CN117866529B - Nickel screen coating material, printed nickel screen, and preparation method and application thereof - Google Patents
Nickel screen coating material, printed nickel screen, and preparation method and application thereof Download PDFInfo
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- CN117866529B CN117866529B CN202410264446.9A CN202410264446A CN117866529B CN 117866529 B CN117866529 B CN 117866529B CN 202410264446 A CN202410264446 A CN 202410264446A CN 117866529 B CN117866529 B CN 117866529B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 557
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 275
- 239000011248 coating agent Substances 0.000 title claims abstract description 68
- 238000000576 coating method Methods 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 105
- 239000002184 metal Substances 0.000 claims abstract description 75
- 229910052751 metal Inorganic materials 0.000 claims abstract description 75
- 229920001721 polyimide Polymers 0.000 claims abstract description 52
- 239000004642 Polyimide Substances 0.000 claims abstract description 50
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000006104 solid solution Substances 0.000 claims abstract description 45
- 239000011159 matrix material Substances 0.000 claims abstract description 39
- 239000000956 alloy Substances 0.000 claims abstract description 32
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 32
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 29
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 150000004985 diamines Chemical class 0.000 claims abstract description 12
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 21
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 125000006158 tetracarboxylic acid group Chemical group 0.000 claims description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 11
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 239000011247 coating layer Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- NOGFHTGYPKWWRX-UHFFFAOYSA-N 2,2,6,6-tetramethyloxan-4-one Chemical compound CC1(C)CC(=O)CC(C)(C)O1 NOGFHTGYPKWWRX-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 6
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004305 biphenyl Substances 0.000 claims description 6
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000006068 polycondensation reaction Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000004753 textile Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 5
- VDQQJMHXZCMNMU-UHFFFAOYSA-N 1-phenylpyrrolidine Chemical compound C1CCCN1C1=CC=CC=C1 VDQQJMHXZCMNMU-UHFFFAOYSA-N 0.000 claims description 5
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- CURJNMSGPBXOGK-UHFFFAOYSA-N n',n'-di(propan-2-yl)ethane-1,2-diamine Chemical compound CC(C)N(C(C)C)CCN CURJNMSGPBXOGK-UHFFFAOYSA-N 0.000 claims description 4
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 3
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract description 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 description 11
- HZONRRHNQILCNO-UHFFFAOYSA-N 1-methyl-2h-pyridine Chemical compound CN1CC=CC=C1 HZONRRHNQILCNO-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000006482 condensation reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004970 Chain extender Substances 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000006297 carbonyl amino group Chemical group [H]N([*:2])C([*:1])=O 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009965 tatting Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention provides a nickel screen coating material, a printed nickel screen, a preparation method and application thereof, wherein the nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: an organic solvent, a triisocyanate modified anhydride, a diamine monomer, a catalyst and a dehydrating agent; the preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, reacting dianhydride monomer, triisocyanate and dimethylformamide for 3-5 hours at 100-150 ℃; the printing nickel screen comprises a printing nickel screen matrix and a nickel screen coating material coated on the printing nickel screen matrix; the printed nickel screen matrix comprises a printed nickel screen substrate and a nickel/metal M solid solution alloy layer on the solid solution surface, wherein the metal M is one or a mixture of a plurality of metals Cr or Mo, or the printed nickel screen substrate is the printed nickel screen substrate. The invention solves the problems of poor interfacial binding force between polyimide and a printed nickel screen substrate, easy stripping of a coating and the like in the prior art.
Description
Technical Field
The invention relates to the technical field of nickel screen coating materials, in particular to a nickel screen coating material, a printed nickel screen, and a preparation method and application thereof.
Background
In the textile industry, environmental factors of the printing process, such as acid-base environment, high temperature and abrasion, often lead to accumulation of nickel residues on the printed fabric, because the acid-base environment promotes release of nickel ions from the printed nickel screen during printing, and further adheres to the fabric, and the high temperature and abrasion exacerbate the phenomenon. These nickel metal residues have a certain stimulating effect on the skin mucosa and respiratory tract of human body, and constitute a potential threat to health. Therefore, how to treat the nickel residue on the printed fabric becomes a hard problem in the industry.
