CN103668520B - A kind of antibacterial regenerated celulose fibre and preparation method thereof - Google Patents
A kind of antibacterial regenerated celulose fibre and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of antibacterial regenerated celulose fibre and preparation method thereof, the chitosan quaternary ammonium salt that contains 0.5～10wt% in described antibacterial regenerated celulose fibre, preparation method comprises the following steps: deionized water, NaOH for chitosan quaternary ammonium salt are made into antiseptic solution by (1). (2) adopting cellulose pulp is that raw material makes spinning viscose. (3) antiseptic solution is added to yellow step to the viscose solution in arbitrary step before spinning, the addition of chitosan quaternary ammonium salt be in viscose solution chemical cellulose weight 0.5～10%, obtain antibacterial spinning viscose solution. (4) by antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, dry and obtain antibacterial regenerated celulose fibre. Antibacterial regenerated celulose fibre of the present invention has the premium properties such as biodegradability, biocompatibility, security and antibiotic property simultaneously, gives the better moisture-absorbing moisture-keeping of viscose rayon, wrinkle resistance, flexibility simultaneously.
Description
Technical field
The present invention relates to functional fiber cellulose fiber, be specifically related to a kind of taking chitosan derivatives as antisepticAntibacterial regenerated celulose fibre and technology of preparing thereof.
Background technology
Shitosan is the alkaline polysaccharide of the unique existence of occurring in nature, have biodegradability, biocompatibility,The premium properties such as security and antibiotic property. Due to the anti-microbial property that shitosan has, its wound suture,Processing the aspects such as vegetable seeds, disinfectant, hand cleanser obtains a wide range of applications. To shitosan by modificationObtaining quaternary chitosan derivatives material, is one of important research direction improving chitosan anti-bacteria,Also be the hot fields of anti-mattress investigation of materials.
Wherein, chitosan quaternary ammonium salt is a kind of important chitosan derivatives, has nontoxic, antibacterial and antibacterialThe feature such as active good, thus be widely used in environmental protection, food processing, drug loading, controlled release andThe technical fields such as the preparation of antibacterial bacteriostatic material. The special molecular structure that shitosan and quaternary ammonium salt thereof have canFor improving moisture absorbability and moisture retentivity, antistatic behaviour, antibiotic property, wrinkle resistance, the flexibility of fabric, and dyeability.
Although chitosan quaternary ammonium salt can give textile many premium properties, in the application of field of textilesBe mainly to use it as after-finishing of textile products agent, when use, mostly adopt traditional rear finishing technique, make to give and knitThe function of thing can not get lasting maintenance. The textile ox of patent documentation CN201310119583.5 as has been publiclyThe chitosan quaternary ammonium salt antibiotic finishing method of young cloth, CN200910200566.8 water-soluble chitosan quaternary ammonium saltAntibacterial finishing agent and preparation thereof and application, CN201310119582.0 jean cloth antibacterial finishing process shellGlycan quaternary ammonium salt dressing liquid is all the skills that adopt chitosan quaternary ammonium salt pair fabric to carry out rear arrangement in these documentsArt. Therefore, the various premium properties that have according to shitosan and derivative thereof, improve chitosan quaternary ammonium saltThe process technology of the textile to variety classes and material, sends out greatly promoting its application at field of textilesExhibition.
Viscose rayon is as regenerated celulose fibre, and it is good that its goods have sucting wet air permeability, spy comfortable and easy to wearPoint, in prior art, based on the feature of cellulose viscose manufacturing technique length, complex process, in recent years, along withThe appearance of various functional viscose fibers, various antibacterial viscose fibers also arise at the historic moment, and wherein also have use shellGlycan to viscose rayon modification prepare the research report of antibacterial viscose fiber. Example is patent documentation as has been publiclyThe manufacture method of CN201010200183.3 hydroxyethyl chitosan modified viscose fiber, CN200610015705.6A kind of hydroxyethyl chitosan modified viscose fiber and manufacture method thereof are all to use hydroxyethyl chitosan to fiberCellulose fiber carries out modification, and due to after shitosan directly adds in viscose solution, viscose solution there will be gel existingResemble, affect spinning spinnability, therefore in prior art, all will carry out alkalization, the yellow etc. of chitosan derivativesComplicated process treatment process, therefore not only exists technological process long, and equipment investment is large, the asking of complex processTopic, and the anti-microbial property of the antibacterial viscose fiber preparing is barely satisfactory, does not even reach national regulationAntibacterial index, cause the industrialization of chitosan anti-bacteria cellulose fibre to be restricted.
