CN110924226A - Deacidifying reinforcing protective agent and preparation method and application thereof - Google Patents
Deacidifying reinforcing protective agent and preparation method and application thereof Download PDFInfo
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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
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Abstract
The invention discloses a deacidification strengthening protective agent and a preparation method and application thereof, wherein the deacidification strengthening protective agent comprises the following components in percentage by mass: 0.1-1% of aminosilane coupling agent, 5-20% of polyurethane, 0.1-3% of nano metal carbonate, 0.1-0.5% of polyethylene wax emulsion and the balance of ultrapure water; the protective agent prepared by the invention has the advantages of strong permeability, good dispersibility, safety, environmental protection, no toxicity and harm to paper and environment, simple and convenient practical operation, good protection effect of deacidification and reinforcement, alkalescence and aging resistance after paper treatment, prolonged preservation life of paper, no color difference change on the surface of the paper after the paper is subjected to protection treatment, and accordance with the principle of 'repairing old as old' of the paper.
Description
Technical Field
The invention provides a deacidification and reinforcement protective agent, a preparation method and application thereof, and belongs to the technical field of restoration and protection of paper cultural relics.
Background
For centuries, paper documents are the most important carriers of written information, such as written documents, books, archives, newspapers, paintings and the like, which are precious products for recording human history and continuing cultural essence, are non-renewable historical cultural heritages of important categories, and have very important artistic cultural value and historical cultural value. However, over time, under the influence of various factors, a large number of paper documents face a series of problems such as aging, yellowing, powdering and crushing in different degrees due to acidification and the like, and the usability and the storage life of the paper documents are greatly reduced. At present, at least more than 1/3 library books and literature data in the world become fragile, and acidification of paper literature becomes the first difficult problem to solve the protection of the paper literature, so that the deacidification protection treatment of a large amount of paper literature has a very important significance.
From literature reports, the current commonly used deacidification methods are an aqueous solution deacidification method, an organic solvent deacidification method and a gas phase deacidification method, the aqueous solution deacidification method is safe and environment-friendly, the deacidification effect is good, certain alkali residue can be formed, and the paper deformation and adhesion are easy to occur; paper treated by the organic solvent deacidification method is fast in drying and not easy to wrinkle, but the deacidification effect is not ideal, so that the handwriting is easy to fade, and the paper has peculiar smell. The non-aqueous organic solvent is toxic and flammable, is not friendly to the environment and has larger potential safety hazard; the gas phase deacidification method has the advantage of strong diffusivity, but has the defects of potential explosion hazard, difficult process control, harsh deacidification equipment condition, incapability of effectively forming alkali residue and the like.
Therefore, a protective agent integrating multiple functions of high permeability, high dispersibility, deacidification, reinforcement, little harm to paper, safety, environmental protection and the like is one of the most interesting research subjects in the field at present.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a water-soluble deacidification strengthening protective agent which is prepared from an aminosilane coupling agent, polyurethane, nano metal carbonate and polyethylene wax emulsion, and is efficient, safe, environment-friendly and simple to operate. According to the invention, an aminosilane coupling agent modified nano deacidification agent is combined with polyurethane, a high-dispersity solution is obtained under the auxiliary action of ultrasonic wave and mechanical stirring, and polyethylene wax emulsion is added to increase the hydrophobicity of paper to prevent the phenomenon of adhesion shrinkage in the deacidification treatment process, compared with untreated paper cultural relics, the pH value of a treated sample is increased to a better range of 7.5-9.0, meanwhile, the mechanical strength of the paper is obviously improved, a certain alkali residue is formed to relieve the aging of the paper, and the storage life of the paper is prolonged; the paper has no influence on the appearance, handwriting and the like of the paper, conforms to the principle of 'old as worn', has no toxic and harmful gas emission, and is safe and environment-friendly.
The technical scheme is as follows: in order to solve the technical problems, the invention provides a deacidification strengthening protective agent which is prepared from the following components in percentage by mass: 0.1 to 1 percent of amino silane coupling agent, 5 to 20 percent of polyurethane, 0.1 to 3 percent of nano metal carbonate, 0.1 to 0.5 percent of polyethylene wax emulsion and the balance of ultrapure water.
