CN114059110A - Radiation-proof polyester fiber surface treatment method and application - Google Patents
Radiation-proof polyester fiber surface treatment method and application Download PDFInfo
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- CN114059110A CN114059110A CN202111286720.5A CN202111286720A CN114059110A CN 114059110 A CN114059110 A CN 114059110A CN 202111286720 A CN202111286720 A CN 202111286720A CN 114059110 A CN114059110 A CN 114059110A
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- 239000000835 fiber Substances 0.000 title claims abstract description 151
- 229920000728 polyester Polymers 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000004381 surface treatment Methods 0.000 title claims abstract description 30
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- 239000010949 copper Substances 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 38
- 239000003513 alkali Substances 0.000 claims abstract description 35
- 238000009713 electroplating Methods 0.000 claims abstract description 31
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims abstract description 26
- 235000011180 diphosphates Nutrition 0.000 claims abstract description 26
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 21
- 239000011701 zinc Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000012266 salt solution Substances 0.000 claims abstract description 18
- 238000007598 dipping method Methods 0.000 claims abstract description 15
- 239000004753 textile Substances 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000007747 plating Methods 0.000 claims description 20
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 14
- 239000013585 weight reducing agent Substances 0.000 claims description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical compound [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 7
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 7
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract description 9
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 238000007788 roughening Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 230000008569 process Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 238000005406 washing Methods 0.000 description 9
- 239000002585 base Substances 0.000 description 8
- 239000004744 fabric Substances 0.000 description 6
- 239000002759 woven fabric Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 description 4
- 239000002657 fibrous material Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- XEGMDUOAESTQCC-UHFFFAOYSA-N 1-(naphthalen-1-ylmethyl)naphthalene;sodium Chemical compound [Na].C1=CC=C2C(CC=3C4=CC=CC=C4C=CC=3)=CC=CC2=C1 XEGMDUOAESTQCC-UHFFFAOYSA-N 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
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- 238000004519 manufacturing process Methods 0.000 description 3
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920005594 polymer fiber Polymers 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical group [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 238000000861 blow drying Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- LCRMGUFGEDUSOG-UHFFFAOYSA-N naphthalen-1-ylsulfonyloxymethyl naphthalene-1-sulfonate;sodium Chemical group [Na].C1=CC=C2C(S(=O)(OCOS(=O)(=O)C=3C4=CC=CC=C4C=CC=3)=O)=CC=CC2=C1 LCRMGUFGEDUSOG-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
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- 238000007738 vacuum evaporation Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Automation & Control Theory (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to the technical field of textile surface treatment, and particularly discloses a radiation-proof polyester fiber surface treatment method and application. The polyester fiber surface treatment method comprises the following steps: putting the polyester fiber in an alkali solution for alkali decrement heat treatment to obtain a pretreated polyester fiber; putting the pretreated polyester fiber into a metal salt solution for zinc dipping treatment to obtain zinc dipped polyester fiber; and (3) placing the zinc-dipped polyester fiber in pyrophosphate electroplating solution for electro-coppering treatment to obtain the copper-plated polyester fiber. Firstly, through alkali decrement heat treatment, micro pits or micro gaps are formed on the smooth surface of the polyester fiber, so that the effects of oil removal and roughening are achieved; then, the zinc dipping and the copper electroplating treatment are carried out to realize the omnibearing adsorption of metal ions and form a compact metal coating film, thereby improving the applicability of the product and the stability of the product quality. The prepared polyester fiber has the square resistance of about 0.05 omega, has good conductive performance, and can meet the scene with higher radiation protection requirements.
Description
Technical Field
The invention belongs to the technical field of textile surface treatment, and particularly relates to a radiation-proof polyester fiber surface treatment method and application.
Background
Modern life and production do not leave various electrical equipment, and electromagnetic radiation generated by the operation of electrical equipment affects instruments and equipment and also causes harm to human bodies, so that electromagnetic radiation protection is more and more a focus of attention of people. The polymer fiber material can realize the best flexible carrier with the electromagnetic shielding function, and the fiber material is subjected to special function finishing, so that the fiber can keep the original excellent wearability such as softness, folding resistance and the like, has unique electromagnetic characteristics, and has wide application value in the fields of life, production and military affairs. The metallization treatment is one of the important means for realizing the electromagnetic protection function of the polymer fiber material, and can be realized by vacuum plating, sputtering plating, chemical plating and other modes. Wherein: the vacuum coating is carried out in a vacuum evaporation coating mode by means of an electron beam heating mode, has the advantages of concentrated energy, controllable and adjustable evaporation temperature and high film forming quality, and is an important surface treatment mode for inorganic materials and high polymer materials. On the basis of vacuum coating research, the method for sputtering and coating the textile material on the surfaces of fiber materials with different forming structures by using an electron beam evaporation deposition method is the most widely researched method at present, and the product has the characteristics of strong friction resistance and is applied to sun-proof fabrics. The chemical plating mode is mainly applied to metal material electroplating, the temperature of the common processing technology is higher, and the temperature resistance of textile fibers is generally below 150 ℃, so that the chemical plating mode is less applied to textiles.