Summary of the invention
First technical problem to be solved by this invention is: for antibacterial regenerated cellulose of the prior artThe problem of fibre antibacterial poor performance, provides a kind of more antibacterial as antibacterial modified dose of chitosan quaternary ammonium salt that useRaw cellulose fibre, the bacteriostatic activity of this anti-bacterial fibre cellulose fiber and bactericidal activity all exceed GB regulation.
Second technical problem to be solved by this invention is: for antibacterial regenerated cellulose fibre in prior artThe production. art long flow path of supporting one's family, equipment investment is large, complex process, and the antibacterial regenerated celulose fibre of preparation is anti-The problem that bacterium property is poor, provides that a kind of technological process is short, technique is simple, the pressing down of the anti-bacterial fibre cellulose fiber of preparationThe preparation method of the antibacterial regenerated celulose fibre that bacterium activity and bactericidal activity are high.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
A kind of antibacterial regenerated celulose fibre, contains 0.5～10wt%'s in described antibacterial regenerated celulose fibreChitosan quaternary ammonium salt, substitution value >=80% of described chitosan quaternary ammonium salt, described antibacterial regenerated celulose fibreBacteriostatic activity value >=2.5, bactericidal activity value >=1.0.
Preferred as one, described chitosan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan.
As further preferably, described chitosan quaternary ammonium salt comprise HACC,At least one in hydroxypropyl alkyl-dimethyl ammonium chloride shitosan.
As further preferred, described chitosan quaternary ammonium salt is HACC.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) deionized water, NaOH for chitosan quaternary ammonium salt are made into antiseptic solution, described antiseptic solutionThe mass concentration of middle chitosan quaternary ammonium salt is 1～10%, and the mass concentration of NaOH is 5～15%.
(2) adopting cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow stepMake cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds the middle yellow step of step (2) to spinningIn viscose solution in front arbitrary step, the addition of described chitosan quaternary ammonium salt is alpha fibers in viscose solution0.5～10% of element weight, obtains antibacterial spinning viscose solution.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, bakingDryly obtain described antibacterial regenerated celulose fibre.
Improve as one, in step (3), add and in the viscose solution before described antiseptic solution, contain α fibreDimension element 8.5～10wt%, NaOH 4～5wt%, the viscosity of viscose solution is that 30～60s(falling ball method is surveyedFixed viscosity), add in the antibacterial spinning viscose solution after described antiseptic solution, contain chemical cellulose 7～9.5wt%, NaOH 4.5～7wt%, the viscosity of antibacterial spinning viscose solution is 30～55s.
Preferred as one, the temperature of described coagulating bath is 40～60 DEG C, sulfur acid 90 in described coagulating bath～130g/l, zinc sulfate and/or aluminum sulfate 5～15g/l, sodium sulphate 270～350g/l.
Preferred as one, the total stretch ratio of described drawing-off is 30～200%.
Preferred as one, described chitosan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan, and described shell is poly-Substitution value >=80% of sugar quaternary ammonium salt.
As further preferably, described chitosan quaternary ammonium salt comprise HACC,At least one in hydroxypropyl alkyl-dimethyl ammonium chloride shitosan.
As further preferred, described chitosan quaternary ammonium salt is HACC.
