WO2012074153A1 - Mélange maître de polyester doté de propriétés antimicrobiennes exceptionnelles et procédé de production - Google Patents

Mélange maître de polyester doté de propriétés antimicrobiennes exceptionnelles et procédé de production Download PDF

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Publication number
WO2012074153A1
WO2012074153A1 PCT/KR2010/008617 KR2010008617W WO2012074153A1 WO 2012074153 A1 WO2012074153 A1 WO 2012074153A1 KR 2010008617 W KR2010008617 W KR 2010008617W WO 2012074153 A1 WO2012074153 A1 WO 2012074153A1
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WIPO (PCT)
Prior art keywords
silver
sulfur
polyester
polyester masterbatch
nanocomposite
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PCT/KR2010/008617
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English (en)
Korean (ko)
Inventor
정성훈
김장회
신유식
최태수
정해림
정기훈
손은종
Original Assignee
주식회사 엔피텍
황영구
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Priority to PCT/KR2010/008617 priority Critical patent/WO2012074153A1/fr
Publication of WO2012074153A1 publication Critical patent/WO2012074153A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/103—Agents inhibiting growth of microorganisms
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers

Definitions

  • the present invention relates to a polyester masterbatch having excellent antimicrobial properties and a method for manufacturing the same, and more particularly, to a method for producing a silver nanosilver composite including sulfur and a polyester master batch including the same.
  • the present invention relates to a polyester masterbatch which can be used in ultrafine polyester warp pile fabrics which are particularly suitable for bedding with permanent antibacterial and deodorizing performance.
  • warp pile fabrics can be used in various tissue designs and applications, they are used as materials for a variety of household goods, ranging from acupuncture products, toys, and baby products.
  • Products made of micro fibers, in particular, fine polyester Textile products have been used in various fields because of their soft touch and excellent quality, but there is a limit of synthetic fibers compared to natural fibers for acupuncture.
  • polyester fibers which are also widely used as clothing, grow microorganisms due to sweat and external pollution of a human body, a large amount of ammonia is generated to cause an unpleasant smell as well as a problem that is harmful to the human body. For this reason, there have been a lot of studies in the development of textile materials in order to give a function of inhibiting the growth of bacteria harmful to the human body.
  • Organic silicon-based quaternary ammonium salt compounds are widely used as one of the methods of imparting antimicrobial properties to the fibers, but have the disadvantage of yellowing when using laundry durability and chlorine-based detergents.
  • nano silver particles are known as materials having excellent antimicrobial properties and are used in various industrial fields.
  • Japanese Laid-Open Patent Publication No. 2005-248161 discloses a method of preparing clay by adding clay containing silver nanoparticles to a polyester. This has the effect of providing antibacterial properties and improving flame retardancy, but there is a problem of aggregation of silver nanoparticles.
  • US Patent Publication 2006/0020108 describes a method of preparing a polyester master batch by mixing and polymerizing a glycol containing a silver precursor with terephthalic acid.
  • the patent has a problem that only a portion of the silver is reduced from the silver precursor, there is a disadvantage that the durability of the silver nanoparticles are poor.
  • Korean Patent Laid-Open Publication No. 2005-0075905 is a technology related to a composite fiber that has a island-in-sea cross-section by composite spinning a polyester polymer containing silver particles, but has a high antibacterial and long antimicrobial duration, but aggregates silver nanoparticles. It has a problem, and it has the disadvantage of not being permanent.
  • the present inventors are directed to providing a polyester masterbatch chip including a nanosilver composite which can solve the disadvantages of improving the dispersibility of silver nanoparticles of the prior art, adhesion between silver nanoparticles and a polymer resin, and low compatibility. Because the polyester masterbatch chip produced in the present invention has an excellent antimicrobial effect, it can be used to produce a very fine polyester warp pile fabric particularly suitable for acupuncture.
  • the present invention provides a polyester masterbatch comprising a silver-sulfur nanocomposite so that the silver-sulfur nanocomposite can function permanently and subsequently form a polyester fiber and a warp pile fabric using the same. To provide that purpose.
  • the present invention provides a polyester master batch comprising a silver-sulfur nanocomposite.
  • the silver-sulfur nanocomposite is prepared by contacting the silver nanoparticles produced by the liquid phase reduction method with a sulfur compound using hydrazine as a reducing agent.
  • the silver-sulfur nanocomposite is prepared by combining silver ions with sulfur and then reducing them with a hydrazine reducing agent.