In order to solve this problem, polyimide in the field of polymer materials is becoming a focus of research. Polyimide has excellent acid and alkali resistance, high temperature resistance and wear resistance, and can cope with various challenges in the printing process. The acid and alkali resistance can ensure that the product can be kept stable in an acid and alkali environment and is not corroded. Meanwhile, the high temperature resistance makes polyimide not easy to degrade in high temperature treatment. The wear resistance of the fabric can effectively reduce the wear of the fabric in the use process, and the risk of nickel residue is reduced. Therefore, polyimide has potential application value in treating nickel residues on the printing and dyeing fabric.
However, despite the many advantages of polyimide in the coating field, there are still some challenges as a printed nickel screen coating. Firstly, polyimide has high shrinkage, and the shrinkage mismatch of polyimide and a printed nickel screen substrate can cause interfacial peeling or separation phenomenon, so that a coating layer can fail under a high-temperature or high-stress environment, and effective protection cannot be provided for a metal substrate; second, the interfacial compatibility between polyimide and metal is to be improved, resulting in an insufficiently stable bond between the coating and the metal substrate, which may lead to peeling, cracking or peeling of the coating during use, thereby degrading its protective properties.
In order to improve the performance and stability of polyimide as a printing nickel screen coating material, it is important to further solve the problems, and meet wider application requirements.
Disclosure of Invention
The invention provides a nickel screen coating material, a printed nickel screen, a preparation method and application thereof, and solves the problems of poor interfacial binding force between polyimide and a printed nickel screen substrate, easy stripping of a coating and the like in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
The nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: 80-140 parts of organic solvent, 20-50 parts of triisocyanate modified anhydride, 18-50 parts of diamine monomer, 2-5 parts of catalyst and 2-4 parts of dehydrating agent;
The preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, reacting dianhydride monomer, triisocyanate and dimethylformamide for 3-5 hours at 100-150 ℃ to obtain triisocyanate modified anhydride, wherein the mass ratio of the dianhydride monomer to the triisocyanate to the dimethylformamide is 5-25: 5-30: 50-75.
The invention adopts triisocyanate as a chain extender, the triisocyanate contains three isocyanate groups, can be subjected to condensation reaction with dianhydride monomers to generate an amide ester structure (CONH), and can gradually prolong the chain length of a polymer precursor through the steps of condensation reaction and chain extension to form a macromolecular precursor. The raw materials are matched, so that the shrinkage rate and the linear expansion coefficient of the prepared polyimide are reduced, and the interface binding force and the performance of the coating are improved.
Preferably, the diamine monomer is one or more of m-phenylenediamine, p-xylylenediamine and p-phenylenediamine.
Preferably, the catalyst is one or more of trimethylamine, N-diethyl ethylenediamine, N-phenylpyrrolidine and N, N-diisopropyl ethylenediamine;
the dehydrating agent is one or more of benzoic anhydride and phthalic anhydride.
Preferably, the dianhydride monomer is one or more of 3,3', 4' -diphenyl tetracarboxylic dianhydride and 3,3', 4' -diphenyl sulfone tetracarboxylic dianhydride.
The addition of the catalyst and the dehydrating agent can solidify the polyimide film at low temperature and improve the interface combination of the film and the printed nickel screen substrate.
As a general inventive concept, the present invention provides a method for preparing a nickel mesh coating layer material, comprising the steps of: under the protection of nitrogen, placing triisocyanate modified anhydride and diamine monomer into an organic solvent, uniformly stirring, performing polycondensation reaction at 20-40 ℃ for 1-2 h, adding a catalyst and a dehydrating agent, stirring for 2-4 h, performing defoaming treatment by ultrasonic for 30min, coating on the surface of a printing nickel screen matrix, and performing curing treatment in a vacuum drying oven at each temperature point of 100 ℃, 150 ℃ and 250 ℃ for 2 h.