Wherein the aminosilane coupling agent is at least one or any combination of a plurality of gamma-aminopropyltriethoxysilane, N- (2-aminoethyl) -3-aminopropyltriethoxysilane, N-2- (aminoethyl) -3-aminopropyltrimethoxysilane, N- β - (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and phenylaminomethyltrimethoxysilane.
Wherein the polyurethane is at least one or any combination of Toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI) and Hexamethylene Diisocyanate (HDI).
Wherein the nano metal carbonate is at least one or two of nano magnesium carbonate and nano calcium carbonate.
The polyethylene wax emulsion is used for increasing the hydrophobicity of paper and reducing adhesion in the process of protecting and treating the paper.
The invention also comprises a preparation method of the deacidification strengthening protective agent, which comprises the following steps:
1) dissolving an aminosilane coupling agent in ultrapure water, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring to obtain a solution 1;
2) slowly adding nano metal carbonate into the solution 1 in the step 1), stirring while adding, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic wave and mechanical stirring to obtain a solution 2;
3) slowly adding polyurethane into the solution 2 obtained in the step 2), stirring while adding, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring to obtain a solution 3;
4) slowly adding the polyethylene wax emulsion in the formula amount into the solution 3 in the step (3), stirring continuously while adding, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring for 10-30 min to obtain the deacidification and reinforcement protective agent.
Wherein the ultrasonic power in the steps 1) to 4) is 30-100 KHz.
Wherein the stirring speed in the steps 1) to 4) is 60-100 r/min
The invention also comprises the application of the deacidification strengthening protective agent in the protection of paper cultural relics.
In the application, paper cultural relics to be treated are directly immersed into the deacidification and reinforcement protective agent, treated for 10-30 min at normal temperature, and then hung and dried for 24-80 h.
Wherein the mass ratio of the aminosilane coupling agent to the polyurethane to the nano metal carbonate to the polyethylene wax emulsion in the reaction is as follows: 0.1-1: 5-20: 0.1-3: 0.1-0.5.
Wherein, the paper cultural relics are paper documents which are produced by adopting a mechanical papermaking technology in the modern period.
The technical points of the invention are as follows: the deacidification strengthening and protecting agent with uniform dispersion is finally obtained by taking ultrapure water as a solvent, an aminosilane coupling agent as a modifier, nano metal carbonate as a deacidification agent, polyurethane as a reinforcing agent and polyethylene wax emulsion as a hydrophobic agent through the synergistic effect of the components.
Has the advantages that: the deacidification strengthening protective agent solvent prepared by the invention is ultrapure water, has no influence on human health and environment, is simple, convenient and easy to control in the operation process at normal temperature and normal pressure, can be suitable for large-scale protection treatment, can uniformly disperse nanoparticles in a polyurethane matrix by modifying the surfaces of the nanoparticles by using an aminosilane coupling agent, and is dissolved under the auxiliary action of ultrasonic waves and mechanical stirring, so that the whole solvent system is uniformly dispersed, and has strong permeability; the protective agent prepared by the invention is safe and environment-friendly, has no toxicity or harm to paper and environment, and is simple and convenient to operate practically. The pH value of the treated paper is increased to be in a better range of 7.5-9.0, so that the treated paper is alkalescent and has aging resistance, the mechanical strength of the paper is obviously improved, the deacidification and reinforcement effects are obvious, certain alkali residue is formed to relieve the aging of the paper, the phenomenon of acid return is avoided, and the storage life of the paper is prolonged. The polyethylene wax emulsion added into the protective agent prevents the paper from being adhered and damaged in the water solution treatment process, and after the paper is subjected to protective treatment, the surface of the paper has no color difference change, and the color difference change of the paper is less than 1.5, so that the principle of 'repairing the old paper' of the paper is met.
