US3771958A - Gaseous diffusion paper deacidification - Google Patents
Gaseous diffusion paper deacidification Download PDFInfo
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- US3771958A US3771958A US00214217A US3771958DA US3771958A US 3771958 A US3771958 A US 3771958A US 00214217 A US00214217 A US 00214217A US 3771958D A US3771958D A US 3771958DA US 3771958 A US3771958 A US 3771958A
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- 238000009792 diffusion process Methods 0.000 title description 3
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims abstract description 94
- 230000006866 deterioration Effects 0.000 claims abstract description 17
- 230000002378 acidificating effect Effects 0.000 claims abstract description 11
- 238000011282 treatment Methods 0.000 claims description 54
- 238000000034 method Methods 0.000 claims description 47
- 238000005470 impregnation Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 230000032683 aging Effects 0.000 description 26
- 238000002474 experimental method Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000002023 wood Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 230000005923 long-lasting effect Effects 0.000 description 4
- 238000003860 storage Methods 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 244000198134 Agave sisalana Species 0.000 description 1
- 240000000491 Corchorus aestuans Species 0.000 description 1
- 235000011777 Corchorus aestuans Nutrition 0.000 description 1
- 235000010862 Corchorus capsularis Nutrition 0.000 description 1
- 240000006240 Linum usitatissimum Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229940079938 nitrocellulose Drugs 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Images
Classifications
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/07—Nitrogen-containing compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
- A61L2/20—Gaseous substances, e.g. vapours
-
- 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
Definitions
- ABSTRACT Paper for example having a pH of about 5.0 or lower, is rendered resistant to the deterioration that is promoted by acidic conditions in paper by impregnating the paper, for example in the form of a book, with gaseous morphoiine.
- This invention relates to a process for treating paper to render it resistant to the deterioration that is promoted by acidic conditions in paper. More particularly, it concerns such a process wherein the treatment constitutes impregnating the paper with gaseous morpholine.
- Still other methods of treatment may require the use of particularly noxious andlor strongly toxic chemicals (e.g., cyclohexylamine), thereby requiring relatively elaborate equipment to conduct the treatment safely.
- particularly noxious andlor strongly toxic chemicals e.g., cyclohexylamine
- FIG. 1 is a view, partly broken away, of an apparatus suited for the practice of the process of the invention.
- FIG. 2 is a horizontal section, taken along line 22 of FIG. 1.
- the extent of morpholine impregnation of paper that is to be deacidified by the process of the present invention is preferably sufficient to provide the paper with a pH (measured after the paper has been allowed to stand at room temperature and atmospheric pressure for 24 hours) of at least about 7.6, preferably at least about 8.5.
- the pH values referred to are those of the resultant aqueous solution when one gram of oneeighth inch square pieces of the treated paper is soaked for 1 hour in ml. of distilled, deionized water at room temperature.
- the initial pH value of paper which is susceptible to the deterioration that is alleviated by the present invention is usually about 5.0 or lower, and frequently about 4.3 or lower.
- the time period required to complete such an impregnation process will of course vary, depending upon the amount and type of paper being treated, the amount of morpholine employed, the treatment temperature, the pH level desired for the paper, etc.
- a book having an initial pH of, for instance, about 4.3 can be made to have a pH of 8.3 in as little as 8 hours when immersed in an approximately [00 percent morpholine atmoshpere at room temperature. No harm to the paper has been observed to occur through prolonged treatments, but it is generally unnecessary to continue the treatment for more than about 4 days.
- the gaseous morpholine used in the present process can, if desired, be in admixture with one or more other gases, such as air, that are non-interfering with the deacidification process.
- the morpholine accounts for at least about one-third, and most preferably a major amount, e.g. about to I00 percent, or even 98 to 100 percent, of the volume of the atmosphere surrounding the paper during treatment.
- impregnation of the paper with the gaseous morpholine can be effected by simply contacting the aper with morpholine vapors.
- the vapors may be under atmospheric, sub-atmosphierc or superatmospheric pressure.
- the pressure exerted by a 100 percent morpholine atmosphere is about 7 to 10 mm. Hg, which is entirely adequate to penetrate the paper.
- paper treated according to the present process retains its high pH slightly better, and therefore better maintains its resistance to deterioration, if it is kept in a dry atmosphere.
- FIG. 1 of the attached drawings there is shown a rigid, round containment vessel fitted with a lid 11 that is clamped in place during use by clamps l2 and 13.
- a rigid, round containment vessel fitted with a lid 11 that is clamped in place during use by clamps l2 and 13.
- an open bowl 14 which contains a much smaller, open dish 15.
- a horizontal screen 16 Resting on the top of bowl 14 is a horizontal screen 16 which substantially fills the cross-sectional area of vessel 10.
- Mounted to the underside of lid 11 is fan blade 17, driven by motor 18.
- Mounted on top of lid 11 is handle 19.
- the diameter of vessel 10 is about inches at its base and about inches at its top.
- the height of the vessel is about 26 inches.
- the above apparatus is used in practicing the present process by placing liquid morpholine in dish 15, then putting screen 16 in place on top of bowl 14, and then placing the paper to be treated on top of screen 16.
- the lid 11 is then clamped into place and fan motor 18 is turned on.
- the morpholine then vaporizes and mixes with the air in the vessel and impregnates the paper.