The cured polyimide has multiple functions in the textile printing process. First, the cured polyimide forms a high strength cross-linked structure that enhances the mechanical strength and abrasion resistance of the printed fabric, enabling it to withstand longer use and washing. In addition, polyimide has higher chemical stability, can resist the erosion of chemical substances, prolongs the service life of the fabric, and the film formed by the cured polyimide has the characteristics of smoothness and softness.
As a general inventive concept, the present invention provides a printed nickel screen, which includes a printed nickel screen substrate and a nickel screen coating material coated on the printed nickel screen substrate, wherein the nickel screen coating material is the nickel screen coating material or the nickel screen coating material prepared by the preparation method; the printing nickel screen matrix comprises a printing nickel screen substrate and a nickel/metal M solid solution alloy layer which is solid-solution on the surface of the printing nickel screen substrate, wherein the metal M is one or a mixture of a plurality of metals Cr or Mo, or the printing nickel screen matrix is the printing nickel screen substrate.
According to the invention, the nickel/metal M solid solution alloy layer is formed on the surface of the printed nickel screen substrate in a solid solution manner, so that the compatibility of the printed nickel screen substrate and polyimide can be improved, and the interface combination can be enhanced. Through solid solution of metal Cr or metal Mo elements, a solid solution alloy layer is formed on the surface of the printed nickel screen substrate, and the solid solution of the metal Cr or metal Mo elements also improves the electronic structure of the surface of the printed nickel screen substrate, so that the printed nickel screen substrate is more active, and the interface interaction with polyimide is enhanced. The interfacial interaction improves the adsorption capacity of the polyimide film on the surface of the printed nickel screen substrate, and further enhances the interfacial combination of polyimide and the printed nickel screen substrate.
Preferably, the thickness of the nickel/metal M solid solution alloy layer is 20-30 nm, and the solid solubility of the metal M in the nickel/metal M solid solution alloy layer is 25-50%;
the thickness of the nickel screen coating layer material is 5-20 mu m;
Preferably, the preparation method of the printed nickel screen matrix comprises the following steps: and (3) magnetically sputtering a metal M layer with the thickness of 5-15 nm on the surface of the printed nickel screen substrate by adopting a magnetron sputtering method, and then performing heat treatment for 1-2 hours at the temperature of 1200-1400 ℃ in a hydrogen environment, wherein the metal M in the metal M layer and nickel element in the printed nickel screen substrate form a nickel/metal M solid solution alloy layer, so as to obtain the printed nickel screen substrate.
Preferably, the printed nickel screen substrate is a pretreated printed nickel screen substrate, and the pretreatment comprises the following steps: respectively ultrasonically cleaning the printed nickel screen substrate by using acetone and deionized water for 5-10 min to remove surface impurities; then, immersing the printed nickel screen substrate in a mixed solution of 20% hydrofluoric acid and 25% nitric acid in a volume ratio of 1:1 for 10-20 min, and polishing to remove an oxide layer;
As a general inventive concept, the present invention provides a method of preparing a printed nickel screen, comprising the steps of: placing the printing nickel screen matrix into a mixed solution of organic amine and toluene with the volume ratio of (10-50) 100 for reaction for 5-10 hours, and then cleaning with deionized water to obtain the printing nickel screen matrix subjected to amino grafting treatment; coating a nickel screen coating material on the surface of the printing nickel screen substrate subjected to the amino grafting treatment;
the organic amine is one or more of triethylamine, isopropylamine and ethylenediamine.
The purpose of the invention that the surface of the nickel/metal M solid solution alloy layer adopts amino grafting treatment is as follows: through amino grafting treatment, the active site on the surface of the nickel/metal M solid solution alloy layer can be increased, the compatibility with the polyimide layer is improved, and the interface binding force is enhanced. The amino group and the triisocyanate modified anhydride and the diamine monomer in the polyimide layer can form a chemical bond with stronger affinity, so that the amino grafting treatment can enhance the binding force between the polyimide layer and the printing nickel screen substrate, and the adhesiveness and durability of the coating layer are improved.