  • the silver-sulfur nanocomposite is selected from the group consisting of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, and polyacrylamide as an dispersant by alcohol reduction.
  • the silver nano colloidal solution is prepared by contacting the sulfur compound.
  • the sulfur compound is characterized in that one selected from the group consisting of sodium sulfide, hydrogen sulfide, sulfur oxides and thiol compounds.
  • the present invention provides a polyester masterbatch comprising a silver-sulfur nanocomposite capable of producing a polyester-based microfine fiber, thereby providing an antimicrobial / deodorant function to provide functions such as sterilization and aroma.
  • a polyester masterbatch comprising a silver-sulfur nanocomposite capable of producing a polyester-based microfine fiber, thereby providing an antimicrobial / deodorant function to provide functions such as sterilization and aroma.
  • the silver nano-composite is prepared in the form of nano powder and master batch is added to the PET spinning process to maximize the adhesion in the fiber can be used permanently.
  • FIG. 1 illustrates XRD analysis to examine the structure and crystallinity of the silver nanocomposite prepared in Example 2.
  • FIG. 1 illustrates XRD analysis to examine the structure and crystallinity of the silver nanocomposite prepared in Example 2.
  • FIG. 2 is a SEM photograph of the silver-sulfur nanocomposite prepared in Example 2.
  • the present invention provides a polyester masterbatch containing nanosilver composites.
  • the nanosilver composite is a nanoparticle in which silver particles and other functional materials are combined, and sulfur (S) may be mentioned as a material that can be suitably used in the present invention.
  • Silver (Ag) is a metal with sterilization ability. When it is made of nanoparticles, the antimicrobial performance of silver is changed qualitatively, and it is not only strong sterilization and antibacterial ability, but also odor removal, electromagnetic wave and UV protection, far infrared rays and anion emission. It has the effect of back and is most used as an antimicrobial material.
  • Sulfur (S) is known to have excellent antibacterial and bactericidal properties as it is widely used as an insecticide component.
  • Silver nanoparticles alone require a long time for the antibacterial and sterilization of harmful bacteria during antibacterial and sterilization, silver nanoparticles have a weak antimicrobial and bactericidal effect against some fungi. Therefore, the present invention can compensate for the shortcomings of these silver nanoparticles using a complex of silver and sulfur.
  • the silver-sulfur nanocomposite prepared in the present invention has sulfur atoms attached to the silver nanoparticles.
  • sulfur compounds are adsorbed on the surface of the nanosilver particles due to the strong bonding force between silver and sulfur.
  • these particles are washed and recovered, only sulfur atoms remain on the surface of the silver nanoparticles, thereby preparing a silver-sulfur nanocomposite.
  • a method of forming a silver-sulfur nanocomposite using a sulfur compound first, silver nanoparticles are formed, and a silver nanoparticle and a sulfur particle are combined by mixing a solution in which the silver nanoparticles are dispersed and a sulfur compound solution and producing silver nanoparticles There is a method in which the total sulfur component is added to reduce the sulfur atoms and silver ions in a bonded state, thereby producing silver / sulfur particles in which silver and sulfur atoms are uniformly bonded.
  • the sulfur compound that can be preferably used in the above is one selected from the group consisting of sodium sulfide (Na 2 S), hydrogen sulfide (H 2 S), sulfur oxides (SOx compounds) and thiol compounds.
  • a silver-sulfur nanocomposite was prepared using a liquid reduction method or an alcohol reduction method.
  • the particle size of the finally prepared nanocomposites can be controlled to about 30 ⁇ 50nm.
  • the liquid phase reduction method is a method of recovering powder from a high concentration of silver colloid, and the present invention is characterized by using a reducing agent to control the particle size.
  • an aqueous solution is prepared by dissolving one kind selected from the group consisting of silver nitrate, silver iodide, silver sulfate, or silver acetate as a silver source in water, and the temperature is lower than 10 ° C. To keep.
  • an aqueous solution of iron sulfate (FeSO 4 ⁇ 2H 2 O) and sodium citrate solution (Na 3 -Citrate, C 6 H 5 Na 3 O 7 ) are prepared, respectively, and mixed to prepare a mixed aqueous solution.
  • hydrazine (N 2 H 4 ) is added to control the size of the nanoparticles produced by controlling the reduction rate during the production process of silver nanoparticles, and the content ratio of hydrazine and silver is preferably 0.5-2: 1 (molar ratio). .
  • the reaction is advanced while slowly pouring the silver aqueous solution into the mixed aqueous solution. After completion of the reaction, the supernatant is removed by centrifugation, and the solid obtained by adding pure water is dispersed again. To the dispersed solution is added sodium citrate solution to precipitate. Repeat the above procedure 2 to 5 times to completely remove the unreacted ionic substance, and then remove excess water by adding acetone or ethanol to the obtained solid. Since acetone or ethanol has a lower boiling point than water, it easily volatilizes even at low temperatures, thereby minimizing aggregation of particles that may occur during drying.