Owing to having adopted technique scheme, the invention has the beneficial effects as follows:
Antibacterial regenerated celulose fibre of the present invention, adopts chitosan quaternary ammonium salt as chitosan antimicrobial agent, shellThe antibiotic property mechanism of glycan quaternary ammonium salt is that the primary amine groups on shitosan and chitosan oligosaccharide C2 becomes occurring in natureUnique alkalescence sugar, makes shitosan and chitosan oligosaccharide have biocidal property and bacterium surface is nearly all acidity, and seasonAmmonium group cation is by the effects such as the hydrophobic binding between electrostatic force, hydrogen bond and protein molecule, adsorption band negative electricityBacterial body, be gathered on cell membrane, can form polyelectrolyte polymer, form not tool at cell peripheralThere is infiltrative top layer, stop nutriment to see through cell membrane and make bacterium can not carry out metabolism, generating chamberInhibition effect, can cause bacterial growth suppressed and dead. Due to chitosan quaternary ammonium salt self have good antibacterialPerformance, and with the good blended characteristic of spinning viscose, the antibacterial regenerated celulose fibre that the present invention makes withTime there is the premium properties such as biodegradability, biocompatibility, security and antibiotic property, antibacterial functions is heldFor a long time, human body is had no side effect, give the better moisture-absorbing moisture-keeping of viscose rayon, wrinkle resistance, flexibility simultaneouslyDeng premium properties. The antibacterial regenerated celulose fibre that the present invention prepares is to gram-positive bacteria and gramNegative bacterium all has good bacteriostasis, and total bacteriostasis rate reaches more than 95%.
In prior art, due to after shitosan and derivative thereof add in viscose solution, can cause viscose glue to occurGelatin phenomenon, thus spinning spinnability affected, and affect fungistatic effect, therefore those skilled in the art are generalAll over thinking, before co-blended spinning, the derivative of shitosan or shitosan first should be alkalized, after yellow,Obtain the xanthogenate solution of shitosan or chitosan derivatives, and then with spinning viscose blend after spinning,The spinning spinnability of guarantee process stabilizing. But not only there is complex process, production in this processLong flow path, the problem such as equipment investment is large, and use carbon disulfide when yellow, also there is work and environment dirtDye problem. And the inventor is devoted for years in the research of cellulose fibre and functional fiber cellulose fiber, warpCross the research and analysis of cellulose and chitosan structure are found, cellulose and shitosan have closely similarMolecular structure, with hydroxypropyl alkyl ammomium chloride shitosan difference be only the hydroxypropyl of C2 on glucose ringAlkyl ammomium chloride and hydroxyl, structural similitude, makes the two should have good compatibility. Therefore,After through lot of experiments checking, the present invention has broken must first shell being gathered that those skilled in the art thinkAfter the derivative xanthic acid esterification of sugar or shitosan with the technical conceive of viscose solution blend, but by shellGlycan quaternary ammonium salt is dissolved in sodium hydroxide solution, then directly with viscose solution blend after spinning, not only simpleChange production stage, reduced equipment investment, alleviated work and environmental pollution, and adopted shitosan seasonAmmonium salt is as bactericide, and the antibacterial cellulose fibre antibacterial effect preparing is more excellent.
The spinning spinnability of spinning spinnability, especially functional viscose fiber in viscose rayon preparation,Owing to having sneaked into functional materials in viscose solution, therefore, in the time of spinning, the performance indications of viscose solution, glueThe matching of sol solution and coagulating bath be all determine spinning spinnability and functional fiber quality decisive because ofElement, the applicant determines by lot of experiment validation, in the viscose solution adding before antiseptic solution, contains αCellulose 8.5～10wt%, NaOH 4～5wt%, the viscosity of viscose solution is 30～60s(falling ball methodThe viscosity of measuring), add in the antibacterial spinning viscose solution after antiseptic solution, contain chemical cellulose 7～9.5wt%, NaOH 4.5～7wt%, the viscosity of antibacterial spinning viscose solution is 30～55s, adopts and is applicable toIn the viscose solution of spinning moulding, be the spinning spinnability that ensured and the performance of finished product anti-bacterial fibre cellulose fiberThe further safeguard measure of index.