- the treatment time in the morpholine-containing vessel was shortened with each succeeding set of experiments, as reported hereinafter in Tables I, ll and Ill.
- Tables I, ll and Ill The treatment time in the morpholine-containing vessel was shortened with each succeeding set of experiments, as reported hereinafter in Tables I, ll and Ill.
- some of the paper samples were immediately evaluated for pH, fold endurance, and tear resistance, while the remainder were first heat-aged in a dry oven for varying periods at l00C.
- the pH levels of the treated samples (reported in Table l) were measured after each aging period, and the fold endurance and tear resistance values (reported in Tables ll and III) were obtained after the 12 day aging period. From the fold endurance and tear resistance values were calculated the useful half-lives of the treated and untreated paper at the dry oven accelerated aging temperature, 100C. These too are reported in Tables ll and III.
- Fold endurance testing was performed with The Mars sachusetts Institute of Technology Folding Endurance Tester which repeatedly bends a 15 mm. wide strip of the paper to be tested across a line in a 270 arc, under A kilogram tension, until failure. The endurance was recorded as the average number of bends endured per strip, after testing 50 strips. Both machine directional fold endurance (M.D.) and cross directional fold endurance (C.D.) were determined in this manner.
- M.D. machine directional fold endurance
- C.D. cross directional fold endurance
- test data in Table 1 illustrate quite clearly the long-lasting quality of the deacidification that is effected by the process of the present invention.
- the test data in Tables I1 and ill demonstrate that the deacidification treatment of the present invention provides resistance to strength loss and a much longer useful life than that to be expected for the untreated paper.
- the paper that had been treated with morpholine for 96 hours i.e., that of set 1
- the untreated paper had a half-life under those conditions of only 2.3 days M.D. and 4 days C.D.
- the tear resistance half-life at 100C. of the paper that was treated with morpholine for 96 hours was about 30 hours in both directions, while the untreated papers half-life was only about 9 hours in both directions.
- samples of the same type of chemical wood paper used in Example 1 were treated with gaseous morpholine, and untreated control samples were tested for tear resistance as well as pH.
- the process of this invention is applicable to any paper that is subject to deterioration due to acidic conditions in the paper.
- the paper can be manufactured from, for instance, sisal, jute, flax, wood, cotton, or any combination of the foregoing.
- Other experiments have been run, for instance, with a paper composed of 50 percent cotton linter and 50 percent chemical wood furnish which had a pH of about 4.7. impregnation with gaseous morpholine raised that pH to about 8.6, and the paper retained its basicity and physical properties as in the case of the 100 percent chemical wood paper.
- a process for treating paper to render it resistant to the deterioration that is promoted by acidic conditions in paper comprises impregnating the paper with a gaseous atmosphere consisting essentially of morpholine, the said morpholine being present in at least about one-third the volume of the said gaseous atmosphere.
- a process of treating a book made of paper having a pH of about 5.0 or lower so as to render the paper resistant to the deterioration that is promoted by acidic conditions comprises impregnating the book with a gaseous atmosphere consisting essentially of morpholine, the said morpholine being present in at least about one-third the volume of said gaseous atmosphere, at about 25 to C. in an amount sufficient to raise the pH of the paper to at least about 8.5, said pH values being as determined by soaking one gram of one-eighth inch squares of the paper for one hour in 70 ml. of distilled, deionized water at room temperature and then measuring the pH of the resultant aqueous solution.
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
Paper, for example having a pH of about 5.0 or lower, is rendered resistant to the deterioration that is promoted by acidic conditions in paper by impregnating the paper, for example in the form of a book, with gaseous morpholine.
Description
United States Patent [1 1 Kusterer, Jr. et a1.
[ Nov. 13, 1973 1 GASEOUS DIFFUSION PAPER DEACIDIFICATION [75] Inventors: James E. Kusterer, Jr.; Reavis C.
Sprouli, both of Richmond, Va.
[73] Assignee: Research Corporation, New York,
[22] Filed: Dec. 30, 1971 [21] Appi. No.: 214,217
[52] US. Cl 21/58, 21/7, 21/76,
117/154, 252/401 [51] Int. Cl A611 13/00 [58] Field of Search 21/58, 7, 76;
[56] References Cited UNITED STATES PATENTS 3,472,611 10/1969 Langweli 21/58 2,185,954 1/1940 Ryner 21/58 UX 3,135,627 6/1964 Sadier 117/143 3,419,498 12/1968 Paiumbo et a1 162/160 X Primary Examiner-Morris O. Wolk Assistant Examiner-D. G. Miilman Attorney-John W. Behringer et a1.
[57] ABSTRACT Paper, for example having a pH of about 5.0 or lower, is rendered resistant to the deterioration that is promoted by acidic conditions in paper by impregnating the paper, for example in the form of a book, with gaseous morphoiine.
10 Claims, 2 Drawing Figures PATENIED NM 13 I975 FIG].
F/GZ.
GASEOUS DIFFUSION PAPER DEACIDIFICATION This invention relates to a process for treating paper to render it resistant to the deterioration that is promoted by acidic conditions in paper. More particularly, it concerns such a process wherein the treatment constitutes impregnating the paper with gaseous morpholine.