Various polyester fibers in the current market have higher requirements on pretreatment, and have more types of spinning additives, if pretreatment work does not completely remove substances influencing alkali decrement on the fiber surface or subsequent zinc-plated copper processing, copper spots can occur on the fiber surface, namely copper is normally plated on some places, the thickness of a copper film on some places is not up to standard, and even the copper film phenomenon is not generated on some places. Meanwhile, polyester products processed by the prior zinc-dipping and copper-plating processes can basically meet the requirements of building inner wall bedding base materials which need common protection, radiation protection and shielding levels, namely common civil requirements; but the radiation protection requirement is higher when the method is applied to some products, such as transformer substation generator rooms, computer data centers and base material fiber structures for medical radiology departments, the fabric density and the copper film thickness need to be improved, profiled fibers, superfine fibers and high-density fabrics need to be adopted as base materials for the products, and a sulfate copper plating process is added after a pyrophosphate copper electroplating process, so that the copper film thickness and uniformity are further improved, and the durability and the use safety are ensured.
Disclosure of Invention
The invention provides a radiation-proof polyester fiber surface treatment method and application, which are used for solving one or more technical problems in the prior art and at least providing a beneficial choice or creation condition.
In order to overcome the technical problems, the invention provides a polyester fiber surface treatment method in a first aspect
Specifically, the polyester fiber surface treatment method comprises the following steps:
(1) putting the polyester fiber in an alkali solution for alkali decrement heat treatment to obtain a pretreated polyester fiber;
(2) putting the pretreated polyester fiber into a metal salt solution for zinc dipping treatment to obtain zinc dipped polyester fiber;
(3) and (3) placing the zinc-dipped polyester fiber in pyrophosphate electroplating solution for electro-coppering treatment to obtain the copper-plated polyester fiber.
The polyester fiber surface treatment method of the present invention is a method for treating a polyester fiber surface, comprising the steps of, first, subjecting a polyester fiber to alkali weight reduction heat treatment in an alkali solution, wherein the alkali weight reduction heat treatment of the present invention is: polyester fiber is hydrolyzed in ester bond under the action of hot alkali solution and is easy to react in weak places, namely alkali decrement reaction, so that micro pits or micro gaps are formed on the smooth surface, the effects of oil removal and roughening treatment can be effectively achieved, meanwhile, the fineness and the activity of the fiber are improved, and the strength and the weight are reduced. Therefore, the alkali weight reduction heat treatment is used for removing spinning oil, antistatic agent and the like introduced in the polyester fiber processing on one hand, so that the fiber surface is clean; on the other hand, the surface roughening treatment is carried out by utilizing the characteristic that the polyester fiber is not alkali-resistant, and the thickness of the fiber is reduced simultaneously, so that the permeability of the fiber to a metal salt solution and a pyrophosphate electroplating solution in the processes of zinc immersion and copper electroplating in the next procedure is improved, and a foundation is laid for the full coverage of a plating layer in the next procedure; then, putting the pretreated polyester fiber into a metal salt solution for zinc dipping treatment so as to form a continuous zinc dipping layer on the surface of the substrate of the polyester fiber; and finally, placing the zinc-dipped polyester fiber in pyrophosphate electroplating solution for copper electroplating treatment, and electrifying the pyrophosphate electroplating solution to generate ion adsorption so as to adsorb copper on the surface of the polyester fiber, thereby realizing omnibearing adsorption of metal ions and forming a compact metal coating, thereby improving the applicability and quality stability of the product.
Furthermore, before the pre-treatment of the polyester fiber, the steps of hot water washing and acetic acid neutralization tap water washing are sequentially carried out, so that the residual alkali solution in the alkali decrement heat treatment process is washed clean.