As a general inventive concept, the invention provides an application of the printed nickel screen or the printed nickel screen prepared by the preparation method in a textile printing process.
The beneficial effects of the invention are as follows:
1. The invention uses the triisocyanate modified anhydride as the chain extender to modify the diamine monomer, and gradually forms macromolecular polyimide through condensation reaction and chain extension steps, the polyimide has low shrinkage and low linear expansion coefficient, and the polyimide is used as a coating and is not easy to be stripped or separated from a printing nickel screen substrate, and has higher interface binding force.
2. In the invention, metallic Cr or metallic Mo element is solid-dissolved on the surface of the printed nickel screen substrate to form a solid solution alloy layer, so that the compatibility of the printed nickel screen substrate and polyimide is improved, and the interface combination is enhanced. In addition, the invention can promote the grafting of amino groups on the surface by forming a layer of nickel/metal M solid solution alloy layer on the surface of the printed nickel screen substrate in a solid solution manner, thereby enhancing interface bonding.
3. The surface of the nickel/metal M solid solution alloy layer is subjected to amino grafting treatment, so that the compatibility of the printing nickel screen matrix and the polyimide layer is improved, and the interface binding force is enhanced.
4. The printed nickel screen has the characteristics of corrosion resistance, wear resistance and durability, and has the performance advantages of greatly reducing nickel residual index, greatly increasing recycling times and remarkably improving service life; the printed nickel screen can continuously print a tatting pigment printing order of 30000 meters, and can ensure that the nickel residue value of a treated printed fabric sample is kept below 0.30ppm and is far lower than that of a common printed rotary screen by 200-300 ppm.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope topography of a magnetron sputtered metal Cr layer on the surface of a printed nickel screen substrate in example 5 of the present invention;
FIG. 2 is a diagram showing the elemental distribution of a metal Cr layer magnetron sputtered on the surface of a printed nickel screen substrate, heat treated, and then dissolved in the metal layer in example 5 of the present invention;
FIG. 3 is an electron microscopic view of a nickel screen coating material coated on the surface of a printed nickel screen substrate in example 5 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
The nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: 120 parts of dimethylformamide, 50 parts of triisocyanate modified anhydride, 42 parts of m-phenylenediamine, 2 parts of trimethylamine and 2 parts of benzoic anhydride;
the preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, 3', 4' -diphenyl tetracarboxylic dianhydride, triisocyanate and dimethylformamide are reacted for 3 hours at 150 ℃ to obtain triisocyanate modified anhydride, wherein the mass ratio of the 3,3', 4' -diphenyl tetracarboxylic dianhydride, triisocyanate and dimethylformamide is 15:20:60.
The preparation method of the nickel screen coating material comprises the following steps: under the protection of nitrogen, placing the triisocyanate modified anhydride and the m-phenylenediamine into dimethylformamide, uniformly stirring, performing polycondensation reaction at 30 ℃ for 2 hours, adding trimethylamine and benzoic anhydride, stirring for 2 hours, performing defoaming treatment by ultrasonic for 30 minutes, coating on the surface of a printing nickel screen matrix, and performing curing treatment in a vacuum drying oven at each temperature point of 100 ℃, 150 ℃ and 250 ℃ for 2 hours.
Example 2:
The nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: 140 parts of N-methylpyridine, 20 parts of triisocyanate modified anhydride, 18 parts of diamine monomer, 4 parts of catalyst and 4 parts of benzoic anhydride; the diamine monomer is mixed with m-phenylenediamine and p-phenylenediamine according to the volume ratio of 2:1, and the catalyst is mixed with trimethylamine and N, N-diisopropylethylenediamine according to the volume ratio of 2:1.
The preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, 3', 4' -diphenyl ether tetracarboxylic dianhydride, triisocyanate and dimethylformamide are reacted for 4 hours at 120 ℃ to obtain triisocyanate modified anhydride, wherein the mass ratio of the 3,3', 4' -diphenyl ether tetracarboxylic dianhydride, triisocyanate and dimethylformamide is 5:5:75.
The preparation method of the nickel screen coating material comprises the following steps: under the protection of nitrogen, placing triisocyanate modified anhydride and diamine monomer into N-methylpyridine, uniformly stirring, performing polycondensation reaction at 20 ℃ for 2 hours, adding a catalyst and benzoic anhydride, stirring for 3 hours, performing defoaming treatment by ultrasonic for 30 minutes, coating on the surface of a printing nickel screen matrix, and performing curing treatment in a vacuum drying oven at each temperature point of 100 ℃, 150 ℃ and 250 ℃ for 2 hours.
Example 3:
The nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: 80 parts of N-methylpyridine, 40 parts of triisocyanate modified anhydride, 50 parts of p-xylylenediamine, 5 parts of N-phenylpyrrolidine and 3 parts of phthalic anhydride;
The preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, reacting dianhydride monomer, triisocyanate and dimethylformamide for 5 hours at 100 ℃ to obtain triisocyanate modified anhydride, wherein the mass ratio of the dianhydride monomer to the triisocyanate to the dimethylformamide is 25:30:50. the dianhydride monomer is prepared by mixing 3,3', 4' -diphenyl tetracarboxylic dianhydride and 3,3', 4' -diphenyl sulfone tetracarboxylic dianhydride according to a mass ratio of 1:1.
The preparation method of the nickel screen coating material comprises the following steps: under the protection of nitrogen, placing triisocyanate modified anhydride and paraxylylenediamine into N-methylpyridine, uniformly stirring, performing polycondensation reaction at 40 ℃ for 1h, then adding N-phenylpyrrolidine and phthalic anhydride, stirring for 4 h, performing defoaming treatment by ultrasonic for 30min, coating on the surface of a printing nickel screen matrix, and finally performing curing treatment in a vacuum drying oven at each temperature point of 100 ℃,150 ℃ and 250 ℃ for 2 h.
Example 4:
The nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: 100 parts of N-methylpyridine, 28 parts of triisocyanate modified anhydride, 29 parts of p-xylylenediamine, 2 parts of a catalyst and 3 parts of phthalic anhydride; the catalyst is prepared by mixing N-phenylpyrrolidine and N, N-diisopropyl ethylenediamine according to a mass ratio of 3:1.
The preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, reacting dianhydride monomer, triisocyanate and dimethylformamide for 4 hours at 120 ℃ to obtain triisocyanate modified anhydride, wherein the mass ratio of the dianhydride monomer to the triisocyanate to the dimethylformamide is 15:30: 75. The dianhydride monomer is 3,3', 4' -diphenyl tetracarboxylic dianhydride and 3,3', 4' -diphenyl sulfone tetracarboxylic dianhydride which are uniformly mixed according to the mass ratio of 3:1.
The preparation method of the nickel screen coating material comprises the following steps: under the protection of nitrogen, placing the triisocyanate modified anhydride and the paraxylylenediamine into N-methylpyridine, uniformly stirring, performing polycondensation reaction at 35 ℃ for 1h, adding a catalyst and phthalic anhydride, stirring for 4 h, performing defoaming treatment by ultrasonic for 30min, coating on the surface of a printing nickel screen matrix, and performing curing treatment in a vacuum drying oven at each temperature point of 100 ℃, 150 ℃ and 250 ℃ for 2 h.