Drawings
FIG. 1 SEM image of unprotected paper processing (a);
FIG. 2 SEM image (b) of unprotected paper after dry heat aging;
FIG. 3 SEM image (c) after the paper protection process;
FIG. 4 SEM image (d) of paper protection treatment after dry heat aging.
Detailed Description
The following claims are presented to illustrate the invention in further detail with reference to specific embodiments, and any limited number of modifications that can be made by one within the scope of the claims will still fall within the scope of the invention.
Example 1
Adding 1g of gamma-aminopropyltriethoxysilane into 1000g of ultrapure water, fully stirring and mixing under the assistance of 30KHz ultrasonic power and 60r/min mechanical stirring to obtain a solution 1, slowly adding 1g of nano magnesium carbonate into the solution 1, mechanically stirring and mixing under 30KHz ultrasonic power and 60r/min mechanical power to obtain a solution 2, slowly adding 50g of toluene diisocyanate into the solution 2, mechanically stirring and mixing under 30KHz ultrasonic power and 60r/min mechanical power to obtain a solution 3, slowly adding 1g of polyethylene wax emulsion into the solution 3, fully stirring at 18 ℃ and carrying out ultrasonic treatment for 10min to obtain the deacidification reinforcement protective agent.
Soaking 6-11 sheets of paper in 800-1000 g of the deacidification strengthening protective agent at normal temperature for 15min, then placing the paper in a constant temperature and humidity environment for sample hanging and drying for 24h, testing the pH and mechanical properties of the paper, and taking the treated paper to test the pH and mechanical properties of the paper after dry heat aging treatment for 72h at 105 +/-2 ℃.
Example 2
Adding 3g of N- (2-aminoethyl) -3-aminopropyltriethoxysilane into 1000g of ultrapure water, fully stirring and mixing under the assistance of 45KHz ultrasonic wave power and 70r/min mechanical stirring to obtain a solution 1, slowly adding 5g of nano calcium carbonate into the solution 1, mechanically stirring and mixing under 45KHz ultrasonic wave power and 70r/min power to obtain a solution 2, slowly adding 80g of toluene diisocyanate into the solution 2, mechanically stirring and mixing under 45KHz ultrasonic wave power and 70r/min power to obtain a solution 3, slowly adding 2g of polyethylene wax emulsion into the solution 3, fully stirring at 30 ℃ and carrying out ultrasonic stirring for 12min to obtain the deacidification reinforcement protective agent.
Soaking 6-11 sheets of paper in 800-1000 g of the deacidification strengthening and protecting agent at normal temperature for 15min, then placing the paper in a constant-temperature constant-humidity environment for sample hanging and drying for 30h, testing the pH and mechanical properties of the paper, and taking the treated paper for dry-heat aging treatment for 72h at 105 +/-2 ℃ to test the pH and mechanical properties of the paper.
Example 3
Adding 5g of N- β - (aminoethyl) -gamma-aminopropyl methyl dimethoxysilane into 1000g of ultrapure water, fully stirring and mixing under the assistance of 60KHz ultrasonic wave power and 80r/min mechanical stirring to obtain a solution 1, slowly adding 10g of mixed nano magnesium carbonate and 5g of mixed nano calcium carbonate into the solution 1, mechanically stirring and mixing under 60KHz ultrasonic wave power and 80r/min power to obtain a solution 2, slowly adding 150g of diphenylmethane diisocyanate (MDI) into the solution 2, mechanically stirring and mixing under 60KHz ultrasonic wave power and 80r/min power to obtain a solution 3, slowly adding 3g of polyethylene wax emulsion into the solution 3, fully stirring and performing ultrasonic deacidification for 15min at 40 ℃ to obtain the reinforcing protective agent.
Soaking 6-11 sheets of paper in 800-1000 g of the deacidification strengthening and protecting agent at normal temperature for 15min, then placing the paper in a constant-temperature constant-humidity environment for sample hanging and drying for 50h, testing the pH and mechanical properties of the paper, and taking the treated paper for dry-heat aging treatment for 72h at 105 +/-2 ℃ to test the pH and mechanical properties of the paper.