Further, before the copper-plated polyester fiber is treated, the zinc-dipped polyester fiber further comprises the steps of washing with tap water and washing with distilled water, so that the metal salt solution remained in the zinc dipping treatment process is washed clean.
Further, after the galvanized polyester fiber is subjected to electrolytic copper plating treatment, the method also comprises the steps of tap water cleaning, sulfuric acid activation, room temperature water washing and cold air blow drying.
As a further improvement of the scheme, the raw material components of the alkali solution in the step (1) comprise: 20-30g/L of sodium hydroxide, 0.5-2g/L of accelerator and 0.5-2g/L of alkaline dispersant.
Preferably, the accelerator is selected from dodecyl dimethyl benzyl ammonium chloride, and the alkaline dispersant is selected from sodium methylene bis-naphthalene sulfonate.
Further, the treatment temperature of the alkali weight reduction heat treatment in the step (1) is 80-85 ℃; the treatment time is 30-45 minutes.
As a further improvement of the scheme, the raw material components of the metal salt solution in the step (2) comprise: 20-30g/L of zinc oxide, 2-8g/L of sodium hydroxide, 150g/L of ferric chloride, 0.5-1g/L of nickel chloride and 0.5-1g/L of copper chloride.
Further, the treatment temperature of the zinc dipping treatment in the step (2) is room temperature; the treatment time is 15-50 seconds.
As a further improvement of the above scheme, the raw material components of the pyrophosphate electroplating bath in the step (3) include: 30-50g/L of copper pyrophosphate, 280g/L of potassium pyrophosphate and 20-25g/L of ammonium citrate;
further, the pH value of the pyrophosphate electroplating solution in the step (3) is 8-9.
Further, the temperature of the electrolytic copper plating treatment in the step (3) is 40 to 45 ℃.
Further, the electro-coppering treatment in the step (3) has a current density of 1.3-1.6A/dm2。
Preferably, a polyester fiber surface treatment method comprises the following steps:
(1) firstly, placing polyester fiber in an alkali solution with the temperature of 80-85 ℃ for 30-45 minutes, wherein the alkali solution is prepared by 20-30g/L of sodium hydroxide, 0.5-2g/L of accelerant and 0.5-2g/L of alkaline dispersing agent; then, the polyester fiber is washed by water with the temperature of 50-60 ℃ for 3 minutes and neutralized by 2 percent acetic acid; finally, washing the fiber with water at 50-60 ℃ for 1 minute to obtain pretreated polyester fiber;
(2) firstly, putting the pretreated polyester fiber into a metal salt solution at room temperature for zinc dipping treatment for 15-50 seconds, wherein the metal salt solution consists of 20-30g/L of zinc oxide, 2-8g/L of sodium hydroxide, 150g/L of ferric chloride, 0.5-1g/L of nickel chloride and 0.5-1g/L of copper chloride; then drying the polyester fiber at the temperature of 130-150 ℃ until no water drops, thus obtaining the zinc-impregnated polyester fiber;
(3) the zinc-dipped polyester fiber is placed in pyrophosphate electroplating solution with the temperature of 40-45 ℃ for electro-coppering treatment, and the current density is controlled to be 1.3-1.6A/dm2Adsorbing copper to the surface of the polyester fiber, wherein the pyrophosphate electroplating solution consists of 30-50g/L of copper pyrophosphate, 280g/L of potassium pyrophosphate and 20-25g/L of ammonium citrate, and the pH value of the pyrophosphate electroplating solution is 8-9, so that 1.8-2.2 mu m of copper is adsorbed to the surface of the polyester fiber, and the copper-plated polyester fiber is obtained.
The second aspect of the invention provides an application of a polyester fiber surface treatment method.
Specifically, the textile is prepared by adopting the polyester fiber surface treatment method, and the prepared textile can meet scenes with high radiation protection requirements, such as transformer substation generator rooms, computer data centers, wall surfaces for medical radiology departments and the like, and can also be used as building base materials or wall cloth, carpets, curtains and the like.
Compared with the prior art, the technical scheme of the invention at least has the following technical effects or advantages:
firstly, through alkali decrement heat treatment, micro pits or micro gaps are formed on the smooth surface of the polyester fiber, so that the effects of oil removal and roughening are achieved; then zinc dipping and copper electroplating are carried out under the specific solution neutralization process condition to realize omnibearing adsorption of metal ions and form a compact metal coating film, thereby improving the applicability of the product and the stability of the product quality. The prepared polyester fiber has the square resistance of about 0.05 omega, has good conductive performance, maintains the original flexibility and folding resistance of the fiber, and can meet scenes with higher radiation protection requirements, such as transformer substation generator rooms, computer data centers, base materials for medical radiology departments and the like.
