CN113322714B - Polyimide compound high-temperature aging resistant auxiliary agent, insulating paper and preparation method thereof - Google Patents
Polyimide compound high-temperature aging resistant auxiliary agent, insulating paper and preparation method thereof Download PDFInfo
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- CN113322714B CN113322714B CN202010131943.3A CN202010131943A CN113322714B CN 113322714 B CN113322714 B CN 113322714B CN 202010131943 A CN202010131943 A CN 202010131943A CN 113322714 B CN113322714 B CN 113322714B
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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
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/143—Agents preventing ageing of paper, e.g. radiation absorbing substances
-
- 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
-
- 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
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
-
- 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
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/47—Condensation polymers of aldehydes or ketones
- D21H17/49—Condensation polymers of aldehydes or ketones with compounds containing hydrogen bound to nitrogen
- D21H17/51—Triazines, e.g. melamine
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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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/55—Polyamides; Polyaminoamides; Polyester-amides
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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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/12—Coatings without pigments applied as a solution using water as the only solvent, e.g. in the presence of acid or alkaline compounds
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/24—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H19/30—Polyamides; Polyimides
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paper (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention provides a polyimide compound high-temperature aging resistant auxiliary agent, a preparation method thereof and application thereof in transformer insulating paper. According to the invention, a polyamine compound and a micromolecular amine compound are compounded to obtain a high-temperature aging resistant auxiliary agent, the high-temperature aging resistant auxiliary agent is added on insulating paper in a mode of adding, spraying, dipping or brushing, and finally drying is carried out; the insulating paper prepared by the preparation method provided by the invention has good insulating property, good high-temperature aging resistance and no pollution to transformer oil.
Description
Technical Field
The invention belongs to the field of insulating materials, and particularly relates to a polyimide compounded high-temperature aging resistant auxiliary agent, insulating paper and a preparation method thereof, and application of the insulating paper in transformer insulating paper.
Background
Pure wood pulp has better mechanical strength when used for transformer insulating paper, but after the transformer is put into operation, the insulating paper is in a higher-temperature environment, cellulose chains are gradually degraded and broken, and because the insulating paper is immersed in transformer oil, the transformer oil can decompose acid or other chemical components to damage the insulating paper at a high temperature, and the two factors greatly reduce the mechanical strength of the insulating paper.
How to improve the performance of natural fiber paper and improve the heat resistance of the natural fiber paper is continuously published by research results for many years. US 2535960 modifies natural fiber with acrylonitrile, and generates cyanoethylated fiber under the action of alkaline catalyst, thereby improving heat resistance, and the service temperature of the cyanided insulating paper can be increased by 20 ℃, but the mechanical strength of the finished paper is reduced because the hydroxyl of the fiber is reduced. US 3102159 uses melamine and dicyandiamide, JP74006766 uses melamine and polyvinylamine to increase the nitrogen content in the fiber and thus to increase the thermal stability. Such use of a nitrogen-containing compound alone to improve thermal stability is also effective, but the effect is limited. CN1176271C is compounded with nitrogenous compounds such as glucomannan and melamine, has better high-temperature resistant and aging resistant effects, but has three problems: (1) The glucomannan is prepared from natural products, and the source and the quality of raw materials are unstable; (2) NaOH is used in the preparation process of glucomannan, and sodium ions can be brought into an auxiliary agent, so that the insulating property of the auxiliary agent is influenced; (3) Glucomannan is a polysaccharide, does not contain nitrogen element, the nitrogen content of the temperature-resistant insulating paper is an important index, and the addition of glucomannan does not help to improve the nitrogen content of the paper.
Disclosure of Invention
In order to solve the technical problems, the invention uses the polyimide which has excellent reinforcing effect and higher nitrogen content to be compounded with one or more nitrogen-containing compounds on the basis of the prior art, and the compounded auxiliary agent is applied to paper in a mode of adding in pulp, spraying, dipping or brushing.
One of the purposes of the invention is to provide a polyimide compound type high-temperature aging resistant auxiliary agent, which comprises a polyamine compound and a small molecular amine compound, wherein the polyamine compound is selected from at least one of polyimide and polyacrylamide; the micromolecular amine compound is at least one selected from melamine, benzoguanamine, urea, guanamine, dicyandiamide, polyvinylamine, triethanolamine and diethanolamine;
wherein the molecular weight of the polyimide is 1000-20000, preferably 1000-5000; the molecular weight of the polyacrylamide is 10-200 ten thousand, preferably 20-50 ten thousand; the mass ratio of the polyamine compound to the small molecule amine compound is 1 (1-20), preferably 1 (1-15).