  • hydrazine N 2 H 4
  • the content ratio of hydrazine and silver nitrate is preferably 0.5-2: 1 (molar ratio).
  • the content ratio of sodium citrate, iron sulfate and silver nitrate is preferably 0.1 to 0.5: 0.5 to 3.0: 1.
  • the content of sodium citrate is 0.1 or less and the concentration of iron sulfate is 0.5 or less, the size of the particles is increased, so it is preferable to control the above range.
  • the content of sodium citrate approaches 0.5
  • the particle size decreases as the electrostatic potential on the particle surface decreases.
  • the concentration of iron sulfate approaches 3 the growth rate decreases due to the increase in nucleation rate. Becomes smaller. Silver oxide is not produced in this process.
  • an aqueous sodium sulfide (Na 2 S) solution is prepared, mixed with the mixed aqueous solution, stirred, and precipitated to remove the supernatant liquid to obtain a solid content.
  • the silver-sulfur nanocomposite may be prepared through a washing process in which the obtained solid content is purely redispersed 2 to 5 times.
  • the sodium sulfide aqueous solution may be added to the step before forming the silver nanoparticles. That is, a mixed aqueous solution of a silver aqueous solution and an aqueous sodium sulfide solution may be prepared first, and then a mixed solution of the iron sulfate aqueous solution and the sodium citrate aqueous solution is added, and the aqueous hydrazine solution may be slowly added to proceed with the reaction.
  • silver nanoparticles can be produced using alcohol reduction.
  • the alcohol reduction method is a chemical synthesis method that does not require a chemical reducing agent.
  • C1-C4 alcohols such as methanol, ethanol, isopropanol and butanol, ethylene glycol, diethylene glycol and propylene glycol are used as solvents and reducing agents.
  • the alcohol reduction method when silver is dissolved or dispersed in alcohol or glycol, and the solution is heated to reflux conditions, silver ions are formed through nucleation and growth by oxidation and reduction reaction between silver ions and a solvent. .
  • polyvinylpyrrolidone in this process, one selected from the group consisting of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, and polyacrylamide may be used, and in particular, polyvinylpyrrolidone may be preferably used.
  • the polyvinylpyrrolidone preferably has a molecular weight of 10,000 to 50,000.
  • the polymer material acts as a dispersant of particles, colloids of silver nanoparticles and metal nanoparticles can be prepared.
  • Silver nanoparticles can be manufactured in uniform size and high concentration using the alcohol reduction method of this invention.
  • Specific manufacturing method is as follows. First, a solvent such as ethanol is added to the reactor and stirred for 5 to 10 minutes. The polymer material is added to the ethanol and dissolved by stirring again for 30 minutes to 1 hour. Next, silver nitrate (AgNO 3 ) was added thereto, stirred for 10 to 20 minutes, and heated and reduced in an oil bath to prepare a silver nano colloid. Reflux was performed using a condenser to prevent the solvent from evaporating by heating. At this time, it is preferable that the molar ratio of a polymer and silver nitrate is 0.5-2: 1. If the molar ratio of the polymer and silver nitrate is less than 0.5, the role of the dispersant to have a uniform size is insignificant. If the ratio exceeds 2.0, it is impossible to expect more than the desired effect, so there is no economic benefit, and the viscosity is increased and workability is increased. Degradation problems may occur.
  • a solvent such as ethanol is added to the reactor and stirred for
  • a sulfur compound preferably a thiol compound, was added to the silver nano colloid to prepare a silver-sulfur nanocomposite colloid.
  • the liquid colloidal form may be used in powder form after removing the solvent and drying.
  • the polyester of the present invention is a polyester (PET) that is commonly used, and is defined as a polymer produced by polycondensation of diols and dicarboxylic acids.
  • Dicarboxylic acids include terephthalic acid, isophthalic acid, phthalic acid, naphthalene dicarboxylic acid, adipic acid, and sebacic acid.
  • Diols include ethylene glycol, trimethylene glycol, tetramethylene glycol and cyclohexane dimethanol.
  • polyesters include polymethylene terephthalate, polyethylene terephthalate, polyethylene-p-oxybenzoate, poly-1,4-cyclohexylene dimethylene terephthalate, and polyethylene-2,6-naphthalate.
  • These polyesters can be copolymers and the copolymerization components are diol components such as diethylene glycol, neopentyl glycol, and polyalkylene glycols and adipic acid, sebacic acid, phthalic acid, isophthalic acid and 2,6-naphthalene dica
  • dicarboxylic acid component such as a letric acid.
  • Preferred for the present invention in terms of mechanical strength, thermal stability, chemical resistance, and durability are polyethylene terephthalate, polypropylene terephthalate, polyethylene isophthalate, polyethylene naphthalate, polyethylene-2,6 naphthalate and their airborne mixtures. There is coalescence.
  • the silver-sulfur nanocomposites and polyester chips are dried in a vacuum of 70 to 90 ° C. to completely remove moisture.