The polyester fiber surface treatment method can realize a continuous processing mode, effectively improve the production efficiency and the quality stability, save the energy consumption and reduce the processing cost, and the process formula is not limited by the use environment and has strong applicability.
Drawings
FIG. 1 is an SEM topography of the polyester fiber of example 1 before alkali weight reduction heat treatment;
FIG. 2 is a first SEM topography after alkali weight loss heat treatment of the polyester fiber of example 1;
FIG. 3 is a second SEM topography after alkali weight loss heat treatment of the polyester fiber of example 1;
FIG. 4 is an SEM topography of the polyester fiber of example 1 after copper plating;
FIG. 5 is a graph showing the spectrum of the polyester fiber of example 1 after copper plating.
Detailed Description
The present invention is described in detail below by way of examples to facilitate understanding of the present invention by those skilled in the art, and it is to be specifically noted that the examples are provided only for the purpose of further illustrating the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
A polyester fiber surface treatment method comprises the following steps:
(1) firstly, placing the polyester fiber polyester woven fabric in an alkaline solution at the temperature of 80 ℃ for 30 minutes, wherein: the alkali solution is prepared by 20g/L of sodium hydroxide, 0.5g/L of promoter dodecyl dimethyl benzyl ammonium chloride and 0.5g/L of alkaline dispersant methylene dinaphthalene sodium sulfonate; then, the polyester fiber is washed by water with the temperature of 50 ℃ for 3 minutes and neutralized by 2 percent acetic acid; finally, washing the fiber with water at 50 ℃ for 1 minute to obtain pretreated polyester fiber;
(2) the method comprises the following steps of firstly, putting the pretreated polyester fiber into a metal salt solution at room temperature for zinc dipping for 15 seconds, wherein: the metal salt solution consists of 20g/L of zinc oxide, 2g/L of sodium hydroxide, 150g/L of ferric chloride, 0.5g/L of nickel chloride and 0.5g/L of copper chloride; drying the polyester fiber at 130 ℃ until no water drops, thereby obtaining zinc-impregnated polyester fiber;
(3) the zinc-dipped polyester fiber is placed in pyrophosphate electroplating solution at 40 ℃ for electro-coppering treatment, and the current density is controlled to be 1.3A/dm2Adsorbing copper to the surface of the polyester woven fabric, wherein: the pyrophosphate electroplating solution is composed of 30g/L of copper pyrophosphate, 250g/L of potassium pyrophosphate and 20g/L of ammonium citrate, the pH value of the pyrophosphate electroplating solution is 8, so that 1.8 mu m of copper is adsorbed on the surface of the polyester fiber, and a finished product of the copper-plated polyester fiber is obtained, the sheet resistance of the finished product is 0.048 omega, the finished product has good conductivity, the original flexibility and folding resistance of the fiber are maintained, and scenes with high radiation protection requirements, such as transformer substation generator rooms, computer data centers and base materials for medical radiology departments, can be met.
Example 2
A polyester fiber surface treatment method comprises the following steps:
(1) firstly, placing the polyester fiber polyester woven fabric in an alkaline solution at the temperature of 82 ℃ for 40 minutes, wherein: the alkali solution is prepared by 25g/L of sodium hydroxide, 1g/L of promoter dodecyl dimethyl benzyl ammonium chloride and 1g/L of alkaline dispersant methylene dinaphthalene sodium sulfonate; then, the polyester fiber is washed by water with the temperature of 55 ℃ for 3 minutes and neutralized by 2 percent acetic acid; finally, washing the fiber with water at 55 ℃ for 1 minute to obtain pretreated polyester fiber;
(2) the method comprises the following steps of firstly, putting the pretreated polyester fiber into a metal salt solution at room temperature for zinc dipping treatment for 30 seconds, wherein: the metal salt solution consists of 25g/L of zinc oxide, 6g/L of sodium hydroxide, 160g/L of ferric chloride, 0.8g/L of nickel chloride and 0.8g/L of copper chloride; drying the polyester fiber at 140 ℃ until no water drops, thereby obtaining zinc-impregnated polyester fiber;
(3) the zinc-dipped polyester fiber is placed in pyrophosphate electroplating solution at 42 ℃ for electrolytic copper plating treatment, and the current density is controlled to be 1.5A/dm2Adsorbing copper to the surface of the polyester fiber, wherein: the pyrophosphate electroplating solution is composed of 40g/L copper pyrophosphate, 260g/L potassium pyrophosphate and 22g/L ammonium citrate, the pH value of the pyrophosphate electroplating solution is 8.5, so that 2.0 mu m copper is adsorbed on the surface of the polyester fiber, and a finished product of the copper-plated polyester fiber is obtained, the sheet resistance of the finished product is 0.05 omega, the copper-plated polyester fiber has good conductivity, the original flexibility and folding resistance of the fiber are maintained, and scenes with high radiation protection requirements, such as transformer substation generator rooms, computer data centers and substrates for medical radiology departments, can be met.