The second purpose of the invention is to provide a preparation method of the high-temperature aging resistant auxiliary agent, which comprises the steps of dispersing and uniformly mixing a polyamine compound and a small molecular amine compound through a solvent to obtain the high-temperature aging resistant auxiliary agent;
wherein the mass ratio of the polyamine compound to the small molecular amine compound is 1 (1-20), preferably 1 (1-15); the polyamine compound and the small molecular amine compound are both powder; the solvent is at least one selected from water, chloroform, m-phenol, dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP) and N, N-Dimethylacetamide (DMA); the preparation condition is that the mixture is stirred for 2 to 4 hours at the temperature of between 50 and 90 ℃.
The invention also aims to provide the high-temperature aging resistant insulating paper which contains oven-dried pulp and the high-temperature aging resistant auxiliary agent or the high-temperature aging resistant auxiliary agent obtained by the preparation method. In the high-temperature aging resistant insulating paper, the dosage of the high-temperature aging resistant auxiliary agent is 1-20% by mass of oven-dried pulp.
The fourth purpose of the invention is to provide the preparation method of the high-temperature aging resistant insulating paper, which comprises the step of adding the high-temperature aging resistant auxiliary agent onto the paper in an adding, spraying, dipping or brushing manner to obtain the high-temperature aging resistant insulating paper. The method specifically comprises the following steps:
adding the high-temperature aging resistant auxiliary agent into pure wood pulp, mixing uniformly, and then making into 40-200 g/m 2 Quantitative paper to obtain the above high temperature resistanceAging the insulating paper; or the like, or a combination thereof,
the pure wood pulp is made into 40 to 200g/m 2 Quantitative paper, fully soaking the paper in the high-temperature aging resistant auxiliary agent to obtain the high-temperature aging resistant insulating paper; or the like, or, alternatively,
the pure wood pulp is made into 40 to 200g/m 2 And (3) quantitatively adding the high-temperature aging resistant auxiliary agent to the insulating paper in a spraying or brushing manner to obtain the high-temperature aging resistant insulating paper.
The obtained high-temperature aging resistant insulating paper is finally dried at the temperature of 80-105 ℃ for 8-20 min.
The fifth purpose of the present invention is to provide transformer insulation paper, which comprises the above insulation paper or the insulation paper obtained by the above preparation method.
According to the invention, the polyimide is added into the high-temperature aging resistant auxiliary agent, is a high polymer material with flexibility, thermal stability, heat resistance and good insulating property, can play a role of a reinforcing agent and a high-temperature aging resistant role when being applied to the high-temperature resistant insulating paper, and can not influence the insulating property of the insulating paper. Meanwhile, polyimide is a nitrogen-containing high molecular compound, and can improve the nitrogen content of the temperature-resistant insulating paper compared with other nitrogen-free reinforcing agents (such as glucomannan, polyvinyl alcohol and the like).
The high-temperature-resistant aging auxiliary agent in the high-temperature-resistant aging insulation paper provided by the invention is added according to 1-20% of oven-dried pulp, so that the nitrogen content in the insulation paper is kept at 1.6-4.2%, the nitrogen content is too low, the thermal stability is low, the nitrogen content is higher than 4.2%, the thermal stability is not further improved, and the thermal stability is reduced along with the further increase of the nitrogen content.
Compared with the prior art, the invention has the advantages that:
1. the polyimide added in the invention has very good flexibility and thermal stability, and can play a role of a reinforcing agent, so that the high-temperature aging resistant auxiliary agent has very good insulation performance and also has very good high-temperature aging resistance;
2. the nitrogen content is an important index of the temperature-resistant insulating paper, the polyimide is a nitrogen-containing compound, and the nitrogen content index of the temperature-resistant insulating paper can be effectively increased by introducing the polyimide into the high-temperature aging-resistant auxiliary agent;
3. the preparation method has the advantages of easily obtained raw materials, easy process, low energy consumption and good repeatability;
4. the high-temperature aging resistant insulating paper prepared by the invention has excellent high-temperature aging resistance, does not pollute transformer oil, and does not influence the insulating property.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The test instruments and test conditions used in the examples were as follows:
high temperature aging resistance experiment: placing the manufactured insulating paper in a vacuum tube, inserting a copper sheet into the vacuum tube to accelerate aging, sealing the vacuum tube, heating to 105 ℃, vacuum-drying for 5 hours to drain water, sucking 25# transformer oil into the vacuum tube until the insulating paper is completely covered, heating to 150 ℃, and testing the mechanical property and the nitrogen content after carrying out constant-temperature and constant-humidity treatment on the obtained insulating paper for 24 hours through a 7-day aging experiment.
