CN110318296A - Paper sheet deacidification agent and preparation method thereof based on alkyl ketene dimer modified magnesium hydroxide - Google Patents
Paper sheet deacidification agent and preparation method thereof based on alkyl ketene dimer modified magnesium hydroxide Download PDFInfo
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- CN110318296A CN110318296A CN201910518397.6A CN201910518397A CN110318296A CN 110318296 A CN110318296 A CN 110318296A CN 201910518397 A CN201910518397 A CN 201910518397A CN 110318296 A CN110318296 A CN 110318296A
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- magnesium hydroxide
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- ketene dimer
- modified magnesium
- alkyl ketene
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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 present invention relates to a kind of deacidification agent and preparation method thereof based on alkyl ketene dimer modified magnesium hydroxide.Magnesium hydroxide is added in the alkyl ketene dimer of melting first and is modified, the magnesium hydroxide being modified then is dispersed in PF 5070, petroleum ether in the mixed solvent, obtains target deacidification agent.The deacidification agent raw material are easy to get, and reaction condition is mild, and method of preparation and use is simple and convenient, and dosage is few, high-efficient, and deacidification effect is good and uniform.
Description
Technical field
The present invention relates to book and file processing and Chemical composition that technical fields, and in particular to one kind is based on alkyl ketene two
The paper sheet deacidification agent and preparation method thereof of aggressiveness modified magnesium hydroxide.
Background technique
Currently, in store ten hundreds of preciousnesses, successive dynasties remnants in various libraries, China, museum, archival agency
The cultural heritages such as books, calligraphy and painting, newspaper, archives, wherein mostly being write and being printed by hand-made paper or mechanical paper wood matter.With
The passage in years, paper document can gradually appear jaundice mildew, dusting fragmentation phenomena such as, this be mainly paper acidification caused by.
The rotten macro manifestations of paper material be discoloration, it is microcosmic on be structure broken ring (mechanical strength decline).
Cellulose is the main component of paper, quite stable under neutral and weak basic condition, be not only difficult to hydrolyze and
It aoxidizes, and its hydrolysis rate increases according to a certain percentage with hydrogen ion concentration increase, i.e. the stronger cellulose of pH value more low in acidity
Hydrolysis rate it is faster.The degree of polymerization reduces after cellulose hydrolysis, causes the intensity of paper material to decrease, finally shows
The result is that paper go bad embrittlement.
There is much sour source in paper, including substances, industrial development such as the sulphite, the alum that add in paper-making process
Lead to the brings acidic materials such as the sour gas gradually increased and external microbe, mould.The acidity of these different approaches
Substance is all the rotten reason of paper document acidification.
The paper document deacidification technique being widely used at present specifically includes that solwution method and vapor phase method, and wherein vapor phase method exists
Technique is more complex, need vacuum cooperation, long processing period, equipment costly the deficiencies of；Solwution method is divided into aqueous systems and organic again
Two kinds of system, deacidification agent used in aqueous systems solwution method will lead to paper curl, adhesion, colour fading etc..Therefore using organic molten
Liquid in terms of papery depickling advantageously.Deacidification agent used in this method generally includes metal oxide or hydroxide (such as
Magnesia, magnesium hydroxide, calcium oxide, calcium hydroxide etc.) and organic solvent (fluoric ether).But due to the polarity of fluoric ether
It is very small, it is very poor in dispersibility wherein to lead to the substances such as magnesium hydroxide, magnesia, so improving depickling substance in organic solvent
In dispersibility be improve deacidification agent efficiency key factor.
Summary of the invention
It is above-mentioned various existing for existing paper sheet deacidification agent it is an object of the invention to overcome the problems, such as, a kind of preparation process is provided
Simply, deacidification agent easy to use, effect is good, preparation method are as follows:
Heat ketene dimer melts it completely, and magnesium hydroxide is then added into molten liquid in proportion, stirring
It is molten to be dispersed in the mixing being made of PF 5070 and petroleum ether by isolated modified magnesium hydroxide after reaction for modified magnesium hydroxide
In agent.
Further, the mass ratio of magnesium hydroxide and alkyl ketene dimer is 0.5-5:1-10.
Further, alkyl ketene dimer, which is heated to 110 DEG C or more, melts it completely.
Further, it is added after magnesium hydroxide and reacts 30min or more in 95-130 DEG C of insulated and stirred, then filter while hot,
Then it is washed using 60-75 DEG C of alcoholic solvent, dries 18-36h after the completion of washing in 30-45 DEG C of environment, be modified
Magnesium hydroxide.
Further, the alcoholic solvent is specially dehydrated alcohol.
Further, the mass ratio of in the mixed solvent PF 5070 and petroleum ether is 1530-1615:32-66.
Further, the mass ratio of modified magnesium hydroxide and mixed solvent is 0.05-1:100.
Further, modified magnesium hydroxide is dispersed in the mixed solvent by homogeneous, ultrasonic treatment.
Another object of the present invention is to provide the deacidification agents that one kind is prepared according to the method described above.