Detailed description of the invention
Further set forth the present invention below in conjunction with specific embodiment.
Embodiment 1
A kind of antibacterial regenerated celulose fibre, the shell that contains 1.5wt% in described antibacterial regenerated celulose fibre is poly-Sugar quaternary ammonium salt, the substitution value of described chitosan quaternary ammonium salt is 85%, described antibacterial regenerated celulose fibre press downBacterium activity value 3.2, bactericidal activity value 1.55.
Embodiment 2
A kind of antibacterial regenerated celulose fibre, the hydroxypropyl that contains 3.5wt% in described antibacterial regenerated celulose fibreBase trimethyl ammonium chloride shitosan, the substitution value of described HACC is 94, described inThe bacteriostatic activity value 4.2 of antibacterial regenerated celulose fibre, bactericidal activity value 2.58.
Embodiment 3
A kind of antibacterial regenerated celulose fibre, the hydroxypropyl that contains 7.5wt% in described antibacterial regenerated celulose fibreBase alkyl-dimethyl ammonium chloride shitosan, the substitution value of described HACC is 92%,The bacteriostatic activity value 3.95 of described antibacterial regenerated celulose fibre, bactericidal activity value 1.9.
Embodiment 4
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) the hydroxypropyl alkyl ammomium chloride that is 88% by substitution value for shitosan deionized water, NaOH joinBecome antiseptic solution, in described antiseptic solution, the mass concentration of hydroxypropyl alkyl ammomium chloride shitosan is 3%, hydrogen-oxygenThe mass concentration of changing sodium is 8%.
(2) adopting cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow stepMake cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution use step (1) being prepared is spun front injection and is added gluing before spinning toIn sol solution, the addition of described hydroxypropyl alkyl ammomium chloride shitosan is chemical cellulose weight in viscose solution1.5%, obtain antibacterial spinning viscose solution.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, bakingDryly obtain described antibacterial regenerated celulose fibre.
Embodiment 5
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) deionized water, the NaOH for HACC that are 90% by substitution valueBe made into antiseptic solution, in described antiseptic solution, the mass concentration of NaOH is 10%.
(2) adopting cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow stepMake cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds fiber in the middle yellow step of step (2) toIn element yellow acid fat, then dissolve and obtain viscose solution, the adding of described HACCAmount, for 2.5% of chemical cellulose weight in viscose solution, obtains antibacterial spinning viscose solution; Add described antibacterialIn viscose solution before solution, contain chemical cellulose 8.5wt%, NaOH 4wt%, the viscosity of viscose solution isThe viscosity that 45s(falling ball method is measured), add in the antibacterial spinning viscose solution after described antiseptic solution and contain αCellulose 7wt%, NaOH 4.5wt%, the viscosity of antibacterial spinning viscose solution is 43s.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, bakingDryly obtain described antibacterial regenerated celulose fibre.
Embodiment 6
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) deionized water, the NaOH for HACC that are 92% by substitution valueBe made into antiseptic solution, in described antiseptic solution, the mass concentration of HACC is 5%,The mass concentration of NaOH is 15%.
(2) adopting cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow stepMake cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds gluing in dissolving step in step (2) toIn sol solution, the addition of described HACC is chemical cellulose weight in viscose solution7.0% of amount, obtains antibacterial spinning viscose solution; Add in the viscose solution before described antiseptic solution and contain αCellulose 9.2wt%, NaOH 4.5wt%, the viscosity of viscose solution is the viscosity that 50s(falling ball method is measured),Add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 8.7wt%, NaOH5.6wt%, the viscosity of antibacterial spinning viscose solution is 47s.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, bakingDryly obtain described antibacterial regenerated celulose fibre, the temperature of described coagulating bath is 51 DEG C, in described coagulating bath, containsSulfuric acid 100g/l, zinc sulfate 9.5g/l, sodium sulphate 290g/l, the total stretch ratio of described drawing-off is 50%.