The recognition of the severe problem of deterioration of documents printed on paper that is or becomes acidic has prompted the development of several different processes for deacidifying such paper so as to halt or slow its deterioration. Prime examples of acidic papers which are susceptible to such deterioration (caused by hydrolysis of acidic ions which impregnate the cellulose during manufacture) are groundwood (as opposed to chemical wood) papers and alum-rosin sized papers, whether made of wood or rags. Some of the deacidification processes which have heretofore been developed are disclosed in "Restoration Methods, by W. J. Barrow, The American Archivist, 6: ll-l54, July 1943; Permanence/Durability of the Book-ll]: Spray Deacidification," published by W. J. Barrow Research Laboratory, 1964; "Vapor Phase Deacidification: A New Preservation Method," by Paul McCarthy, The American Archivist, 32: 333-342, October i969; and U.S. Pat. No. 3,472,611 to Langwell. Each of these processes shares at least one common ob jective: to efi'ect a long lasting elevation of the pH of the paper. If this is accomplished, then the deterioration of the paper that is induced by acidic conditions therein will be substantially alleviated.
The paper deacidification processes heretofore developed, however, often possess significant drawbacks. Some, for example those involving a leaf-by-leaf treatment, while perhaps technically effective, are prohibitively expensive. Others, such as ammoniation, may provide only a short-lived resistance to deterioration. Still other processes may be longer lasting in their intended effect, but have one or more undesirable side effects, such as causing discoloration, e.g., yellowing, of the paper, diminution of the papers fold endurance, cockling of the paper, and leaving the paper with a lingering, unpleasant odor. Still other methods of treatment may require the use of particularly noxious andlor strongly toxic chemicals (e.g., cyclohexylamine), thereby requiring relatively elaborate equipment to conduct the treatment safely. There is, then, an urgent need for effective, safe and relatively inexpensive methods of treating paper so as to render it resistant to acid-catalyzed deterioration. The magnitude of the problem is revealed, for example, in The Case of the Vanishing Records, by David G. Lowe, American Heritage, volume XX, No. 5 (1969), page 34.
The invention will be understood from the following description, made with reference to the accompanying drawings. In the drawings:
FIG. 1 is a view, partly broken away, of an apparatus suited for the practice of the process of the invention; and
FIG. 2 is a horizontal section, taken along line 22 of FIG. 1.
it has now been discovered that paper which is susceptible to acid-catalyzed deterioration can be efi'ectively, safely, and relatively inexpensively deacidified, and thereby made resistant to such deterioration, if it is impregnated with gaseous morpholine. Moreover, it
has been found that such treatment can be effected even with tightly closed books, so well will 7.6, penetrate them, and the resultant deacidification is extremely long lasting, maybe even permanent.
The extent of morpholine impregnation of paper that is to be deacidified by the process of the present invention is preferably sufficient to provide the paper with a pH (measured after the paper has been allowed to stand at room temperature and atmospheric pressure for 24 hours) of at least about 7.6, preferably at least about 8.5. The pH values referred to are those of the resultant aqueous solution when one gram of oneeighth inch square pieces of the treated paper is soaked for 1 hour in ml. of distilled, deionized water at room temperature. As determined by this method, the initial pH value of paper which is susceptible to the deterioration that is alleviated by the present invention is usually about 5.0 or lower, and frequently about 4.3 or lower.
The time period required to complete such an impregnation process will of course vary, depending upon the amount and type of paper being treated, the amount of morpholine employed, the treatment temperature, the pH level desired for the paper, etc. As an example, however, a book having an initial pH of, for instance, about 4.3 can be made to have a pH of 8.3 in as little as 8 hours when immersed in an approximately [00 percent morpholine atmoshpere at room temperature. No harm to the paper has been observed to occur through prolonged treatments, but it is generally unnecessary to continue the treatment for more than about 4 days.
No special treatment temperature is required for the present process; however, preferred operating temperatures are in the range of about 5C. to 128C, most especially about 25C. to C.
The gaseous morpholine used in the present process can, if desired, be in admixture with one or more other gases, such as air, that are non-interfering with the deacidification process. Preferably, though, the morpholine accounts for at least about one-third, and most preferably a major amount, e.g. about to I00 percent, or even 98 to 100 percent, of the volume of the atmosphere surrounding the paper during treatment.
impregnation of the paper with the gaseous morpholine can be effected by simply contacting the aper with morpholine vapors. The vapors may be under atmospheric, sub-atmosphierc or superatmospheric pressure. At room temperature the pressure exerted by a 100 percent morpholine atmosphere is about 7 to 10 mm. Hg, which is entirely adequate to penetrate the paper.
It may be desirable after treating paper according to the present process to pass air over the paper under subatrnospheric pressure so as to permit the escape of any excess morpholine present and thereby lessen the residual morpholine odor of the .paper.
It has been observed that the treatment of this invention can discolor and/or render tacky any book covers that contain pyroxylin. Such covers should therefore preferably either be removed or tightly encased in a protective covering such as polyethylene film prior to treatment of the book.
It has also been observed that paper treated according to the present process retains its high pH slightly better, and therefore better maintains its resistance to deterioration, if it is kept in a dry atmosphere. The
more humid the storage atmosphere, the somewhat poorer will be the pH retention. Nevertheless, the present process is useful even if not followed by storage in a dry atmosphere, as evidenced by the fact that even 6 months storage under I percent relative humidity at 23C. will cause only a modest drop in pH, e.g., from about 8.5 to 7.4 or 7.7.
