CN110318294A - Deacidification agent and preparation method thereof based on alkyl ketene dimer modified Nano magnesia - Google Patents
Deacidification agent and preparation method thereof based on alkyl ketene dimer modified Nano magnesia Download PDFInfo
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- CN110318294A CN110318294A CN201910518375.XA CN201910518375A CN110318294A CN 110318294 A CN110318294 A CN 110318294A CN 201910518375 A CN201910518375 A CN 201910518375A CN 110318294 A CN110318294 A CN 110318294A
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- nano magnesia
- ketene dimer
- modified nano
- 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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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a kind of deacidification agents and preparation method thereof based on alkyl ketene dimer modified Nano magnesia.Nano magnesia is added in the alkyl ketene dimer of melting first and is modified, the nano magnesia 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 Nano magnesia.
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, mainly paper acidification caused by.Paper
The rotten macro manifestations of 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 nano magnesia is then added into molten liquid in proportion, stirs
It mixes and has reacted separation, obtain modified Nano magnesia；Modified Nano magnesium oxide dispersion is formed by PF 5070 and petroleum ether
In the mixed solvent.
Further, the mass ratio of nano magnesia and alkyl ketene dimer is in 0.5-5:0.25-10.
Further, alkyl ketene dimer, which is heated to 110 DEG C or more, melts it completely.
Further, it is added after nano magnesia and reacts 30min or more in 95-130 DEG C of insulated and stirred, then take out while hot
Filter is then washed using 60-75 DEG C of alcoholic solvent, dries 18-36h after the completion of washing in 30-45 DEG C of environment.
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 Nano magnesia and mixed solvent is 0.02-1:100.
Further, modified Nano magnesia 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 nano magnesia, can make the reduction of its apparent activation energy, enhance the compatible of nano magnesia and organic solvent
Property, be conducive to improve dispersibility of the nano magnesia in PF 5070, prevent its aggregation.The alkane of excess molten state is used herein
Base ketene dimer can be such that nano magnesia comes into full contact with modifying agent, improve it and change in this way as dispersion and modification medium
Property rate.The polarity of PF 5070 is very low, and modified oxygen can be increased by doing solubilizer using petroleum ether similar in the polarity dissolved each other with it
Change dispersibility of the magnesium 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 nano magnesia using the transmission electron microscope photo before and after 1 method modification of the embodiment of the present invention.
Fig. 2 is paper document using the electromicroscopic photograph of deacidification agent depickling 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, melts it completely, adds 1.5g nano magnesia and herein
At a temperature of stir 30min.It filters, is washed repeatedly several times with the hot ethanol for amounting to 100mL 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 and for 24 hours, obtains modified Nano magnesia.
800g PF 5070 and 16g petroleum ether are mixed evenly, mixed solvent is obtained.By modification of the 1.5g after dry
Nano magnesia 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.
Embodiment 2
2.5g alkyl ketene dimer, which is heated to 110 DEG C, melts it completely, add 2.5g nano magnesia and
30min is stirred at a temperature of this.Filter after the reaction was completed, with amount to 120mL or so, hot ethanol that temperature is 75 DEG C several times repeatedly
Filter cake is washed, filter cake is finally placed in drying in 35 DEG C of vacuum and for 24 hours, obtains modified Nano magnesia.
1615g PF 5070 and 35g petroleum ether are mixed evenly, mixed solvent is obtained.By 2.5g changing after dry
Property nano magnesia is added in the mixed solvent, and gained mixture is transferred in homogenizer homogeneous under the conditions of 8000r/min
8min, then ultrasound 30min, as deacidification agent.
Comparative example 1
Nano oxidized magnesium dust is placed in 35 DEG C of environment and is dried in vacuo for 24 hours, then directly by nano magnesia, perfluor heptan
Alkane is mixed with the mass ratio of 1:800, and 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 magnesia, PF 5070, petroleum ether with
The mass ratio of 1:800:40 mixes.