Alkyl ketene dimer is a kind of sizing agent, itself may be used for the reparation of paper.With alkyl ketene dimerization
Body is modified magnesium hydroxide, and the apparent activation energy of magnesium hydroxide can be made to reduce, and enhances magnesium hydroxide and organic solvent
Compatibility is conducive to improve dispersion of the magnesium hydroxide in PF 5070.The application uses the alkyl ketene two of excess molten state
Aggressiveness can be such that magnesium hydroxide comes into full contact with modifying agent in this way as decentralized medium, improve the degree of modification of magnesium hydroxide.Perfluor
The polarity of heptane is very low, does solubilizer using petroleum ether similar in the polarity dissolved each other with it, can increase modified magnesium hydroxide and exist
Dispersibility in PF 5070.
Compared with prior art, the invention has the following advantages: raw material are easy to get, reaction condition is mild, preparation and
Application method is simple and convenient, avoids using complicated, expensive vacuum equipment, has advantageously reduced cost；Using compound organic
Dicyandiamide solution reduces adverse effect of the deacidification to paper；Deacidification agent dosage is few, high-efficient, and deacidification effect is good and uniform.
Detailed description of the invention
Fig. 1 is that magnesium hydroxide uses the transmission electron microscope photo of 1 method of modifying of the embodiment of the present invention before and after the processing.
Fig. 2 is paper document using the electromicroscopic photograph of deacidification agent before and after the processing made from the embodiment of the present invention 1.
Specific embodiment
To make those of ordinary skill in the art fully understand technical solution of the present invention and beneficial effect, below in conjunction with specific
Embodiment is further described.
Embodiment 1
2g alkyl ketene dimer, which is heated to 110 DEG C or so, melts it completely, adds 2g magnesium hydroxide and herein
At a temperature of stir 30min.It filters while hot after the reaction was completed, it is anti-several times with the hot ethanol for amounting to 100mL or so, temperature is 75 DEG C
Filter cake is washed in after backwashing, and filter cake is finally placed in drying in 35 DEG C of vacuum environment and for 24 hours, obtains modified magnesium hydroxide.
1600g PF 5070 and 32g petroleum ether are mixed evenly, mixed solvent is obtained.By modification of the 2g after dry
Magnesium hydroxide is added in the mixed solvent, and gained mixture is transferred in homogenizer homogeneous 8min under the conditions of 8000r/min, so
Ultrasound 30min, as deacidification agent afterwards.
Embodiment 2
1.6g alkyl ketene dimer, which is heated to 110 DEG C, melts it completely, adds 1.6g magnesium hydroxide and herein
At a temperature of stir 30min.It filters, is washed repeatedly several times with the hot ethanol for amounting to 50mL or so, temperature is 75 DEG C after the reaction was completed
Filter cake is washed, filter cake is finally placed in drying in 35 DEG C of vacuum environment and for 24 hours, obtains modified magnesium hydroxide.
1615g PF 5070 and 38g petroleum ether are mixed evenly, mixed solvent is obtained.By 1.5g changing after dry
Property magnesium hydroxide is added in the mixed solvent, and gained mixture is transferred in homogenizer homogeneous 8min under the conditions of 8000r/min,
Then ultrasound 30min, as deacidification agent.
Comparative example 1
Magnesium hydroxide powder is placed in 35 DEG C of environment and is dried in vacuo for 24 hours, then directly by magnesium hydroxide and PF 5070
It is mixed with the ratio of 1:800, gained mixture is transferred in homogenizer homogeneous 8min under the conditions of 8000r/min, then ultrasonic
30min, as deacidification agent.
Comparative example 2
Comparative example 2 and comparative example 1 are essentially identical, the difference is that: directly by magnesium hydroxide, PF 5070, petroleum ether
Three is mixed with the ratio of 1:800:40.
Comparative example 3
Comparative example 3 and comparative example 1 are essentially identical, the difference is that: directly by magnesium hydroxide, PF 5070, alkyl alkene
Ketone dimer three is mixed with the ratio of 1:800:0.2.
Immersion depickling has been carried out to paper document using deacidification agent made from embodiment 1,2 and comparative example 1-3 at room temperature
It handles (soaking time 3min), then takes out air-dried, depickling treated paper performance test is as shown in table 1 below.
The different deacidification agent deacidification effect tables of table 1
To embodiment 1 before modified after magnesium hydroxide carried out transmission electron microscope analysis, as a result as shown in Figure 1 (left side for be modified
Before, the right side is modified).As shown in Figure 1, there is one layer of wrappage by modified magnesium hydroxide surface, this shows to pass through modified alkyl
Ketene dimer is coated on magnesium hydroxide surface in the form of clad, is conducive to dispersion of the magnesium hydroxide in PF 5070.
Immersion depickling processing (soaking time has been carried out to paper document using deacidification agent made from embodiment 1 at room temperature
3min), then take out it is air-dried, by the microstructure change of scanning electron microscope analysis paper document depickling before and after the processing, as a result such as
(left side is before depickling, the right side is after depickling) shown in Fig. 2.As shown in Figure 2, by depickling, treated that paper fibre surface is attached with greatly
The solid particle of amount, and the structure of solid particle and the structure of nano magnesia are almost the same, explanation is magnesium oxide particle attachment
The effect of depickling is played on paper fibre surface.