  • the polyester chip and the silver-sulfur nanocomposite are put into a twin screw mix and mixed.
  • the content of the silver-sulfur nanocomposite in the polyester chip is preferably 0.1 to 1wt% by weight.
  • the raw material is melt-mixed at 50 to 100 rpm at 220 to 260 ° C. so that the silver-sulfur nanocomposite particles are evenly attached to the polyester chip.
  • the silver-sulfur nanocomposite particles should be evenly attached so that the silver-sulfur nanocomposite particles do not separate from the fibers during melt spinning or after spinning and have excellent physical properties.
  • the antibacterial activity of the polyester masterbatch prepared according to the present invention was measured physical properties according to the method shown below.
  • Staphylococcus aureus ATCC 6538
  • E. coli Escherichia coli, ATCC 25922
  • the cultured bacteria are diluted with saline to titrate the number of bacteria, and 1 ml of bacterial solution diluted with saline is added to 9 ml of nutrient medium to inoculate the sample.
  • the sample is placed in a plastic solution containing 100 ml of distilled water and shaken at 120 rpm.
  • R is a percentage of the reduction rate
  • A represents the microbial population after 24 hours after inoculating the microorganisms in the experimental group
  • B represents the number of microbial communities inoculated in the experimental group.
  • the obtained silver nano slurry is dispersed in 2,000 g of pure water, 400 g of sodium sulfide aqueous solution in which 17 g of sodium sulfide (Na 2 S) is dissolved is added thereto, stirred, and then precipitated to remove the supernatant liquid to obtain a solid content.
  • the silver-sulfur nanocomposite particles were finally prepared through a washing process of redispersing the obtained solid content twice again with pure water.
  • the prepared silver-sulfur nanocomposite particles were maximally removed with a centrifuge and dried using a lyophilizer to prepare 100g of silver-sulfur composite powders with sulfur adsorbed on silver particles.
  • Pure water is added to the obtained solids and redispersed, followed by further adding 2,000 g of 25% sodium citrate aqueous solution to precipitate. This process was repeated three times to obtain a silver nanoparticle slurry from which the unreacted material was removed, and finally, the final silver-sulfur composite particles were prepared through two washing processes in which redispersed with pure water.
  • the silver-sulfur composite particles thus prepared were 100-g of silver-sulfur nanocomposite powder in which sulfur was adsorbed to silver particles by removing moisture as much as possible by centrifugation and drying using a lyophilizer.
  • FIG. 1 illustrates XRD analysis to examine the structure and crystallinity of the silver nanocomposite prepared in Example 2.
  • FIG. 1 Referring to FIG. 1, a 2 theta value of the main peak of the particles showed represented a 38.25 (111) 44.35 (200) 64.6 (220) 77.55 (311) to a typical silver pattern may be an oxide of Ag 2 O or AgO It can be seen that is not generated.
  • 2 is a SEM photograph of the silver-sulfur nanocomposite prepared in Example 2.
  • polyvinylpyrrolidone (molecular weight 40,000) is added to 539 g of ethanol and dissolved by heating at 50 ° C.
  • 10 g of 1-mercapto-2-propanol was added to the prepared silver nano colloid, and the reaction was performed for 60 minutes to prepare a silver-sulfur nanocomposite colloid in which silver particles and sulfur were combined.
  • the antimicrobial activity of the three prepared master batches was measured by the method described above, and the results using Staphylococcus aureus, ATCC 6538 are shown in Table 1 below, and the results using Escherichia coli, ATCC 25922 are shown in Table 2 below.
  • Example 1 Example 2
  • Example 3 Initial bacterial count of control sample 3.5 x 10 5 After 24 hours incubation 3.1 x 10 6 Number of bacteria in test sample after incubation for 24 hours ⁇ 10 ⁇ 10 6.5 x 10 3 Bacteriostatic reduction rate (%) 99.9 99.9 99.8
  • Example 1 Example 2
  • Example 3 Initial bacterial count of control sample 1.3 x 10 6 After 24 hours incubation 5.7 x 10 7 Number of bacteria in test sample after incubation for 24 hours ⁇ 10 ⁇ 10 ⁇ 10 Bacteriostatic reduction rate (%) 99.9 99.9 99.8
  • the silver-sulfur nanocomposite polyester masterbatch prepared in the present invention exhibits excellent antimicrobial activity when exposed to microorganisms.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention porte sur un mélange maître de polyester doté de propriétés antimicrobiennes exceptionnelles et sur un procédé de production dudit mélange maître. L'invention concerne, plus particulièrement, un procédé qui comprend une étape de production d'un nanocomposite d'argent et de soufre renfermant du soufre et une étape de production d'un mélange maître de polyester renfermant ledit nanocomposite. L'invention se rapporte à un mélange maître de polyester destiné aux articles de literie qui possède des propriétés antimicrobiennes et désodorisantes permanentes et, en particulier, qui peut être utilisé dans un tricot de polyester duveté à mailles jetées ultrafin.
PCT/KR2010/008617 2010-12-03 2010-12-03 Mélange maître de polyester doté de propriétés antimicrobiennes exceptionnelles et procédé de production WO2012074153A1 (fr)