Example 5:
A printed nickel screen comprising a printed nickel screen substrate and a nickel screen coating material coated on the printed nickel screen substrate, wherein the nickel screen coating material is the nickel screen coating material in example 1, and the thickness of the nickel screen coating material is 5 μm; the printed nickel screen matrix comprises a printed nickel screen substrate and a nickel/metal Cr solid solution alloy layer which is solid-solution on the surface of the printed nickel screen substrate, wherein the thickness of the nickel/metal M solid solution alloy layer is 20nm, and the solid solubility of metal Cr in the nickel/metal Cr solid solution alloy layer is 25%.
The preparation method of the printing nickel screen matrix comprises the following steps:
1) Pretreatment: respectively ultrasonically cleaning the printed nickel screen substrate for 5min by using acetone and deionized water to remove surface impurities; then, immersing the printed nickel screen substrate in a mixed solution of 20% hydrofluoric acid and 25% nitric acid in a volume ratio of 1:1 for 10min, and polishing to remove an oxide layer;
2) And (2) performing magnetron sputtering on the surface of the printed nickel screen substrate pretreated in the step (1) by adopting a magnetron sputtering method to form a metal Cr layer with the thickness of 5nm, and performing heat treatment for 1.5 hours at the temperature of 1200 ℃ in a hydrogen environment to form a nickel/metal Cr solid solution alloy layer by using metal Cr in the metal Cr layer and nickel element in the printed nickel screen substrate, thereby obtaining the printed nickel screen substrate.
The preparation method of the printed nickel screen comprises the following steps:
Putting the printing nickel screen matrix into a mixed solution of triethylamine and toluene in a volume ratio of 20:100 for reaction for 5 hours, and then cleaning with deionized water to obtain the printing nickel screen matrix subjected to amino grafting treatment; then the method in the example 1 is adopted to coat the nickel screen coating material on the surface of the printing nickel screen substrate which is subjected to the amino grafting treatment.
FIG. 1 shows a magnetron sputtered metal Cr layer on the surface of a printed nickel screen substrate in this embodiment, and the Cr layer can be seen to uniformly cover the nickel metal surface. Fig. 2 shows the element distribution of the metal Cr layer magnetically sputtered on the surface of the printed nickel screen substrate after heat treatment, and it can be seen that the metal Cr atoms are solid-dissolved in the printed nickel screen substrate to form a metal solid-solution layer. Fig. 3 shows the nickel screen coating layer material (modified polyimide coating layer) coated on the surface of the printed nickel screen substrate in this embodiment, and it can be seen that the modified polyimide is uniformly coated on the nickel surface.
Example 6:
A printed nickel screen comprising a printed nickel screen substrate and a nickel screen coating material coated on the printed nickel screen substrate, wherein the nickel screen coating material is the nickel screen coating material in example 2, and the thickness of the nickel screen coating material is 8 μm; the printing nickel screen substrate comprises a printing nickel screen substrate and a nickel/metal Mo solid solution alloy layer which is solid-solution on the surface of the printing nickel screen substrate, wherein the thickness of the nickel/metal Mo solid solution alloy layer is 22nm, and the solid solubility of metal Mo in the nickel/metal Mo solid solution alloy layer is 36%.
The preparation method of the printing nickel screen matrix comprises the following steps:
1) Pretreatment: respectively ultrasonically cleaning the printed nickel screen substrate by using acetone and deionized water for 10min to remove surface impurities; then, immersing the printed nickel screen substrate in a mixed solution of 20% hydrofluoric acid and 25% nitric acid in a volume ratio of 1:1 for 10min, and polishing to remove an oxide layer;
2) And (2) performing magnetron sputtering on the surface of the printed nickel screen substrate pretreated in the step (1) by adopting a magnetron sputtering method to form a metal Mo layer with the thickness of 6nm, and performing heat treatment for 1h at the temperature of 1250 ℃ in a hydrogen environment to form a nickel/metal Mo solid solution alloy layer by using metal Mo in the metal Mo layer and nickel element in the printed nickel screen substrate, thereby obtaining the printed nickel screen substrate.