After the same method, influence of the soaking time to deacidification effect is had studied using deacidification agent made from embodiment 1,
The results are shown in Table 2.
Influence result table of 2 soaking time of table to deacidification effect
Above the results showed that soaking time is too short (1min or less), deacidification agent is less in paper surface adhesion amount, right
The processing of paper acidity is unobvious；Long soaking time (5min or more), pH value do not increase significantly, and macroscopically it is observed that
There is apparent white accumulation in paper surface, this will affect the Fundamental Physical Properties of paper.Soaking time is moderate both to can guarantee paper
The deacidification effect opened is significant, and can guarantee that the physical property of paper is basically unchanged, microcosmic upper deacidification agent adhesion amount foot on paper
Enough, macroscopically paper surface is without apparent white accumulation, therefore controlling soaking time is 1-5min.The experiment also illustrates, perfluor
Heptane-petroleum ether composite solvent system short time immersion treatment influences the basic performances such as the brittleness of paper little.
Similar effect can also be obtained by carrying out above-mentioned experiment using deacidification agent made from embodiment 2.
Claims (9)
1. the preparation method of the paper sheet deacidification agent based on alkyl ketene dimer modified magnesium hydroxide, it is characterised in that including following
Step: heat ketene dimer melts it completely, and magnesium hydroxide is then added into molten liquid in proportion, is stirred to react
Modified magnesium hydroxide is dispersed in the in the mixed solvent being made of PF 5070 and petroleum ether by isolated modified magnesium hydroxide afterwards
?.
2. preparation method as described in claim 1, it is characterised in that: the mass ratio of magnesium hydroxide and alkyl ketene dimer is
0.5-5:1-10。
3. preparation method as described in claim 1, it is characterised in that: alkyl ketene dimer, which is heated to 110 DEG C or more, makes it
Melting completely.
4. preparation method as described in claim 1, it is characterised in that: anti-in 95-130 DEG C of insulated and stirred after addition magnesium hydroxide
30min or more is answered, is then filtered while hot, is then washed using 60-75 DEG C of alcoholic solvent, at 30-45 DEG C after the completion of washing
Dry 18-36h, obtains modified magnesium hydroxide in environment.
5. preparation method as claimed in claim 4, it is characterised in that: the alcoholic solvent is specially dehydrated alcohol.
6. preparation method as described in claim 1, it is characterised in that: the mass ratio of in the mixed solvent PF 5070 and petroleum ether
For 1530-1615:32-66.
7. preparation method as described in claim 1, it is characterised in that: the mass ratio of modified magnesium hydroxide and mixed solvent is
0.05-1:100。
8. preparation method as described in claim 1, it is characterised in that: modified magnesium hydroxide is uniform by homogeneous, ultrasonic treatment
It is dispersed in the mixed solvent.
9. a kind of paper sheet deacidification agent based on alkyl ketene dimer modified magnesium hydroxide, it is characterised in that the deacidification agent is according to power
Benefit requires any method of 1-8 to be prepared.
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| CN201910518397.6A CN110318296B (en) | 2019-06-15 | 2019-06-15 | Paper deacidification agent based on alkyl ketene dimer modified magnesium hydroxide and preparation method thereof |
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| CN110318296B CN110318296B (en) | 2021-08-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115874485A (en) * | 2021-09-28 | 2023-03-31 | 华南理工大学 | Organic phase deacidification enhancement repair liquid and preparation method and application thereof |
| CN116676807A (en) * | 2023-05-17 | 2023-09-01 | 中国人民大学 | Paper deacidification dispersion liquid and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088870A (en) * | 2015-07-15 | 2015-11-25 | 国家图书馆 | Paper deacidification agent, and paper deacidification system and method thereof |
| CN105862513A (en) * | 2016-04-22 | 2016-08-17 | 国家图书馆 | Paper deacidifying solution and preparation method thereof |
| CN107012736A (en) * | 2017-05-03 | 2017-08-04 | 清华大学 | A kind of depickling liquid for having strengthening for paper effect concurrently and preparation method thereof |
-
2019
- 2019-06-15 CN CN201910518397.6A patent/CN110318296B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088870A (en) * | 2015-07-15 | 2015-11-25 | 国家图书馆 | Paper deacidification agent, and paper deacidification system and method thereof |
| CN105862513A (en) * | 2016-04-22 | 2016-08-17 | 国家图书馆 | Paper deacidifying solution and preparation method thereof |
| CN107012736A (en) * | 2017-05-03 | 2017-08-04 | 清华大学 | A kind of depickling liquid for having strengthening for paper effect concurrently and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115874485A (en) * | 2021-09-28 | 2023-03-31 | 华南理工大学 | Organic phase deacidification enhancement repair liquid and preparation method and application thereof |
| CN115874485B (en) * | 2021-09-28 | 2024-04-26 | 华南理工大学 | Organic phase deacidification enhancement repair liquid and preparation method and application thereof |
| CN116676807A (en) * | 2023-05-17 | 2023-09-01 | 中国人民大学 | Paper deacidification dispersion liquid and preparation method and application thereof |
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