CN103437247A - Preparation method of paper with antibacterial effect - Google Patents
Preparation method of paper with antibacterial effect Download PDFInfo
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- CN103437247A CN103437247A CN2013103728232A CN201310372823A CN103437247A CN 103437247 A CN103437247 A CN 103437247A CN 2013103728232 A CN2013103728232 A CN 2013103728232A CN 201310372823 A CN201310372823 A CN 201310372823A CN 103437247 A CN103437247 A CN 103437247A
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Abstract
The invention discloses a preparation method of paper with an antibacterial effect. The preparation method comprises the following steps: grafting cyclodextrin to papermaking cationic starch by an epoxy crosslinking agent; enveloping antibacterial agents by means of lyophobic cavities of cyclodextrin on the cationic starch; and adding the antibacterial agents to paper by way of internal addition, so as to improve the strength performance of paper while paper is endowed with good antibacterial performance. According to the preparation method provided by the invention, the antibacterial agents are embedded by cyclodextrin, so that antibacterial functional paper products with slow release performance can be prepared. The retention rate of the antibacterial agents on fibers is improved by means of efficient retention rate of cationic starch on fibers, so that the antibacterial effect of paper is enhanced, and the preparation method has the advantages of simplicity in production process, low equipment investment and strong adaptability.
Description
Technical field
The present invention relates to field of papermaking, particularly a kind of preparation method with paper of antibacterial effect.
Background technology
Along with growth in the living standard, people more focus on the health of self and the safety of surrounding enviroment, wish to have anti-microbial property with live closely-related various material and goods thereof of people.Paper is requisite articles for daily use during people live, and research and development antibacterial functions paper has great importance, especially for the paper of the field of circulation, as books, playing card, medical record paper, menu, bank-note paper etc.These paper or paper products frequent exchange, easily bring the chance of spread of germs or cross infection.In addition, anti-bacteria paper all has wide practical use at food wrapper, medicinal paper, the aspects such as indoor environment protection paper using, historical relic's protection paper using and paper for daily use.Therefore, the exploitation of antibacterial functions paper, improves the aspect such as people's quality of life and has important Social benefit and economic benefit for improving the papermaking product class with application.
At present, in life, most anti-bacteria paper is in paper production, and antibacterials make in modes such as additive processs in sprinkling, top sizing, coating, dipping, slurry, makes it obtain antibiotic property.Chinese patent CN1472388 discloses the preparation method of the special-purpose anti-bacteria paper of a kind of bank note, and hydroxyl-2,4 bromo-1,5 glutaraldehyde antiseptic is added in paper and prepares the special-purpose anti-bacteria paper of bank note by coating, glue spraying, impregnating method.Japan Patent JP11178899 adopts the coating processing method to make a kind of anti-bacteria paper, then binds and make antibiotic packaging material with resin film or aluminium foil, and not only anti-microbial property is good, and very attractive in appearance.Chinese patent CN102031722A discloses a kind of preparation method of anti-bacteria paper, to be starched interior the mixing with slurry with respect to the load zeolite of oven dry stock quality 2.5～10%, 3.3～10% the load zeolite that maybe will be equivalent to pigment mass is mixed together to prepare anti-bacteria paper with the pigment of coating use.Although these modes of production have been given the paper anti-microbial property, all exist certain limitation.Anti-bacteria paper prepared by spray method exists antiseptic shortcoming pockety; It is consuming time oversize that infusion process prepares anti-bacteria paper, is not suitable for the production of large high-speed paper machine; The antibacterial effect of anti-bacteria paper prepared by top sizing and rubbing method can lose efficacy gradually with the variation of resting period, humidity in deep-processing process; Although it is simple to operate that the interior additive process of slurry prepares anti-bacteria paper, but because the molecular weight of antibacterials is generally less, be easy to plain boiled water, run off in upper network process, cause the antibacterials consumption excessive, and be retained in antimicrobial component in paper seldom, both increase cost, do not reached again good antibacterial effect.