The preparation method of the printed nickel screen comprises the following steps:
Putting the printing nickel screen matrix into a mixed solution of isopropylamine and toluene in a volume ratio of 10:100 for reaction for 6 hours, and then cleaning with deionized water to obtain the printing nickel screen matrix subjected to amino grafting treatment; and then the surface of the printed nickel screen matrix subjected to the amino grafting treatment is coated with a nickel screen coating material by adopting the method in the embodiment 2.
Example 7:
A printed nickel screen comprising a printed nickel screen substrate and a nickel screen coating material coated on the printed nickel screen substrate, wherein the nickel screen coating material is the nickel screen coating material in example 3, and the thickness of the nickel screen coating material is 10 μm; the printed nickel screen matrix comprises a printed nickel screen substrate and a nickel/metal Cr solid solution alloy layer which is solid-solution on the surface of the printed nickel screen substrate. The thickness of the nickel/metal Cr solid solution alloy layer is 25nm, and the solid solubility of the metal Cr in the nickel/metal Cr solid solution alloy layer is 40%.
The preparation method of the printing nickel screen matrix comprises the following steps:
1) Pretreatment: respectively ultrasonically cleaning the printed nickel screen substrate by using acetone and deionized water for 8min to remove surface impurities; then, immersing the printed nickel screen substrate in a mixed solution of 20% hydrofluoric acid and 25% nitric acid in a volume ratio of 1:1 for 20min to perform polishing treatment to remove an oxide layer;
2) And (2) performing magnetron sputtering on the surface of the printed nickel screen substrate pretreated in the step (1) by adopting a magnetron sputtering method to form a metal Cr layer with the thickness of 10nm, and performing heat treatment for 1.5 hours at the temperature of 1300 ℃ in a hydrogen environment to form a nickel/metal Cr solid solution alloy layer by using metal Cr in the metal Cr layer and nickel element in the printed nickel screen substrate, thereby obtaining the printed nickel screen substrate.
The preparation method of the printed nickel screen comprises the following steps:
putting the printing nickel screen matrix into a mixed solution of ethylenediamine and toluene with the volume ratio of 50:100 for reaction for 8 hours, and then cleaning with deionized water to obtain the printing nickel screen matrix subjected to amino grafting treatment; and then the surface of the printed nickel screen matrix subjected to the amino grafting treatment is coated with a nickel screen coating material by adopting the method in the embodiment 3.
Example 8:
A printed nickel screen comprising a printed nickel screen substrate and a nickel screen coating material coated on the printed nickel screen substrate, wherein the nickel screen coating material is the nickel screen coating material in example 4, and the thickness of the nickel screen coating material is 20 μm; the printed nickel screen matrix comprises a printed nickel screen substrate and a nickel/metal Mo solid solution alloy layer which is solid-solution on the surface of the printed nickel screen substrate.
The preparation method of the printing nickel screen matrix comprises the following steps:
1) Pretreatment: respectively ultrasonically cleaning the printed nickel screen substrate for 5min by using acetone and deionized water to remove surface impurities; then, immersing the printed nickel screen substrate in a mixed solution of 20% hydrofluoric acid and 25% nitric acid in a volume ratio of 1:1 for 20min to perform polishing treatment to remove an oxide layer;
2) And (2) performing magnetron sputtering on the surface of the printed nickel screen substrate pretreated in the step (1) by adopting a magnetron sputtering method to form a metal Mo layer with the thickness of 15nm, and performing heat treatment for 2 hours at the temperature of 1400 ℃ in a hydrogen environment to form a nickel/metal Mo solid solution alloy layer by using metal Mo in the metal Mo layer and nickel element in the printed nickel screen substrate, thereby obtaining the printed nickel screen substrate. The thickness of the nickel/metal Mo solid solution alloy layer is 30nm, and the solid solubility of the metal Mo in the nickel/metal Mo solid solution alloy layer is 50%.