The tensile strength before and after aging is measured according to the national standard GB/T453-2002, and the test instrument is a tensile strength tester.
The nitrogen content is measured according to the general rule of JY/T017-1996 elemental analyzer method, and the instrument is an elemental analyzer.
The sources of the compounds employed in the examples are as follows:
polyimide (I): mitsubishi chemical of Japan
Melamine: yulong chemical industry
Polyacrylamide: chemical science of cologne
Dicyandiamide: chemical science of cologne
Urea: chemical science of cologne
DMSO, DMSO: chemical science of cologne
Chloroform: chemical science of cologne
Example 1
The polyimide, the melamine and the polyacrylamide are dissolved and dispersed by stirring with water at 90 ℃ for 2h according to the weight ratio of 1.1 to 2, 20 percent of absolute dry pulp is added into the beaten pure wood pulp and uniformly mixed, and the mixture is beaten into 60g/m by a paper sample beater to be stirred into 60g/m 2 And (3) drying the quantified paper for 10min at 105 ℃ to obtain the high-temperature aging resistant insulating paper. The nitrogen content in the alloy is tested by element analysis, and the mechanical properties are shown in Table 1 after aging test.
Example 2
The pure wood pulp is made into 60g/m by a paper pattern making device 2 The paper, which was quantified, was pre-dried to 80% moisture. Polyimide, urea and melamine are dissolved and dispersed by DMSO at 90 ℃ for 2h according to the weight ratio of 1. The nitrogen content in the alloy is tested by element analysis, and the mechanical properties are shown in Table 1 after aging test.
Example 3:
according to the example 2, polyimide, dicyandiamide and melamine are dissolved and dispersed by stirring with chloroform at 90 ℃ for 2h according to the weight ratio of 1. The nitrogen content in the alloy is tested by element analysis, and the mechanical properties are shown in table 1 after aging test.
Examples 4 to 6:
according to the embodiment 3, the weight ratio of the polyimide to the dicyandiamide to the melamine in the compound auxiliary agent is adjusted to be 1.
Comparative example 1
The beaten pure wood pulp is made into 60g/m by a paper sample making device 2 The amount of the paper to be used is determined,after drying at 105 ℃ a comparative sample 1 was obtained. The mechanical properties measured by the aging test are shown in Table 1.
Comparative example 2
Dissolving melamine and polyacrylamide in water according to the weight ratio of 20 2 Quantitative paper, dried at 105 ℃ to obtain comparative sample 2. The nitrogen content in the alloy is tested by element analysis, and the mechanical properties are shown in Table 1 after aging test.
Comparative example 3
The pure wood pulp is made into 60g/m by a paper pattern making device 2 The paper was then pre-dried to 80% moisture. Urea and melamine were dissolved and dispersed in DMSO at a weight ratio of 1. The nitrogen content in the alloy is tested by element analysis, and the mechanical properties are shown in Table 1 after aging test.
Comparative example 4
The pure wood pulp is made into 60g/m by a paper pattern making device 2 Quantitative paper is pre-dried to contain 80% of moisture, dicyandiamide and melamine are dissolved and dispersed by chloroform according to the weight ratio of 1. The nitrogen content in the alloy is tested by element analysis, and the mechanical properties are shown in Table 1 after aging test.
TABLE 1 high temperature aging test data of examples 1 to 3 and comparative examples 1 to 4
Note retention = post/pre aging, reflecting post aging mechanical strength retention
As can be seen from Table 1, the high temperature aging resistance of the insulation paper is obviously improved after the high temperature aging resistance auxiliary agent of the invention is added, and the high temperature aging resistance of the insulation paper can be obviously improved by introducing the polyimide into the high temperature aging resistance auxiliary agent in comparison with the comparative examples 2 to 4 without adding the polyimide in the examples 1 to 3 with the polyimide.
TABLE 2 data of high temperature aging resistance test for the insulation papers of examples 4-6 with different nitrogen contents
Note retention = post/pre aging, reflecting post aging mechanical strength retention
As can be seen from table 2, the aging resistance of the insulating paper showed an increase and then a decrease as the nitrogen content increased.