The invention will be better understood by reference to the following non-limiting examples.
EXAMPLE 1 Four sets of experiments were run using the apparatus shown in FIG. 1 of the attached drawings. Referring now to H6. I, there is shown a rigid, round containment vessel fitted with a lid 11 that is clamped in place during use by clamps l2 and 13. In the bottom of vessel 10 is an open bowl 14 which contains a much smaller, open dish 15. Resting on the top of bowl 14 is a horizontal screen 16 which substantially fills the cross-sectional area of vessel 10. Mounted to the underside of lid 11 is fan blade 17, driven by motor 18. Mounted on top of lid 11 is handle 19. The diameter of vessel 10 is about inches at its base and about inches at its top. The height of the vessel is about 26 inches.
The above apparatus is used in practicing the present process by placing liquid morpholine in dish 15, then putting screen 16 in place on top of bowl 14, and then placing the paper to be treated on top of screen 16. The lid 11 is then clamped into place and fan motor 18 is turned on. The morpholine then vaporizes and mixes with the air in the vessel and impregnates the paper.
In each experiment samples of 100 percent chemical wood paper were treated in the apparatus of FIG. I with gaseous morpholine at room temperature. The paper is composed of 49 percent Puget sulphite pulp, 24 percent bleached soda pulp, and 27 percent Astracel hardwood pulp, is filled with bag clay, and is sized with alumrosin. Control samples of the paper (untreated) were tested for pH, tear resistance, and fold endurance.
The treatment time in the morpholine-containing vessel was shortened with each succeeding set of experiments, as reported hereinafter in Tables I, ll and Ill. After treatment, some of the paper samples were immediately evaluated for pH, fold endurance, and tear resistance, while the remainder were first heat-aged in a dry oven for varying periods at l00C. The pH levels of the treated samples (reported in Table l) were measured after each aging period, and the fold endurance and tear resistance values (reported in Tables ll and III) were obtained after the 12 day aging period. From the fold endurance and tear resistance values were calculated the useful half-lives of the treated and untreated paper at the dry oven accelerated aging temperature, 100C. These too are reported in Tables ll and III.
Fold endurance testing was performed with The Mars sachusetts Institute of Technology Folding Endurance Tester which repeatedly bends a 15 mm. wide strip of the paper to be tested across a line in a 270 arc, under A kilogram tension, until failure. The endurance was recorded as the average number of bends endured per strip, after testing 50 strips. Both machine directional fold endurance (M.D.) and cross directional fold endurance (C.D.) were determined in this manner.
Tear resistance testing was performed with the Elmendorf Tear Tester.
TABLE I pH Length of pll after treatment and aging at 100 C. for the following helore morpholine pH after number of days treattreatment, treatment. Sel. merit hours before aging 2 days 4 days 6 days 8 days 10 days 12 (lays 4.3 8 4 8.4 8.8 7.!) 7.8 7.6 7,5 4. 3 8. 6 8. 4 8.] 7. 7 7. 5 ti. 4 fl. [l 4. 3 8. 7 7 S 7. ll 7. 2 6. l G. 9 ti. 6 4. 3 8. 6 7 7 6. 8 7.0 5. ti 5. H (i. I)
TABLE It Average told endurance after treatment, bends per strip I Average [old endurance before treatment or ag- Length of After treatment, After treatment, Hall-life (days) mg, bends per strip morpholine before aging after 12 days aging at 100 C. treatment, Set MI). 0 D hours M.D. C.D. MD. C.D. M1). (3.1).
397 88 9B 347 El 62 36 4. 6 l0. 7 397 88 48 360 B1 21 3 7 397 88 24 418 98 24 26 3 6. 4 397 88 8 352 91 11 i7 2. 4 4. 6 397 88 None 397 88 1D 12 2. 3 4
Aged but not treated with morpholine.
TABLE III Average tear resistance alter treatment, grams tear Average tear resistance before treatment. or aging, Length of Alter treatment, After treatment, Hall-lilo (days) grams tear morpholine before aging alter 1'2 days aging at I00" (7. treatment, e hot v1.1) C D hours MI). (3.1). MI). (Ll). MA). (3.1).
5'2. 0 57. z 96 56. 2 60. 1 41. l 43. 8 3D. 2 52. [l 57. .2 4B 53. 2 B2. 0 33. 7 40. 0 2t). 4 21 52.1) 57. 2. 24 53. U 65. 0 39. J 48.1) 27 27 52.0 57. .2 it 54.1 50.8 34. 38.5 18.7 17.3 52.1) 57. 2 Nom- '5.!. ll 57. Z '17.!) 2}. 4 8 7 J. 3
Aged but not treated with morpholine.
The test data in Table 1 illustrate quite clearly the long-lasting quality of the deacidification that is effected by the process of the present invention.
The test data in Tables I1 and ill demonstrate that the deacidification treatment of the present invention provides resistance to strength loss and a much longer useful life than that to be expected for the untreated paper. Thus, for example, the paper that had been treated with morpholine for 96 hours (i.e., that of set 1), had a fold endurance half-life at 100C. of 4.6 days in the machine direction and 10.7 days in the cross direction, whereas the untreated paper had a half-life under those conditions of only 2.3 days M.D. and 4 days C.D. Similarly, the tear resistance half-life at 100C. of the paper that was treated with morpholine for 96 hours was about 30 hours in both directions, while the untreated papers half-life was only about 9 hours in both directions.