Summary of the invention
Above-mentioned shortcoming and deficiency in order to overcome prior art, the object of the present invention is to provide a kind of preparation method with paper of good antibacterial effect, improved the long acting antibiotic of paper.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method with paper of antibacterial effect comprises the following steps:
(1) under room temperature, cyclodextrin is joined in the sodium hydroxide solution that concentration is 100～600g/L, then slowly add the epoxies crosslinking agent, stir 10～30min under 30～80 ℃, then add the cationic starch after gelatinization, continue to stir 1～4h, regulate pH to neutral with hydrochloric acid solution, add organic solvent, centrifugation, obtain the grafted cyclodextrin cationic starch after freeze drying;
Wherein, the mass ratio of described cyclodextrin and sodium hydroxide solution is 1:4～1:8; The mol ratio of described epoxies crosslinking agent and cyclodextrin is 2:1～10:1; Described cationic starch after gelatinization and the mass ratio of cyclodextrin are 1:2～1:6;
(2) the grafted cyclodextrin cationic starch prepared by step (1) is placed in mortar, add the deionized water of 2～5 times of weight to grind well, fully grind again 15～30min after adding antibacterials, be placed in again the dry 3～6h of 40～60 ℃ of air dry ovens, and then with the deionized water washing, obtain the grafted cyclodextrin cationic starch of inclusion antibacterials after freeze drying; The addition of described antibacterials is 10%～40% of grafted cyclodextrin cationic starch quality;
(3) the grafted cyclodextrin cationic starch of the inclusion antibacterials that prepared by step (2) joins in fibrous suspension, the paper of manufacturing paper with pulp; 0.1%～2% of the over dry stock quality that the addition of the grafted cyclodextrin cationic starch of described inclusion antibacterials is fibrous suspension.
Described epoxies crosslinking agent is a kind of in epoxychloropropane, ethylene glycol diglycidylether or bisphenol A diglycidyl ether.
Described cationic starch is a kind of in cornstarch or farina, and substitution value is 0.01～0.07.
Described cyclodextrin is beta-schardinger dextrin-.
Described antibacterials are a kind of in Ciprofloxacin Hydrochloride, lavo-ofloxacin hydrochloride or retens.
The described organic solvent of step (1) is a kind of in ethanol, methyl alcohol or acetone.
Step (1) is centrifugal, is specially:
The centrifugation rotating speed is 3000～5000r/min, and centrifugation time is 15～30min.
Compared with prior art, the present invention has the following advantages and effect:
(1) the present invention is grafted to cyclodextrin on cationic starch, utilizes and is grafted to the cyclodextrin encapsulated antibacterials on cationic starch, realizes the shielding action to antibacterials, controls the release of medicine, further brings into play its drug effect, reduces side effect.
(2) the present invention utilizes cationic starch efficient retention in paper, has overcome addition manner in traditional slurry and has prepared the antibacterials losing issue that anti-bacteria paper exists, thereby effectively reduced production costs.
(3) the grafted cyclodextrin cationic starch of inclusion antibacterials of the present invention is added in paper making wet part as auxiliary agent, improves the strength character of page when giving the good anti-microbial property of paper; .
(4) preparation method of the present invention is simple to operate, with low cost.
The accompanying drawing explanation
TG figure before and after the cationic starch grafted cyclodextrin that Fig. 1 is embodiment 2.
Fig. 2 is the SEM figure that does not add the grafted cyclodextrin cationic starch paper of inclusion antibacterials in embodiment 5.
The SEM figure of the paper that the grafted cyclodextrin cationic starch addition that Fig. 3 is inclusion antibacterials in embodiment 5 is needle-leaved wood fibre suspension over dry stock quality 2%.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) under room temperature, the 5g beta-schardinger dextrin-joins in the sodium hydroxide solution that 25ml concentration is 300g/L, slowly add 1ml epoxychloropropane solution, stir 20min under 50 ℃, the substitution value that then adds the 2.5g gelatinization is 0.021 cationic starch, continues to stir 2h, solution neutralizes and is neutral with the hydrochloric acid solution of 1.5mol/L, add the 50ml ethanolic solution, centrifugation 15min under 5000r/min, freeze drying 12h obtains the grafted cyclodextrin cationic starch
(2) grafted cyclodextrin cationic starch 2g made is placed in mortar, add the 4g deionized water to grind well, fully grind again 20min after adding the 200mg Ciprofloxacin Hydrochloride, be placed in 40 ℃ of dry 4h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion Ciprofloxacin Hydrochloride;
(3) will join in the broad-leaved wood fiber suspension that mass fraction is 0.5% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion Ciprofloxacin Hydrochloride of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
The cationic starch of the present embodiment is cornstarch.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
Embodiment 2
(1) under room temperature, the 6g beta-schardinger dextrin-joins in the sodium hydroxide solution that 25ml concentration is 400g/L, slowly add 2.42ml epoxychloropropane solution, stir 30min under 60 ℃, then adding the substitution value of 2.5g after gelatinization is 0.033 cationic starch, continues to stir 3h, solution neutralizes and is neutral with the hydrochloric acid solution of 1mol/L, add the 50ml ethanolic solution, centrifugation 20min under 4000r/min, freeze drying 12h obtains the grafted cyclodextrin cationic starch;
(2) grafted cyclodextrin cationic starch 2g made is placed in mortar, add 6g water to grind well, fully grind again 20min after adding the 300mg lavo-ofloxacin hydrochloride, be placed in 50 ℃ of dry 3h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion lavo-ofloxacin hydrochloride;
(3) will join in the needle-leaved wood fibre suspension that mass fraction is 0.3% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion lavo-ofloxacin hydrochloride of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
TG figure before and after cationic starch grafted cyclodextrin that Fig. 1 is the present embodiment, as seen from Figure 1, the grafted cyclodextrin cationic starch has good heat endurance, and below 200 ℃ the time, the weightlessness of polymer is very little.Initial decomposition temperature is 224.9 ℃, and maximum decomposition temperature is 246.6 ℃.