Claims (12)
1. The application of the polyimide compounded high-temperature aging resistant auxiliary agent in the high-temperature aging resistant insulating paper comprises a polyamine compound and a micromolecular amine compound, wherein the polyamine compound is polyimide; the small molecular amine compound is at least one selected from melamine, benzoguanamine, urea, guanamine, dicyandiamide, polyvinylamine, triethanolamine and diethanolamine, the mass ratio of the polyamine compound to the small molecular amine compound is 1 (1-20), and the polyimide compounded high-temperature aging resistant auxiliary agent keeps the nitrogen content in the insulating paper at 1.6-4.2%.
2. Use according to claim 1,
the molecular weight of the polyimide is 1000-20000; and/or the presence of a gas in the gas,
the mass ratio of the polyamine compound to the small molecular amine compound is 1 (1 to 15).
3. The use according to claim 2,
the molecular weight of the polyimide is 1000 to 5000.
4. The application of the high-temperature aging resistant auxiliary agent as claimed in claim 1 or 2, wherein the preparation method of the high-temperature aging resistant auxiliary agent comprises the step of uniformly dispersing and mixing the polyamine compound and the small molecule amine compound through a solvent to obtain the high-temperature aging resistant auxiliary agent.
5. The use according to claim 4,
the polyamine compound and the micromolecular amine compound are powdery; and/or the presence of a gas in the gas,
the solvent is at least one selected from water, chloroform, m-phenol, dimethyl sulfoxide, N-methylpyrrolidone and N, N-dimethylacetamide; and/or the presence of a gas in the gas,
the preparation condition is that the mixture is stirred for 2 to 4 hours at the temperature of between 50 and 90 ℃.
6. The use according to claim 5,
the mass ratio of the polyamine compound to the small molecular amine compound is 1 (1 to 15).
7. The high-temperature aging resistant insulating paper contains oven-dried pulp and a polyimide compounded high-temperature aging resistant auxiliary agent, wherein the polyimide compounded high-temperature aging resistant auxiliary agent comprises a polyamine compound and a micromolecular amine compound, and the polyamine compound is polyimide; the small molecular amine compound is at least one selected from melamine, benzoguanamine, urea, guanamine, dicyandiamide, polyvinylamine, triethanolamine and diethanolamine, the mass ratio of the polyamine compound to the small molecular amine compound is 1 (1-20), and the polyimide compounded high-temperature aging resistant auxiliary agent keeps the nitrogen content in the insulating paper at 1.6-4.2%.
8. The insulation paper according to claim 7, wherein the amount of the high-temperature aging resistant auxiliary is 1 to 20% by mass of oven-dried pulp.
9. The method for preparing the high-temperature aging resistant insulating paper according to claim 7 or 8, comprising the step of adding the high-temperature aging resistant auxiliary agent to the insulating paper in a manner of adding, spraying, dipping or brushing to obtain the high-temperature aging resistant insulating paper.
10. The method according to claim 9, comprising the steps of:
adding the high-temperature aging resistant auxiliary agent into the pure wood pulp, mixing uniformly, and then making into 40-200 g/m 2 Quantitative paper is used for obtaining the high-temperature aging resistant insulating paper; or the like, or a combination thereof,
making the pure wood pulp into 40 to 200g/m 2 Quantitative paper, fully soaking the paper in the high-temperature aging resistant auxiliary agent to obtain the high-temperature aging resistant insulating paper; or the like, or, alternatively,
making the pure wood pulp into 40 to 200g/m 2 And (3) quantitative paper, wherein the high-temperature aging resistant auxiliary agent is added on the insulating paper in a spraying or brushing manner to obtain the high-temperature aging resistant insulating paper.
11. The preparation method of claim 9 or 10, wherein the high temperature aging resistant insulating paper is finally dried at a temperature of 80-105 ℃ for 8-20 min.
12. A transformer insulating paper, comprising the high-temperature aging resistant insulating paper of claim 7 or 8 or the high-temperature aging resistant insulating paper obtained by the preparation method of any one of claims 9 to 11.
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| CN202010131943.3A CN113322714B (en) | 2020-02-28 | 2020-02-28 | Polyimide compound high-temperature aging resistant auxiliary agent, insulating paper and preparation method thereof |
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| CN113322714B true CN113322714B (en) | 2022-12-02 |
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