Example 4
Adding 8g of N-2- (aminoethyl) -3-aminopropyltrimethoxysilane into 1000g of ultrapure water, fully stirring and mixing under the assistance of 75KHz ultrasonic waves with power and 90r/min mechanical stirring to obtain a solution 1, slowly adding 10g of nano magnesium carbonate and 10g of nano calcium carbonate into the solution 1, fully stirring and mixing under the assistance of 75KHz ultrasonic waves with power and 90r/min mechanical stirring to obtain a solution 2, slowly adding 180g of hexamethylene diisocyanate into the solution 2, fully stirring and mixing under the assistance of 75KHz ultrasonic waves with power and 90r/min mechanical stirring to obtain a solution 3, slowly adding 4g of polyethylene wax emulsion into the solution 3, fully stirring at 50 ℃, and carrying out ultrasonic stirring for 18min to obtain the deacidification strengthening protective agent.
Soaking 6-11 sheets of paper in 800-1000 g of the deacidification strengthening and protecting agent at normal temperature for 15min, then placing the paper in a constant-temperature constant-humidity environment for sample hanging and drying for 65h, testing the pH and mechanical properties of the paper, and taking the treated paper for dry-heat aging treatment for 72h at 105 +/-2 ℃ to test the pH and mechanical properties of the paper.
Example 5
Adding 10g of phenylaminomethyltrimethoxysilane into 1000g of ultrapure water, fully stirring and mixing under the assistance of 100KHz ultrasonic wave and 100r/min mechanical stirring to obtain a solution 1, slowly adding 12g of mixed nano magnesium carbonate and 18g of mixed nano magnesium carbonate into the solution 1, fully stirring and mixing under the assistance of 100KHz ultrasonic wave and 100r/min mechanical stirring to obtain a solution 2, slowly adding 100g of Toluene Diisocyanate (TDI) and 100g of diphenylmethane diisocyanate into the solution 2, fully stirring and mixing under the assistance of 100KHz ultrasonic wave and 100r/min mechanical stirring to obtain a solution 3, slowly adding 5g of polyethylene wax emulsion into the solution 3, fully stirring at 60 ℃, and carrying out ultrasonic stirring for 20min to obtain the deacidification and reinforcement protective agent.
Soaking 6-11 sheets of paper in 800-1000 g of the deacidification strengthening and protecting agent at normal temperature for 15min, then placing the paper in a constant-temperature constant-humidity environment for sample hanging and drying for 80h, testing the pH and mechanical properties of the paper, and taking the treated paper for dry-heat aging treatment for 72h at 105 +/-2 ℃ to test the pH and mechanical properties of the paper.
Comparative example 1
In the comparative example, 1g of nano magnesium carbonate is added into 1000g of ultrapure water, and the deacidification protection solution is obtained by fully stirring and mixing under the assistance of 30KHz ultrasonic waves and 60r/min mechanical stirring, and the subsequent use and test method are the same as those in example 1.
Comparative example 2
The paper protectant used in this comparative example was the same as that used in example 1, except that toluene diisocyanate was not added, and the preparation and subsequent use and test method were the same as in example 1.
Comparative example 3
The paper protective agent used in this comparative example was the same as in example 1, except that toluene diisocyanate was replaced with chitosan of equal mass, and the preparation and subsequent use and test methods were the same as in example 1.
The color difference is an important index for measuring the optical performance of the paper, the DRK whiteness instrument is used for evaluating the chroma of the paper in the experiment, and the calculation formula of the color difference is as follows:
ΔE＝((ΔL*)2+(Δa*)2+(Δb*)2)1/2
wherein the parameters L, a, b represent the luminance, hue and color saturation measures, respectively. The greater the Δ E value, the more pronounced the color change.