The cationic starch of the present embodiment is farina.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
Embodiment 3
(1) under room temperature, 7.5g beta-schardinger dextrin-joins in the sodium hydroxide solution that 25ml concentration is 400g/L, slowly add 2.42ml epoxychloropropane solution, stir 20min under 60 ℃, then adding the substitution value of 2.5g after gelatinization is 0.043 cationic starch, continues to stir 4h, solution neutralizes and is neutral with the hydrochloric acid solution of 1.5mol/L, add the 50ml acetone soln, centrifugation 30min under 5000r/min, freeze drying 12h obtains the grafted cyclodextrin cationic starch;
(2) grafted cyclodextrin cationic starch 2g made is placed in mortar, add 8g water to grind well, fully grind again 20min after adding the 400mg retens, be placed in 40 ℃ of dry 4h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion retens;
(3) will join in the bamboo pulp fiber suspension that mass fraction is 0.4% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion retens of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
The cationic starch of the present embodiment is cornstarch.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
Embodiment 4
(1) under room temperature, the 5g beta-schardinger dextrin-joins in the sodium hydroxide solution that 25ml concentration is 200g/L, slowly add 1.8ml ethylene glycol diglycidylether solution, stir 15min under 40 ℃, then adding the substitution value of 2.5g after gelatinization is 0.043 cationic starch, continues to stir 3h, solution neutralizes and is neutral with the hydrochloric acid solution of 1.5mol/L, add 50ml ethanol, centrifugation 20min under 4000r/min, freeze drying 12h obtains the grafted cyclodextrin cationic starch;
(2) grafted cyclodextrin cationic starch 2g made is placed in mortar, add 4g water to grind well, fully grind again 20min after adding the 200mg Ciprofloxacin Hydrochloride, be placed in 40 ℃ of dry 5h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion Ciprofloxacin Hydrochloride;
(3) will join in the broad-leaved wood fiber suspension that mass fraction is 0.5% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion Ciprofloxacin Hydrochloride of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
The cationic starch of the present embodiment is cornstarch.
Embodiment 5
(1) under room temperature, the 6g beta-schardinger dextrin-joins in the sodium hydroxide solution that 25ml concentration is 300g/L, slowly add the 2.5ml ethylene glycol diglycidylether, stir 15min under 50 ℃, then adding the substitution value of 2.5g after gelatinization is 0.033 cationic starch, continues to stir 2h, neutralize and be neutral with the hydrochloric acid solution of 1mol/L, add the 50ml methanol solution, centrifugation 15min under 5000r/min, freeze drying 12h obtains the grafted cyclodextrin cationic starch;
(2) grafted cyclodextrin cationic starch 2g made is placed in mortar, add 6g water to grind well, fully grind again 20min after adding the 300mg lavo-ofloxacin hydrochloride, be placed in 50 ℃ of dry 4h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion lavo-ofloxacin hydrochloride;
(3) will join in the needle-leaved wood fibre suspension that mass fraction is 0.4% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion lavo-ofloxacin hydrochloride of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
By Fig. 2～3, can be found out, when not adding the grafted cyclodextrin cationic starch of inclusion antibacterials, paper pulp fiber distributes loose, and fiber fines is fewer, and Gap-Ratios is larger; When the addition over dry stock quality that is needle-leaved wood fibre suspension 2% the time, fiber fines increases, fiber architecture becomes closely, the fiber fines showed increased is arranged evenly.