EXAMPLE [I Four more sets of experiments were run, but using a different apparatus than that depicted in FIG. 1 of the attached drawings. The essential difference was that the apparatus used for this set of experiments was airthis example was considerably greater, due to the removal of air by the vacuum pump. To prevent morpholine from contacting and possibly harming the pump, a condenser was placed in the line between the treatment chamber and the vacuum pump.
in this apparatus and manner, then, samples of the same type of chemical wood paper used in Example 1 were treated with gaseous morpholine, and untreated control samples were tested for tear resistance as well as pH.
Again the treatment time was shortened with each succeeding set of experiments, as reported hereinafter in Tables 1V, V, and V1. After treatment, some of the paper samples were immediately evaluated for pH, folding endurance, and tear resistance, while the remainder were first heat-aged in a dry oven for varying periods at 100C. The pH levels of the treated samples (reported in Table IV) were measured after each aging period, and the fold endurance and tear resistance values were obtained after the 12 day aging period. From the folding endurance and tear resistance values there was calculated for each sample the half-lives (both M.D. and CD.) after the 12 day accelerated aging process. These percentages are reported in Tables V & V1.
TABLE IV 1V" 4.3 96 9.1 8.9 8.8 8.7 8.5 8.5 8.5 2V" 4.3 48 9.1 8. 5 8.8 8.3 8. 4 8.5 8. 4 3V 4.3 24 8.9 8.5 8. l 8.4 8.4 8.3 8. .2 4V 4.3 8 9.0 8. 5 8. 5 8.3 7. 4 7.8 8. 0
"V=Treated in vacuum chamber.
TABLE V Average 101d endurance Average told endurance after treatment, bends per strip before treatment or ag- Length of After treatment After treatment, Half-life (days) ing, bends per strip morpholine before aging after 12 days aging at 100 C.
res ment Set MJ) C.D. hours M.D. C.D. M.D. C.D. M.D. (1.1).
397 88 96 136 19 16 4. 5 1(1 397 88 48 143 44 20 16 4. 7 $1 397 88 24 171 49 2B 20 5 10. 3 397 88 B 154 54 23 Z] 4. 3 R. 7 397 88 None 397 '88 10 12 2. 3 4
Aged but not treated with morpholine. "V=Ireated in vacuum chamber.
TABLE VI Average tear resistance after treatment, grams tear Average tear resistance before treatment or Length of After treatment, After treatment, Half-life (days) aging, grams tear morpholine before aging alter 12 days aging at 100 C. treatment, W Set M.D C.D. hours M.D. O.D. M.D. C.D. M.D. CD
52. 0 57. 2 96 56. 8 64. 0 37. 9 43. 6 23. 4 27 52. 0 57. 2 48 56. 0 60. 4 41. 8 47. 2 33. 7 35 52. 0 57. 2 24 53. 3 60. l) 40. l 47. 0 3'2 34. 3 52. 0 57. 2 8 54. 7 62. 5 40. 8 47. 4 25. 7 28 Control 52. 0 57. 2 None '52. 0 '57. 2 '17. El 21. 4 8. 7 9. 3
'Aged but not treated with morpholine. =Treated in vaceum chamber.
tight and attached to a vacuum pump. in each of the present experiments, then, the impregnation chamber was placed under a partial vacuum, measuring about 30 inches of mercury. Thus, as compared to the experiments of Example 1, the morpholine concentration in the gaseous atmosphere around the paper treated in The test data in Table IV again illustrate quite clearly the long-lasting quality of the deacidification that is effected by the process of the present'lnvention. Also, the values indicate that higher pH values are obtained by using a more concentrated morpholine atmosphere in treating the paper than that used in Example I.
It was also noted, but not reported in Table N, that a decrease in the pH of the treated paper is generally effected by extensive handling of the paper, as, for example, in testing it for tear resistance. This pH depression is generally slight, however. In the case of the samples reported on in Table IV, for instance, the pH of the paper after aging and testing was usually at least 8.0 and was always at least 7.5.
The test data reported in Tables V and V] again show quite clearly that the morpholine treatment of the present invention enables the paper to withstand much better the accelerated aging process, insofar as the papers tear resistance and folding endurance properties are concerned, than if the paper were not so treated.
As indicated above, the process of this invention is applicable to any paper that is subject to deterioration due to acidic conditions in the paper. Thus, the paper can be manufactured from, for instance, sisal, jute, flax, wood, cotton, or any combination of the foregoing. Other experiments have been run, for instance, with a paper composed of 50 percent cotton linter and 50 percent chemical wood furnish which had a pH of about 4.7. impregnation with gaseous morpholine raised that pH to about 8.6, and the paper retained its basicity and physical properties as in the case of the 100 percent chemical wood paper.
We claim:
1. A process for treating paper to render it resistant to the deterioration that is promoted by acidic conditions in paper, which process comprises impregnating the paper with a gaseous atmosphere consisting essentially of morpholine, the said morpholine being present in at least about one-third the volume of the said gaseous atmosphere.