Comparative example 3
Comparative example 3 and comparative example 1 are essentially identical, the difference is that: directly by magnesia, PF 5070, alkyl ketene
Dimer is mixed with the mass ratio of 1:800:0.2.
Paper document has been carried out at immersion depickling using deacidification agent made from embodiment 1,2 and comparative example 1-3 at room temperature
It manages (soaking time 3min), then takes out air-dried, test result is as follows shown in table 1 for depickling treated paper performance.
The different deacidification agent depickling results of property tables of table 1
To embodiment 1 before modified after nano magnesia carried out transmission electron microscope analysis, as a result as shown in Figure 1 (Zuo Weigai
Property before, the right side be it is modified).As shown in Figure 1, there is one layer of wrappage by modified Nano mgo surface, this shows to pass through modification
Alkyl ketene dimer is coated on mgo surface in the form of clad, is conducive to dispersion of the magnesia in PF 5070,
Prevent its aggregation.
Immersion depickling processing (soaking time has been carried out to paper document using deacidification agent made from embodiment 1 at room temperature
3min), air-dried microstructure change before handling by scanning electron microscope analysis paper document depickling is then taken out, as a result such as Fig. 2
Shown (left side is before depickling, the right side is after depickling).As shown in Figure 2, by depickling, treated that paper fibre surface is attached with largely
Solid particle, and the structure of solid particle and the structure of nano magnesia are almost the same, illustrate nano oxidized magnesium granules 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 can guarantee paper
The deacidification effect opened significantly can guarantee that the physical property of paper is basically unchanged again, 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 deacidification agent based on alkyl ketene dimer modified Nano magnesia, it is characterised in that including following step
Rapid: heat ketene dimer melts it completely, and nano magnesia is then added into molten liquid in proportion, is stirred to react
Complete separation obtains modified Nano magnesia；By modified Nano magnesium oxide dispersion in the mixing being made of PF 5070 and petroleum ether
In solvent.
2. preparation method as described in claim 1, it is characterised in that: the mass ratio of nano magnesia and alkyl ketene dimer
In 0.5-5:0.25-10.
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: be added after nano magnesia in 95-130 DEG C of insulated and stirred
30min or more is reacted, is then filtered while hot, is then washed using 60-75 DEG C of alcoholic solvent, in 30-45 after the completion of washing
Dry 18-36h in DEG C 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 Nano magnesia and mixed solvent is
0.02-1:100。
8. preparation method as described in claim 1, it is characterised in that: modified Nano magnesia is equal by homogeneous, ultrasonic treatment
It is even to be dispersed in the mixed solvent.
9. a kind of deacidification agent based on alkyl ketene dimer modified Nano magnesia, it is characterised in that the deacidification agent is according to right
It is required that the described in any item methods of 1-8 are prepared.
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| CN201910518375.XA CN110318294B (en) | 2019-06-15 | 2019-06-15 | Deacidification agent based on alkyl ketene dimer modified nano magnesium oxide and preparation method thereof |
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| CN201910518375.XA CN110318294B (en) | 2019-06-15 | 2019-06-15 | Deacidification agent based on alkyl ketene dimer modified nano magnesium oxide and preparation method thereof |
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| CN110318294B CN110318294B (en) | 2021-08-03 |
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Citations (4)
| 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 |
| CN106393361A (en) * | 2016-10-11 | 2017-02-15 | 阜阳市伟叶家具有限公司 | Fast growing wood modifier capable of achieving hydrophobicity synergetic enhancement through alkyl ketene dimers and nano titanium dioxide |
| 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 CN201910518375.XA patent/CN110318294B/en active Active
Patent Citations (4)
| 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 |
| CN106393361A (en) * | 2016-10-11 | 2017-02-15 | 阜阳市伟叶家具有限公司 | Fast growing wood modifier capable of achieving hydrophobicity synergetic enhancement through alkyl ketene dimers and nano titanium dioxide |
| 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 |
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