Embodiment 7
A preparation method for antibacterial regenerated celulose fibre, comprises the following steps:
(1) the hydroxypropyl alkyl-dimethyl ammonium chloride that is 95% by substitution value is deionized water, hydrogen-oxygen for shitosanChange sodium and be made into antiseptic solution, in described antiseptic solution, the quality of hydroxypropyl alkyl-dimethyl ammonium chloride shitosan is denseDegree is 2.5%, and the mass concentration of NaOH is 12%.
(2) adopting cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow stepMake cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step.
(3) antiseptic solution step (1) being prepared adds gluing in maturation step in step (2) toIn sol solution, the addition of described hydroxypropyl alkyl-dimethyl ammonium chloride shitosan is alpha fibers in viscose solution5.0% of element weight, obtains antibacterial spinning viscose solution; Add in the viscose solution before described antiseptic solution and containHave chemical cellulose 9.5wt%, NaOH 5wt%, the viscosity of viscose solution is the sticky of 55s(falling ball method mensurationDegree), add in the antibacterial spinning viscose solution after described antiseptic solution and contain chemical cellulose 9.2wt%, hydrogen-oxygenChange sodium 6.5wt%, the viscosity of antibacterial spinning viscose solution is 53s.
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, then through refining, bakingDryly obtain described antibacterial regenerated celulose fibre, the temperature of described coagulating bath is 55 DEG C, in described coagulating bath, containsSulfuric acid 125g/l, aluminum sulfate 12g/l, sodium sulphate 320g/l, the total stretch ratio of described drawing-off is 120%.
Comparative example 1
Comparative example 1 is that with the difference of embodiment 6 antiseptic using is hydroxyethyl chitosan, all the otherAll identical.
Comparative example 2
Comparative example 2 is with the difference of embodiment 6: step (1), in the time preparing antiseptic solution, adoptsAlkalization, the yellow technique of HACC prepare: 1. alkalization: by hydroxypropyl threeAmmonio methacrylate for shitosan deionized water, dissolution of sodium hydroxide become alkalizing solution, hydroxyl in described alkalizing solutionThe mass concentration of oxypropyl trimethyl ammonium chloride shitosan is 5%, and the mass concentration of NaOH is 15%; 2. yellowOrtho acid esterification: the alkalizing solution of gained HACC in is 1. placed in to sealing anti-Answer in still, add the carbon disulfide of HACC quality 45%, keep reaction temperatureBe 15 DEG C, yellow reaction 4 hours, obtains the antibacterial molten of HACC xanthateLiquid.
Comparative example 3
Comparative example 3 is with the difference of comparative example 2: the antiseptic of use is hydroxyethyl chitosan, itsYu Jun is identical.
Anti-microbial property and the mechanical performance of the anti-bacterial fibre that embodiment 4-7 and comparative example 1-3 prepareIndex situation sees the following form. While detecting anti-microbial property, testing bacterial classification is: staphylococcus aureus ATCC6538, pressesThe test of JISL1902-2008 textile fabrics antibacterial activity, inoculation bacterial concentration (CFU/ml) 1.6 × 105，Incubation time 18h, bacteria concentration mensuration-colony counting method.
As can be seen from the above table, constant in process, only convert under the prerequisite of antiseptic, the present invention selectsChitosan quaternary ammonium salt has better antibacterial effect than hydroxyethyl chitosan, under the identical prerequisite of antiseptic, makesWith direct blending of the present invention and use first by chitosan derivatives through alkalization, after yellow again with viscose solutionBlend, anti-microbial property the indifference of its anti-bacterial fibre cellulose fiber of preparing.