2. The process of claim 1 wherein the paper is in the form of a book.
3. The process of claim 1 wherein the morpholine accounts for about 90 to 100 volume percent of the atmosphere surrounding the paper during the impregnation.
4. The process of claim 3 wherein the paper is in the form of a book.
5. The process of claim 1 wherein the amount of morpholine impregnated into the paper is sufficient to provide the paper with a pH (measured after the paper has been allowed to stand at room temperature and atmospheric pressure for 24 hours) of at least about 7.6, as determined by soaking one gram of one-eighth inch squares of the paper for one hour in ml. of distilled, deionized water at room temperature and then measuring the pH of the resultant aqueous solution.
6. The process of claim 5 wherein the paper is in the form of a book.
7. The process of claim 5 wherein the paper prior to treatment has a pH of about 5.0 or lower.
8. The process of claim 7 wherein the paper is in the form of a book.
9. A process of treating a book made of paper having a pH of about 5.0 or lower so as to render the paper resistant to the deterioration that is promoted by acidic conditions, which process comprises impregnating the book with a gaseous atmosphere consisting essentially of morpholine, the said morpholine being present in at least about one-third the volume of said gaseous atmosphere, at about 25 to C. in an amount sufficient to raise the pH of the paper to at least about 8.5, said pH values being as determined by soaking one gram of one-eighth inch squares of the paper for one hour in 70 ml. of distilled, deionized water at room temperature and then measuring the pH of the resultant aqueous solution.
10. The process of claim 9 wherein the morpholine accounts for about to volume percent of the atmosphere surrounding the book during the impregnatlon.
t I i U UNIT D STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No. 3,77 ,95 Dated November 3, 973
InVentOI-(S) James E. Kusterer, Jr., and Reavis C. Sproull It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
Column 2, line 2, "7.6, should read --the morpholine--:
'line 46, "aper" should read --paper--;
line +8, "sub-atmosphierc should read --subatmospheric--. Columns 3 and 4, Table III. fifth column, "53.0" should read --5 I.O--. Columns 5 and 6, Table IV should have column headings so as to read as follows:
new
'pH Before I length 0! pH After Treatment, pH After Treatment and Aging 100 C}. for the Set Treatment Morphollne Before Aging fiollowlng number of days Treatment 2 days 4 days 6 days 8 days 10 days 12 days 1 V" 4.3 hours 9.1 8.9 8.8 8.7 8.5 8.5 8.5
a v 4.3 48 hours 7 9.1 8.5 8.8 8.3 8.4 8.5 Y 8.4
a v 4.3 24 hours 8.9 8.5 8.1 8.4 8.4 8.3 8.2
4 V" 4.3 8 hours 9.0 8.6 8.5 8.3 "7.4 7.8 8.0
Treated invacuum chamber Signed and sealed this 2nd day of April 1971;.
(SEAL) Attest:
EDWARD M.FIETCHER,JR. c. MARSHALL DANN Attesting Officer Commissioner of Patents FORM PO-l050 (IO-69) USCOMM-DC 60376-P69 U.S. GOVERNMENT PRINTING OFFICE I989 O'366-8J4.
Patent No. 3577 895 Dated November 35 973 In e t James E. Kusterer, Jr., and Reavis C. Sproull It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
Column 2,1 line 2, "7.6, should read --the morpholine-:
"line '46, "aper" should read --p-aper--;
line 48, "sub-atmosphierc" should read --subatmospheric--. Columns 3 and 4, .Table III. fifth column, "53.0" should 7 read --5 +.0- I Columns 5 and 6, Table IV should have column headings so 1 as to read as follows:
pH Before Length of pH After Treatment, pH Mme; "Treatment 'and Aging 100 C. for the Set Treatment Morphollne Before Aging iollowing number of days Treatment 2 days 4 days 6 days 8 bye 10 days 12 days 1v" 4.3 95mm 9.1 8.9 8.8 8.7 8.5 I 8.5 8.5
1v 4.3 48 hour! 8.1 v 8.5 8.8 8.3 8.4 8.5 8.4 3 4,3 24 hours 8.9 8.5 8.1 8.4 8.4 8.3 8.2
4V" 4.3 Shouts 9.0 I 8.6 I 8.5 8.3 "7.4 7.8 8.0
" .ITIGIIBG in vacuum: 'chamber Signed and sealed this 2nd day of April 1978.:
(SEAL) Attest: I
EDWARD M.FIETCHER,JR. c. MARSHALL DANN Attest'ing Officer Commissioner of Patents U.S. GOVERNMENT PRINTING OFFICE l9, 0-30-834.
FORM Po-1o5o (10-69) USCOMWDC x Patent No.
Inventor(s) Dated November 13, 1973 James E. Kusterer, Jr., and Reavis C. Sproull It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
Column 2, line 2, "7.6, should read --the morpholine--:
line 46, "aper" should read --paper-; line 48, "sub-atmosphierc" should read --subatmospheric".
Columns 3 and 4, Table III, fifth column, "53.0" should read 54.0".