Example 3
A polyester fiber surface treatment method comprises the following steps:
(1) firstly, placing the polyester fiber polyester woven fabric in an alkaline solution at the temperature of 85 ℃ for 45 minutes, wherein: the alkali solution is prepared by 30g/L of sodium hydroxide, 2g/L of promoter dodecyl dimethyl benzyl ammonium chloride and 2g/L of alkaline dispersant methylene dinaphthalene sodium sulfonate; then, the polyester fiber is washed by water with the temperature of 60 ℃ for 3 minutes and neutralized by 2 percent acetic acid; finally, washing the fiber with water at 60 ℃ for 1 minute to obtain pretreated polyester fiber;
(2) the pre-treated polyester fiber is placed in a metal salt solution at room temperature for zinc dipping treatment for 50 seconds, wherein: the metal salt solution consists of 30g/L of zinc oxide, 8g/L of sodium hydroxide, 180g/L of ferric chloride, 1g/L of nickel chloride and 1g/L of copper chloride; drying the polyester fiber at 150 ℃ until no water drops, thereby obtaining zinc-impregnated polyester fiber;
(3) the zinc-dipped polyester fiber is placed in pyrophosphate electroplating solution at 45 ℃ for electro-coppering treatment, and the current density is controlled to be 1.6A/dm2Adsorbing copper to the surface of the polyester fiber, wherein: the pyrophosphate electroplating solution is composed of 50g/L of copper pyrophosphate, 280g/L of potassium pyrophosphate and 25g/L of ammonium citrate, the pH value of the pyrophosphate electroplating solution is 9, so that 2.2 mu m of copper is adsorbed on the surface of the polyester fiber, and a finished product of the copper-plated polyester fiber is obtained, the sheet resistance of the finished product is 0.049 omega, the finished product has good conductivity, the original flexibility and folding resistance of the fiber are maintained, and scenes with high radiation protection requirements, such as transformer substation generator rooms, computer data centers and substrates for medical radiology departments, can be met.
Comparative example 1
A polyester fiber surface treatment method comprises the following steps:
(1) firstly, putting polyester fiber polyester woven fabric into a metal salt solution at room temperature for zinc dipping treatment for 15 seconds, wherein: the metal salt solution consists of 20g/L of zinc oxide, 2g/L of sodium hydroxide, 150g/L of ferric chloride, 0.5g/L of nickel chloride and 0.5g/L of copper chloride; drying the polyester fiber at 130 ℃ until no water drops, thereby obtaining zinc-impregnated polyester fiber;
(2) the zinc-dipped polyester fiber is placed in pyrophosphate electroplating solution at 40 ℃ for electro-coppering treatment, and the current density is controlled to be 1.3A/dm2Adsorbing copper to the surface of the polyester woven fabric, wherein: the pyrophosphate electroplating solution is composed of 30g/L of copper pyrophosphate, 250g/L of potassium pyrophosphate and 20g/L of ammonium citrate, the pH value of the pyrophosphate electroplating solution is 8, and copper with the diameter of 1.8 mu m is adsorbed on the surface of the polyester fiber, so that a finished product of the copper-plated polyester fiber is obtained.
Comparative example 1 differs from example 1 in that: the polyester fiber of comparative document 1 was not subjected to the alkali weight reduction heat treatment, and the zinc-impregnation and copper-plating process conditions were the same as in example 1. The square resistance of the prepared finished product is 0.069 omega, the phenomenon that the plating layer is discontinuous in some places due to too small space between fibers, the plating layer is easy to fall off and the like occurs, the radiation-proof effect is not good, and the radiation-proof shielding grade can only meet the common civil protection radiation-proof shielding grade, such as building inner wall bedding base materials and the like; the material cannot be applied to scenes with high radiation protection requirements, such as transformer substation generator rooms, computer data centers, base materials for medical radiology departments and the like.
