting the two polar plates with a voltage-stabilizing direct current, wherein the voltage is 1.5V, and the electric adsorption time is 8 minutes; then the power supply is cut off, the cushion layer is taken off, and the paper is naturally dried. See table 4 for a comparison of the conditions before and after deacidification of the paper.
Table 4 example 4 comparative table of analysis indexes before and after deacidification of paper
Example 5
Soaking a non-woven fabric cushion layer in deionized water, and then spreading the soaked cushion layer on an anode plate, wherein the anode plate is made of flat graphite, and activated carbon fiber cloth (the thickness is 1.2mm, BET: 1200 m) is spread on the flat graphite2/g)；
Laying the single-page paper to be processed (one page of pages of' Jiu Bai Han Shi Annotation in English printed by Beijing Business print library in 1978; 16K, offset paper printing) on the cushion layer, pressing the flat graphite cathode plate, and clamping the two electrode plates;
connecting the two polar plates with a voltage-stabilizing direct current, wherein the voltage is 1.5V, and the electric adsorption time is 5 minutes; then the power supply is cut off, the cushion layer is taken off, and the paper is naturally dried. See table 5 for a comparison of the conditions before and after deacidification of the paper.
Table 5 example 5 comparative table of analytical index before and after deacidification of paper
Example 6
Soaking a non-woven fabric cushion layer in a saturated calcium hydroxide solution, and then spreading the soaked cushion layer on an anode plate, wherein the anode plate is made of flat graphite, and activated carbon fiber cloth (the thickness is 1.5mm, BET: 1000 m) is spread on the flat graphite2/g)；
Laying the single-page paper to be processed (one page of pages of' Jiu Bai Han Shi Annotation in English printed by Beijing Business print library in 1978; 16K, offset paper printing) on the cushion layer, pressing the flat graphite cathode plate, and clamping the two electrode plates; connecting the two polar plates with a voltage-stabilizing direct current, wherein the voltage is 1.5V, and the electric adsorption time is 5 minutes; then the power supply is cut off, the cushion layer is taken off, and the paper is naturally dried. See table 6 for a comparison of the conditions before and after deacidification of the paper.
Table 6 example 6 comparative table of analysis indexes before and after deacidification of paper
Comparative example
For comparison with other paper deacidification methods, the following comparative tests were performed on adjacent pages of the pages of "Jiu Bai Han Shi Annotation" printed in Beijing Business handbook of 1978. The test methods, conditions and results are shown in tables 7 and 8.
The specific test conditions of the comparative group 1 are as follows: the pages are put into a container containing 0.15 percent calcium hydroxide solution for 30 minutes, and then are naturally dried after being taken out.
The specific test conditions for comparative group 2 were as follows: the activated carbon fiber cloth covered on the electrode plates in example 1 was removed, and the two electrode plates were connected to a DC power supply with a DC current of 0.8A for 10 minutes. And (5) cutting off the power, taking out and naturally drying.
Table 7 example 7 comparative experiment on different paper deacidification methods
TABLE 8 anion concentration in cold draw solutions of paper samples treated with different deacidification methods (unit: μ g/mL)
| Deacidifying treatment method | Cl- | SO4 2- | NO3 - |
| Untreated virgin paper samples | 5.931 | 10.824 | Not detected |
| The present invention relates to an electric adsorption method | 1.430 | 3.720 | Not detected |
| Soaking in alkaline solution | 3.569 | 1.707 | Not tested |
| Electrolytic process | 0.848 | 3.306 | Not tested |
As can be seen from the above examples, the deacidification of the paper by the capacitance or capacitance adsorption method in the embodiment of the invention has lower voltage, and is easier and safer to operate. In particular in terms of safety: because the voltage is low, only the electro-adsorption process is needed, the electrode plate has no electrolytic reaction and the like, the temperature of the electrode plate is lower, and the safety of the processed paper document is ensured. In addition, the deacidification time can also be shortened. Meanwhile, the porous carbon electrode can be easily desorbed and can be repeatedly used. More important points are: the capacitor or the electric adsorption can reserve space for the subsequent paper deacidification-cleaning-reinforcement (even sterilization) integration, and has wider application prospect.
The technology of the invention is suitable for processing single, multiple and whole volumes of paper cultural relics, files and books, and can control the pH value more accurately than other deacidification methods. The invention has greatly improved efficiency, can reduce the problems of paper shrinkage, deformation, whole book sticking, low efficiency and the like caused by the traditional aqueous solution deacidification method to the maximum extent, and can also reinforce the paper. In conclusion, the deacidification technology has the remarkable advantages of good effect, high efficiency, low cost, good controllability, safety, environmental protection and the like.
The above description is only a preferred embodiment of the present invention, and it should be noted that various modifications to these embodiments can be implemented by those skilled in the art without departing from the technical principle of the present invention, and these modifications should be construed as the scope of the present invention.
Claims (9)
1. A method for deacidifying paper by an electro-adsorption method comprises the following steps:
s1, contacting the paper to be processed with a water absorption cushion layer, wherein the water absorption cushion layer contains water to wet the paper to be processed;
s2, clamping the paper wetted in the S1 and a water absorption cushion layer in contact with the paper between an inert anode plate and an inert cathode plate, covering the surface of the inert anode plate with a porous carbon material, conducting direct current to form a closed loop, conducting electric adsorption at the voltage of 0.6-1.6V, and obtaining paper after deacidification;
the inert anode plate and the inert cathode plate are graphite electrode plates; the porous carbon material is one or more of activated carbon fiber, carbon aerogel and a nano carbon tube.
2. The method according to claim 1, characterized in that the paper to be treated has a pH value of 4.5 to 6.5.
3. The method of claim 1, wherein the absorbent pad layer is a water-containing woven fabric, a water-containing non-woven fabric, or a water-containing absorbent paper.
4. The method of claim 1, wherein the porous carbon material has a BET of 500m2More than g.
5. The method of claim 4, wherein the surface of the inert anode plate is coated with activated carbon fiber cloth or activated carbon fiber felt.
6. The method according to claim 5, wherein the thickness of the activated carbon fiber cloth or activated carbon fiber felt is 1 to 5 mm.
7. A method according to any one of claims 1 to 6, wherein the time of electrosorption does not exceed 15 minutes.
8. The method of claim 7, wherein the time for the electrosorption is 1 minute to 8 minutes.
9. The method according to any one of claims 1 to 6, wherein the water-absorbing cushion layer further contains a deacidification agent, and the deacidification agent is one or more selected from calcium oxide, calcium hydroxide, calcium carbonate, calcium bicarbonate, magnesium carbonate, magnesium bicarbonate and magnesium hydroxide.
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