Columns 5 and 6, Table IV should have column headings so as to read as follows:
Table IV pH Before length 0! pH After Treatment, pH After Treatment and Aging 100' C. to; the Set Treatment Morpholme Beflore Aging following number of days Treatment 2 dayl 4 days 6 days 8 days 10 days 12 days IV" 4.3 96hourl 9.1 8.9 8.8 8.7 8.5 8.5 8.5
i V" 4.3 48 houtl 9.1 8.5 8.8 8.3 8.4 8.5 8.4
3 V" 4.3 24 hour! 8.9 8.5 8.1 8.4 8.4 8.3 8.2
4V" 4.3 Bhourl 9.0 8.6 8.5 8.3 7.4 7.8 8.0
" I Tuned in vacuum chamber Signed and sealed this 2nd (SEAL) Attest:
EDWARD M.FIETCHER,JR. Attesting Officer II PO-IDSO (10-69) day of April 1971+.
USCOMM'DC 5376-P59 1! [1.5. GOVIHNIENT HIIIIIIIG OIIICE llll 0-588-314.
Claims (9)
- 2. The process of claim 1 wherein the paper is in the form of a book.
- 3. The process of claim 1 wherein the morpholine accounts for about 90 to 100 volume percent of the atmosphere surrounding the paper during the impregnation.
- 4. The process of claim 3 wherein the paper is in the form of a book.
- 5. The process of claim 1 wherein the amount of morpholine impregnated into the paper is sufficient to provide the paper with a pH (measured after the paper has been allowed to stand at room temperature and atmospheric pressure for 24 hours) of at least about 7.6, as determined by soaking one gram of one-eighth inch squares of the paper for one hour in 70 ml. of distilled, deionized water at room temperature and then measuring the pH of the resultant aqueous solution.
- 6. The process of claim 5 wherein the paper is in the form of a book.
- 7. The process of claim 5 wherein the paper prior to treatment has a pH of about 5.0 or lower.
- 8. The process of claim 7 wherein the paper is in the form of a book.
- 9. A process of treating a book made of paper having a pH of about 5.0 or lower so as to render the paper resistant to the deterioration that is promoted by acidic conditions, which process comprises impregnating the book with a gaseous atmosphere consisting essentially of morpholine, the said morpholine being present in at least about one-third the volume of said gaseous atmosphere, at about 25* to 75*C. in an amount sufficient to raise the pH of the paper to at least about 8.5, said pH values being as determined by soaking one gram of one-eighth inch squares of the paper for one hour in 70 ml. of distilled, deionized water at room temperature and then measuring the pH of the resultant aqueous solution.
- 10. The process of claim 9 wherein the morpholine accounts for about 90 to 100 volume percent of the atmosphere surrounding the book during the impregnation.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US21421771A | 1971-12-30 | 1971-12-30 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3771958A true US3771958A (en) | 1973-11-13 |
Family
ID=22798244
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00214217A Expired - Lifetime US3771958A (en) | 1971-12-30 | 1971-12-30 | Gaseous diffusion paper deacidification |
Country Status (2)
Country | Link |
---|---|
US (1) | US3771958A (en) |
GB (1) | GB1422385A (en) |
Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3969549A (en) * | 1974-12-24 | 1976-07-13 | The United States Of America As Represented By The Librarian Of Congress | Method of deacidifying paper |
US4051276A (en) * | 1974-12-24 | 1977-09-27 | The United States Government As Represented By The Librarian Of Congress | Method of deacidifying paper |
DE3913293A1 (en) * | 1988-04-26 | 1989-11-09 | Morris Jesse Warren | METHOD FOR THE PRESERVATION OF PRINTED CELLULOSE MATERIALS |
FR2665690A1 (en) * | 1990-05-08 | 1992-02-14 | Fmc Corp | PERFORATED BOOK BOX. |
US5104997A (en) * | 1988-09-30 | 1992-04-14 | Fmc Corporation | Mass treatment of cellulosic materials |
US5277842A (en) * | 1991-02-14 | 1994-01-11 | Battelle-Institut E.V. | Solvents for agents to mass deacidify books and other paper products in an environmentally safe manner |
US5433827A (en) * | 1993-12-21 | 1995-07-18 | Pulp And Paper Research Institute Of Canada | Method for the deacidification of papers and books |
FR2748282A1 (en) * | 1996-05-06 | 1997-11-07 | Lehmans Jean Pierre | Container for washing paper documents |
US6080448A (en) * | 1998-04-03 | 2000-06-27 | Preservation Technologies Lp | Deacidification of cellulose based materials using hydrofluoroether carriers |
US6214165B1 (en) | 1999-07-13 | 2001-04-10 | Joseph Zicherman | Method for deacidification of papers and books by fluidizing a bed of dry alkaline particles |
EP1273707A2 (en) * | 2001-07-04 | 2003-01-08 | Consiglio Nazionale Delle Ricerche | Method for the deacidification of paper products |
US6641877B2 (en) | 2001-03-02 | 2003-11-04 | Ronald E. Johnson | Article and method for retarding the deterioration rate of acidic paper |
US20040216642A1 (en) * | 2003-01-25 | 2004-11-04 | Farkas Barbara J. | Archival spray composition |
CN103898801A (en) * | 2014-04-22 | 2014-07-02 | 四川省档案局档案科学技术研究所 | Simple and high-efficiency paper deacidification method |