The cationic starch of the present embodiment is cornstarch.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
Embodiment 6
(1) under room temperature, the 10g beta-schardinger dextrin-joins in the sodium hydroxide solution that 25ml concentration is 600g/L, slowly add 3.6ml ethylene glycol diglycidylether solution, stir 20min under 60 ℃, then adding the substitution value of 2.5g after gelatinization is 0.021 cationic starch, continues to stir 4h, neutralize and be neutral with the hydrochloric acid solution of 2mol/L, add 50ml ethanol, centrifugation 30min under 3000r/min, freeze drying 12h obtains the cationic starch of grafted cyclodextrin;
(2) grafting ring 2g made is stuck with paste cationic starch and is placed in mortar, add 8g water to grind well, fully grind again 20min after adding the 500mg retens, be placed in 60 ℃ of dry 4h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion retens;
(3) will join in the bamboo pulp fiber suspension that mass fraction is 0.6% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion antibacterials of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
The cationic starch of the present embodiment is farina.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
Embodiment 7
(1) under room temperature, the 5g beta-schardinger dextrin-joins in the sodium hydroxide solution that concentration is 100g/L, slowly add bisphenol A diglycidyl ether, stir 10min under 30 ℃, then adding the substitution value after gelatinization is 0.01 cationic starch, continues to stir 1h, neutralize and be neutral with the hydrochloric acid solution of 1.5mol/L, add 50ml acetone, centrifugation 30min under 3000r/min, freeze drying 12h obtains the cationic starch of grafted cyclodextrin;
Wherein, the mass ratio of described cyclodextrin and sodium hydroxide solution is 1:4; The mol ratio of described bisphenol A diglycidyl ether and cyclodextrin is 2:1; Described cationic starch after gelatinization and the mass ratio of cyclodextrin are 1:2;
(2) grafting ring 2g made is stuck with paste cationic starch as in mortar, add 4g water to grind well, fully grind again 10min after adding the 200mg Ciprofloxacin Hydrochloride, be placed in 40 ℃ of dry 6h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion Ciprofloxacin Hydrochloride;
(3) will join in the needle-leaved wood fibre suspension that mass fraction is 0.3% with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion Ciprofloxacin Hydrochloride of over dry stock quality, manufacturing paper with pulp is quantitatively 60g/m
2paper.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
The cationic starch of the present embodiment is cornstarch.
Embodiment 8
(1) under room temperature, 7.5g beta-schardinger dextrin-joins in the sodium hydroxide solution that concentration is 600g/L, then slowly add bisphenol A diglycidyl ether, stir 30min under 80 ℃, then adding the substitution value of 2.5g after gelatinization is 0.07 cationic starch, continues to stir 4h, neutralize and be neutral with the hydrochloric acid solution of 1mol/L, add 50ml ethanol, centrifugation 15min under 5000r/min, freeze drying 12h obtains the grafting ring and sticks with paste cationic starch;
Wherein, the mass ratio of described cyclodextrin and sodium hydroxide solution is 1:8; The mol ratio of described bisphenol A diglycidyl ether and cyclodextrin is 10:1; Described cationic starch after gelatinization and the mass ratio of cyclodextrin are 1:6;
(2) grafting ring 2g made is stuck with paste cationic starch as in mortar, add 10g water to grind well, fully grind again 30min after adding the 800mg retens, be placed in 60 ℃ of dry 3h of air dry oven, and then with deionized water washing 3 times, freeze drying 12h obtains the grafted cyclodextrin cationic starch of inclusion retens;
(3) will with respect to the grafted cyclodextrin cationic starch of 0%, 0.1%, 1%, 2% inclusion retens of over dry stock quality join in the broad-leaved wood fiber suspension that mass fraction is 0.6%, manufacturing paper with pulp is quantitatively 60g/m
2paper.
The cationic starch of the present embodiment is farina.
The antibacterial effect of paper prepared by the present embodiment and mechanical properties results are in Table 1.