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PCT/KR2010/008617 WO2012074153A1 (fr) 2010-12-03 2010-12-03 Mélange maître de polyester doté de propriétés antimicrobiennes exceptionnelles et procédé de production

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105037754A (zh) * 2015-06-26 2015-11-11 上海纳米技术及应用国家工程研究中心有限公司 一种采用浆料法制备功能性聚酯母粒的工艺

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990074216A (ko) * 1998-03-07 1999-10-05 이상진 항균제
KR100535916B1 (ko) * 2005-09-13 2005-12-09 강석주 은나노분말을 이용한 항균섬유의 제조방법
KR100861399B1 (ko) * 2007-12-17 2008-10-02 주식회사 잉크테크 은 나노입자 분산 수지의 제조 방법
JP2010523344A (ja) * 2007-04-04 2010-07-15 パーレン コンヴァーティング アクチェンゲゼルシャフト 抗菌性材料
JP2010530016A (ja) * 2007-06-11 2010-09-02 ビーエーエスエフ ソシエタス・ヨーロピア 抗菌性ポリオレフィン及びポリエステル組成物

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990074216A (ko) * 1998-03-07 1999-10-05 이상진 항균제
KR100535916B1 (ko) * 2005-09-13 2005-12-09 강석주 은나노분말을 이용한 항균섬유의 제조방법
JP2010523344A (ja) * 2007-04-04 2010-07-15 パーレン コンヴァーティング アクチェンゲゼルシャフト 抗菌性材料
JP2010530016A (ja) * 2007-06-11 2010-09-02 ビーエーエスエフ ソシエタス・ヨーロピア 抗菌性ポリオレフィン及びポリエステル組成物
KR100861399B1 (ko) * 2007-12-17 2008-10-02 주식회사 잉크테크 은 나노입자 분산 수지의 제조 방법

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105037754A (zh) * 2015-06-26 2015-11-11 上海纳米技术及应用国家工程研究中心有限公司 一种采用浆料法制备功能性聚酯母粒的工艺
CN105037754B (zh) * 2015-06-26 2017-12-08 上海纳米技术及应用国家工程研究中心有限公司 一种采用浆料法制备功能性聚酯母粒的工艺

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