US20200157742A1 (en) * | 2017-11-28 | 2020-05-21 | South China University Of Technology | Novel device for deacidifying, reinforcing and strengthening ancient books |
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US2185954A (en) * | 1936-10-02 | 1940-01-02 | Preservators Ltd | Impregnation of paper or other materials, more especially for the protection of vegetable and animal goods during storage |
US3135627A (en) * | 1961-08-08 | 1964-06-02 | Mc Graw Edison Co | Thermally stabilized cellulose materials for electrical insulation |
US3419498A (en) * | 1966-07-13 | 1968-12-31 | Westinghouse Electric Corp | Thermally stable cellulose products |
US3472611A (en) * | 1965-08-27 | 1969-10-14 | William Herbert Langwell | Prevention of deterioration of cellulose-based records |
-
1971
- 1971-12-30 US US00214217A patent/US3771958A/en not_active Expired - Lifetime
-
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- 1973-09-26 GB GB4518873A patent/GB1422385A/en not_active Expired
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US2185954A (en) * | 1936-10-02 | 1940-01-02 | Preservators Ltd | Impregnation of paper or other materials, more especially for the protection of vegetable and animal goods during storage |
US3135627A (en) * | 1961-08-08 | 1964-06-02 | Mc Graw Edison Co | Thermally stabilized cellulose materials for electrical insulation |
US3472611A (en) * | 1965-08-27 | 1969-10-14 | William Herbert Langwell | Prevention of deterioration of cellulose-based records |
US3419498A (en) * | 1966-07-13 | 1968-12-31 | Westinghouse Electric Corp | Thermally stable cellulose products |
Cited By (25)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3969549A (en) * | 1974-12-24 | 1976-07-13 | The United States Of America As Represented By The Librarian Of Congress | Method of deacidifying paper |
US4051276A (en) * | 1974-12-24 | 1977-09-27 | The United States Government As Represented By The Librarian Of Congress | Method of deacidifying paper |
DE3913293A1 (en) * | 1988-04-26 | 1989-11-09 | Morris Jesse Warren | METHOD FOR THE PRESERVATION OF PRINTED CELLULOSE MATERIALS |
US5104997A (en) * | 1988-09-30 | 1992-04-14 | Fmc Corporation | Mass treatment of cellulosic materials |
FR2665690A1 (en) * | 1990-05-08 | 1992-02-14 | Fmc Corp | PERFORATED BOOK BOX. |
US5277842A (en) * | 1991-02-14 | 1994-01-11 | Battelle-Institut E.V. | Solvents for agents to mass deacidify books and other paper products in an environmentally safe manner |
US5433827A (en) * | 1993-12-21 | 1995-07-18 | Pulp And Paper Research Institute Of Canada | Method for the deacidification of papers and books |
FR2748282A1 (en) * | 1996-05-06 | 1997-11-07 | Lehmans Jean Pierre | Container for washing paper documents |
US6080448A (en) * | 1998-04-03 | 2000-06-27 | Preservation Technologies Lp | Deacidification of cellulose based materials using hydrofluoroether carriers |
US6342098B1 (en) | 1998-04-03 | 2002-01-29 | Preservation Technologies Lp | Deacidification of cellulose based materials using hydrofluoroether carriers |
US6214165B1 (en) | 1999-07-13 | 2001-04-10 | Joseph Zicherman | Method for deacidification of papers and books by fluidizing a bed of dry alkaline particles |
US6641877B2 (en) | 2001-03-02 | 2003-11-04 | Ronald E. Johnson | Article and method for retarding the deterioration rate of acidic paper |
EP1273707A2 (en) * | 2001-07-04 | 2003-01-08 | Consiglio Nazionale Delle Ricerche | Method for the deacidification of paper products |
EP1273707A3 (en) * | 2001-07-04 | 2004-10-13 | Consiglio Nazionale Delle Ricerche | Method for the deacidification of paper products |
US20050147827A1 (en) * | 2003-01-25 | 2005-07-07 | Farkas Barbara J. | Archival spray composition |
US6890455B2 (en) * | 2003-01-25 | 2005-05-10 | The Sherwin-Williams Company | Archival spray composition |
US20050139125A1 (en) * | 2003-01-25 | 2005-06-30 | Farkas Barbara J. | Archival spray composition |
US20050139809A1 (en) * | 2003-01-25 | 2005-06-30 | Farkas Barbara J. | Archival spray composition |
US20040216642A1 (en) * | 2003-01-25 | 2004-11-04 | Farkas Barbara J. | Archival spray composition |
US6974632B2 (en) * | 2003-01-25 | 2005-12-13 | The Sherwin-Williams Company | Archival spray composition |
US6984416B2 (en) * | 2003-01-25 | 2006-01-10 | The Sherwin-Williams Company | Archival spray composition |
US7041236B2 (en) * | 2003-01-25 | 2006-05-09 | The Sherwin-Williams Company | Archival spray composition |
CN103898801A (en) * | 2014-04-22 | 2014-07-02 | 四川省档案局档案科学技术研究所 | Simple and high-efficiency paper deacidification method |
US20200157742A1 (en) * | 2017-11-28 | 2020-05-21 | South China University Of Technology | Novel device for deacidifying, reinforcing and strengthening ancient books |
US11549218B2 (en) * | 2017-11-28 | 2023-01-10 | South China University Of Technology | Device for deacidifying, reinforcing and strengthening ancient books |
Also Published As
Publication number | Publication date |
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GB1422385A (en) | 1976-01-28 |
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