And (3) microstructure analysis:
the polyester fibers of example 1 at various stages of the process were observed under a scanning electron microscope, and the results are shown in FIGS. 1 to 4.
As can be seen from fig. 1, the surface of the polyester fiber before the alkali weight reduction heat treatment is smooth and flat, and the arrangement between yarns and between fibers is tight.
As can be seen from FIG. 2, after the polyester fiber is subjected to alkali weight reduction heat treatment, the spinning oil on the surface of the fiber is removed, and chemical corrosion is generated, so that the polyester fiber is obviously thinned.
Further, when the polyester fiber after the alkali weight reduction heat treatment is observed in an enlarged manner, as can be seen from fig. 3, the surface of the fiber becomes rough, and many micro pits and micro gaps are formed, so that the specific surface of the whole fiber is increased, and the adhesion of a zinc layer is facilitated.
As can be seen from fig. 4, the polyester fiber surface after being subjected to zinc immersion and copper plating forms a film layer, the copper film uniformly covers gaps between yarns and between visual fibers, the texture and texture are weakened, the fabric after alkali decrement treatment is subjected to zinc immersion and copper plating treatment, a compact plated film is formed on the surface, and the plated layer not only covers the surface of the fabric, but also penetrates into gaps between the yarns and the fibers. It was found through experiments that the thickness of the copper film would increase with time. As shown in fig. 5, the elemental composition of the fiber surface after coating was analyzed by an energy spectrum analyzer carried by a scanning electron microscope, and it was found that the film layer was mainly composed of copper and also contained a part of oxygen (hydrogen could not be measured by the energy spectrum analyzer), indicating that the polyester fiber was subjected to the zincification and copper plating processes, the fiber surface formed a copper film with a certain thickness, and the copper film was uniformly covered between the fibers and in the gaps; the oxygen element in the detection result is copper oxide which is generated by the oxidation with air after the copper film is formed.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are intended to be within the scope of the invention.
Claims (10)
1. A polyester fiber surface treatment method is characterized by comprising the following steps:
(1) putting the polyester fiber in an alkali solution for alkali decrement heat treatment to obtain a pretreated polyester fiber;
(2) putting the pretreated polyester fiber into a metal salt solution for zinc dipping treatment to obtain zinc dipped polyester fiber;
(3) and (3) placing the zinc-dipped polyester fiber in pyrophosphate electroplating solution for electro-coppering treatment to obtain the copper-plated polyester fiber.
2. The surface treatment method of polyester fiber according to claim 1, wherein the raw material components of the alkali solution in step (1) comprise: 20-30g/L of sodium hydroxide, 0.5-2g/L of accelerator and 0.5-2g/L of alkaline dispersant.
3. The surface treatment method for polyester fiber according to claim 1 or 2, wherein the treatment temperature of the alkali weight reduction heat treatment in step (1) is 80 to 85 ℃; the treatment time is 30-45 minutes.
4. The surface treatment method for polyester fiber according to claim 1, wherein the raw material composition of the metal salt solution in the step (2) comprises: 20-30g/L of zinc oxide, 2-8g/L of sodium hydroxide, 150g/L of ferric chloride, 0.5-1g/L of nickel chloride and 0.5-1g/L of copper chloride.
5. The surface treatment method of polyester fiber according to claim 1 or 4, wherein in the step (2), the treatment temperature of the zincating treatment is room temperature; the treatment time is 15-50 seconds.
6. The method for surface treatment of polyester fiber according to claim 1, wherein the pyrophosphate electroplating solution of step (3) comprises the following raw material components: 30-50g/L of copper pyrophosphate, 280g/L of potassium pyrophosphate and 20-25g/L of ammonium citrate.
7. The method for surface treatment of polyester fiber according to claim 6, wherein the pH of the pyrophosphate electroplating solution in step (3) is 8 to 9.
8. The surface treatment method of polyester fiber according to claim 1 or 6, wherein the temperature of the electrolytic copper plating treatment in step (3) is 40-45 ℃.
9. The surface treatment method of polyester fiber according to claim 8, wherein the electro-coppering treatment in the step (3) has a current density of 1.3-1.6A/dm2。
10. A textile article, characterized by: the textile is manufactured by the polyester fiber surface treatment method according to any one of claims 1 to 9.
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