Claims (3)
1. a preparation method for antibacterial regenerated celulose fibre, is characterized in that comprising the following steps:
(1) deionized water, NaOH for chitosan quaternary ammonium salt are made into antiseptic solution, described antiseptic solutionThe mass concentration of middle NaOH is 5～15%, substitution value >=80% of described chitosan quaternary ammonium salt;
(2) adopting cellulose pulp is raw material, through comprising dipping, squeezing, pulverizing, experienced, yellow stepMake cellulose sulfonate, and then make spinning viscose through dissolving, deaeration and filtration step;
(3) antiseptic solution step (1) being prepared adds the middle yellow step of step (2) to spinningIn viscose solution in front arbitrary step, the addition of described chitosan quaternary ammonium salt is α fibre in viscose solutionTie up 0.5～10% of plain weight, obtain antibacterial spinning viscose solution; Add gluing before described antiseptic solutionIn sol solution, contain chemical cellulose 8.5～10wt%, NaOH 4～5wt%, the viscosity of viscose solution is30～60s, add in the antibacterial spinning viscose solution after described antiseptic solution, contain chemical cellulose 7～9.5wt%, NaOH 4.5～7wt%, the viscosity of antibacterial spinning viscose solution is 30～55s;
(4) by described antibacterial spinning viscose solution through coagulating bath spinning, draw forming, always the leading of described drawing-offStretch than being 50～120%; Then obtain described antibacterial regenerated celulose fibre through refining, oven dry, described inThe temperature of coagulating bath is 40～60 DEG C, sulfur acid 90～130g/l in described coagulating bath, zinc sulfate and/Or aluminum sulfate 5～15g/l, sodium sulphate 270～350g/l.
2. the preparation method of antibacterial regenerated celulose fibre as claimed in claim 1, is characterized in that: described shellGlycan quaternary ammonium salt is hydroxypropyl alkyl ammomium chloride shitosan.
3. the preparation method of antibacterial regenerated celulose fibre as claimed in claim 2, is characterized in that: described shellGlycan quaternary ammonium salt comprises that HACC, hydroxypropyl alkyl-dimethyl ammonium chloride shell gatherAt least one in sugar.
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| JP6203158B2 (en) | 2014-10-15 | 2017-09-27 | ユニ・チャーム株式会社 | Method for producing recycled pulp from used sanitary products |
| CN109983172A (en) * | 2016-09-19 | 2019-07-05 | 格拉姆工业有限公司 | Antibacterial regenerated celulose fibre and preparation method thereof |
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| CN106757521B (en) * | 2016-12-15 | 2018-12-28 | 宜宾屏山辉瑞油脂有限公司 | A kind of preparation method of chitosan oligosaccharide cellulose fibre |
| CN106905438B (en) * | 2017-03-14 | 2021-11-30 | 西南交通大学 | Chitosan quaternary ammonium salt antibacterial cellulose and preparation method thereof |
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| CN110172741B (en) * | 2019-02-26 | 2020-09-15 | 东华大学 | Preparation method of functional cellulose fiber |
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| CN111450304A (en) * | 2020-03-17 | 2020-07-28 | 青岛博益特生物材料股份有限公司 | Positively charged biological fiber hemostatic and bacteriostatic material and preparation method and application thereof |
| CN113151925A (en) * | 2021-04-07 | 2021-07-23 | 罗莱生活科技股份有限公司 | Polyquaternary ammonium salt/aloe antibacterial fiber, preparation method thereof and application thereof in antibacterial towels |
| CN115897061A (en) * | 2022-09-06 | 2023-04-04 | 河南省超亚医药器械有限公司 | Novel degradable spunlaced nonwoven material |
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Effective date of registration: 20211206 Address after: 224400 Jiangsu Yancheng Funing high tech Industrial Development Zone Aoyang Avenue Saideli (Yancheng) Fiber Co., Ltd Patentee after: Saideli (Yancheng) Fiber Co.,Ltd. Address before: 224400 No. 1, Aoyang Avenue, Aoyang Industrial Park, Funing County, Yancheng City, Jiangsu Province Patentee before: FUNING AOYANG TECHNOLOGY CO.,LTD. |
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