The test result of the paper with antibacterial effect of table 1 embodiment 1～8 preparation
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (7)
1. the preparation method with paper of antibacterial effect, is characterized in that, comprises the following steps:
(1) under room temperature, cyclodextrin is joined in the sodium hydroxide solution that concentration is 100～600g/L, then slowly add the epoxies crosslinking agent, stir 10～30min under 30～80 ℃, then add the cationic starch after gelatinization, continue to stir 1～4h, regulate pH to neutral with hydrochloric acid solution, add organic solvent, centrifugation, obtain the grafted cyclodextrin cationic starch after freeze drying;
Wherein, the mass ratio of described cyclodextrin and sodium hydroxide solution is 1:4～1:8; The mol ratio of described epoxies crosslinking agent and cyclodextrin is 2:1～10:1; Described cationic starch after gelatinization and the mass ratio of cyclodextrin are 1:2～1:6;
(2) the grafted cyclodextrin cationic starch prepared by step (1) is placed in mortar, add the deionized water of 2～5 times of weight to grind well, fully grind again 15～30min after adding antibacterials, be placed in again the dry 3～6h of 40～60 ℃ of air dry ovens, and then with the deionized water washing, obtain the grafted cyclodextrin cationic starch of inclusion antibacterials after freeze drying; The addition of described antibacterials is 10%～40% of grafted cyclodextrin cationic starch quality;
(3) the grafted cyclodextrin cationic starch of the inclusion antibacterials that prepared by step (2) joins in fibrous suspension, the paper of manufacturing paper with pulp; 0.1%～2% of the over dry stock quality that the addition of the grafted cyclodextrin cationic starch of described inclusion antibacterials is fibrous suspension.
2. the preparation method with paper of antibacterial effect according to claim 1, is characterized in that, described epoxies crosslinking agent is a kind of in epoxychloropropane, ethylene glycol diglycidylether or bisphenol A diglycidyl ether.
3. the preparation method with paper of antibacterial effect according to claim 1, is characterized in that, described cationic starch is a kind of in cornstarch or farina, and substitution value is 0.01～0.07.
4. the preparation method with paper of antibacterial effect according to claim 1, is characterized in that, described cyclodextrin is beta-schardinger dextrin-.
5. the preparation method with paper of antibacterial effect according to claim 1, is characterized in that, described antibacterials are a kind of in Ciprofloxacin Hydrochloride, lavo-ofloxacin hydrochloride or retens.
6. the preparation method with paper of antibacterial effect according to claim 1, is characterized in that, the described organic solvent of step (1) is a kind of in ethanol, methyl alcohol or acetone.
7. the preparation method with paper of antibacterial effect according to claim 1, is characterized in that, step (1) is centrifugal, is specially:
The centrifugation rotating speed is 3000～5000r/min, and centrifugation time is 15～30min.
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| CN106349396A (en) * | 2016-08-26 | 2017-01-25 | 湖南尔康制药股份有限公司 | Ultrasonic-sensitive crosslinked starch |
| CN107881846A (en) * | 2017-11-21 | 2018-04-06 | 常州思宇环保材料科技有限公司 | A kind of preparation method of the antibacterial cardboard of high bond strength |
| CN107936416A (en) * | 2017-12-21 | 2018-04-20 | 宁波爱克创威新材料科技有限公司 | A kind of medical antibacterial thin-film material and preparation method thereof |
| CN108990979A (en) * | 2018-08-14 | 2018-12-14 | 广州超威日化股份有限公司 | It a kind of cationic germicide and reduces cationic germicide irritation and extends the method for antibacterial time |
| CN112796161A (en) * | 2020-12-31 | 2021-05-14 | 南京林业大学 | Modified natural polymer and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106349396A (en) * | 2016-08-26 | 2017-01-25 | 湖南尔康制药股份有限公司 | Ultrasonic-sensitive crosslinked starch |
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| CN107936416A (en) * | 2017-12-21 | 2018-04-20 | 宁波爱克创威新材料科技有限公司 | A kind of medical antibacterial thin-film material and preparation method thereof |
| CN108990979A (en) * | 2018-08-14 | 2018-12-14 | 广州超威日化股份有限公司 | It a kind of cationic germicide and reduces cationic germicide irritation and extends the method for antibacterial time |
| CN112796161A (en) * | 2020-12-31 | 2021-05-14 | 南京林业大学 | Modified natural polymer and preparation method and application thereof |
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| CN103437247B (en) | 2016-03-02 |
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