TABLE 1. DELTA.E evaluation criteria
The results of the experiment are shown in table 2:
the test result shows that the protective agent for the paper cultural relics prepared by the invention has good deacidification and reinforcement effects, the alkaline range of the paper after deacidification is controlled to be 7.5-9.0, the mechanical strength of the paper is also obviously improved, the color difference change of the paper cultural relics is controlled to be less than 1.5, and the paper cultural relics can be considered to have no color change, namely, the color difference change of the paper is not influenced, and the paper cultural relics conform to the principle of 'repairing the old' of the paper. While the deacidification agent in the comparative example 1 is the same, but the deacidification effect is poor due to the lack of the modifier, and the polyurethane is respectively lacked and replaced in the comparative examples 2 and 3, so that the deacidification strengthening protective agent prepared by only using the nano metal carbonate subjected to the surface treatment of the aminosilane coupling agent is poor in strength and stability and is introduced into a polyurethane chain, the surface treatment of the aminosilane coupling agent can strengthen the interaction between the nano metal carbonate and a polyurethane matrix, a three-dimensional crosslinking system is formed by the bridging among fibers, and the tensile strength and the aging performance of paper are obviously improved macroscopically. Chitosan is not easy to hydrolyze in an alkaline environment, the reinforcing effect is not ideal, and yellowing is easy to occur after aging.
Claims (9)
1. The deacidification strengthening protective agent is characterized by comprising the following components in percentage by mass: 0.1-1% of aminosilane coupling agent, 5-20% of polyurethane, 0.1-3% of nano metal carbonate, 0.1-0.5% of polyethylene wax emulsion and the balance of ultrapure water.
2. The deacidification strengthening and protecting agent according to claim 1, wherein the aminosilane coupling agent is at least one of gamma-aminopropyltriethoxysilane, N- (2-aminoethyl) -3-aminopropyltriethoxysilane, N-2- (aminoethyl) -3-aminopropyltrimethoxysilane, N- β - (aminoethyl) -gamma-aminopropylmethyldimethoxysilane and phenylaminomethyltrimethoxysilane or any combination of several kinds of these.
3. The deacidification strengthening and protecting agent according to claim 1, wherein the polyurethane is at least one or any combination of toluene diisocyanate, diphenylmethane diisocyanate and hexamethylene diisocyanate.
4. A method for preparing a deacidification strengthening and protecting agent as claimed in any one of claims 1 to 3, which comprises the following steps:
1) dissolving an aminosilane coupling agent in ultrapure water, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring to obtain a solution 1;
2) slowly adding nano magnesium carbonate or/and nano calcium carbonate into the solution 1 in the step 1), stirring while adding, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring to obtain a solution 2;
3) slowly adding polyurethane into the solution 2 obtained in the step 2), stirring while adding, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring to obtain a solution 3;
4) slowly adding the polyethylene wax emulsion in the formula amount into the solution 3 in the step (3), stirring continuously while adding, and dissolving at 18-60 ℃ under the auxiliary action of ultrasonic waves and mechanical stirring for 10-30 min to obtain the deacidification and reinforcement protective agent.
5. The preparation method of the deacidification strengthening protective agent according to claim 4, wherein the ultrasonic power in the steps 1) to 4) is 30 to 100 KHz.
6. The preparation method of the deacidification strengthening and protecting agent according to claim 4, wherein the stirring speed in the step 1) to 4) is 60 to 100 r/min.
7. Use of the deacidification strengthening and protecting agent as claimed in any one of claims 1 to 3 in the protection of paper cultural relics.
8. The application of the paper cultural relics as claimed in claim 7, wherein the paper cultural relics to be treated are directly immersed into the deacidification, reinforcement and protection agent, treated for 10-30 min at normal temperature, and then hung and dried for 24-80 h.
9. The use of claim 8, wherein the mass ratio of the aminosilane coupling agent to the polyurethane to the nano metal carbonate to the polyethylene wax emulsion in the reaction is 0.1-1: 5-20: 0.1-3: 0.1 to 0.5.
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| CN113882188A (en) * | 2021-09-28 | 2022-01-04 | 复旦大学 | Protection method of paper cultural relics containing transition metal |
| CN116289318A (en) * | 2023-04-28 | 2023-06-23 | 常州大学 | Paper deacidification and reinforcement method |
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