The preparation method of the printed nickel screen comprises the following steps:
Putting the printing nickel screen matrix into a mixed solution of ethylenediamine and toluene with the volume ratio of 30:100 for reaction for 10 hours, and then cleaning with deionized water to obtain the printing nickel screen matrix subjected to amino grafting treatment; and then the method in the example 4 is adopted to coat the nickel screen coating material on the surface of the printing nickel screen substrate which is subjected to the amino grafting treatment.
Example 9:
Unlike example 5, the method of preparing the printed nickel screen comprises the steps of: the method in example 1 is directly adopted to coat the surface of the printing nickel screen matrix with a nickel screen coating material, and the surface of the printing nickel screen matrix is not subjected to amino grafting treatment.
Example 10:
Unlike example 5, the printed nickel screen substrate was a printed nickel screen substrate (the printed nickel screen substrate was pretreated but not magnetron sputtered with a metallic Cr layer).
Example 11:
Unlike example 5, the printed nickel screen substrate was a printed nickel screen substrate (the printed nickel screen substrate was pretreated but not magnetron sputtered with a metallic Cr layer), and the method of making the printed nickel screen comprised the steps of: the method in example 1 is directly adopted to coat the surface of the printing nickel screen matrix with a nickel screen coating material, and the surface of the printing nickel screen matrix is not subjected to amino grafting treatment.
Comparative example 1:
Unlike example 10, the starting triisocyanate modified anhydride in the modified polyimide was replaced with 3,3', 4' -diphenyltetracarboxylic dianhydride.
Performance test:
The peel strength of the nickel screen coating materials (polyimide layers) and the nickel residual amount of the printed nickel screen in examples 5 to 11 and comparative example 1 were tested.
Polyimide peel strength test: the nickel screen coating material was peeled from the surface of the printed nickel screen substrate at an angle of 90 ° using a soft substrate peel jig, the peel strength was evaluated, in N/mm, and standard reference IPC-TM-650 was tested.
The residual nickel content is tested by referring to GB/T18885-2020 technical requirement for ecological textiles. The test samples were: the printed fabric was woven with 30000 m of the dope continuously printed, and then the residual amount of nickel on the printed fabric was tested. The infant water fastness was tested with reference to GB/T18885-2020.
The specific test results are shown in table 1.
Table 1:
As can be seen from the comparison of the examples 5 and 9 and the comparison of the examples 10 and 11, the amino grafting treatment is carried out on the printed nickel screen substrate, so that the binding force between the printed nickel screen substrate and polyimide can be improved, and the comparison of the examples 5 and 10 and the comparison of the examples 9 and 11 shows that the nickel/metal Cr solid solution alloy layer is formed on the surface of the printed nickel screen substrate in a solid solution manner, so that the binding force between the printed nickel screen substrate and polyimide can be further improved, and the nickel residue can be obviously reduced. As can be seen from comparison of example 11 and comparative example 1, if the material of the nickel screen coating layer is not modified by triisocyanate, but is directly modified by ordinary dianhydride monomer, the shrinkage rate of the prepared polyimide is larger, so that the interface binding force between the printed nickel screen substrate and the polyimide interface is weaker due to elastic mismatch.
The Standard document Oeko-Tex Standard 100 published by the International Environment protection textile Association prescribes that the nickel limit value of the product grade I is 0.5ppm, and the nickel residue of the printed nickel screen is lower than 0.3 ppm, thereby completely meeting the requirements. GB/T18885-2020 provides that the water-resistant color fastness of infants is not lower than 3-4 grades, and the water-resistant color fastness of the printed nickel screen is 5 grades, so that the requirements are completely met.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The printing nickel screen is characterized by comprising a printing nickel screen substrate and a nickel screen coating material coated on the printing nickel screen substrate, wherein the printing nickel screen substrate comprises a printing nickel screen substrate and a nickel/metal M solid solution alloy layer which is solid-solution on the surface of the printing nickel screen substrate, and the metal M is a mixture of one or more of metal Cr and metal Mo;
the nickel screen coating material is modified polyimide, and the modified polyimide comprises the following raw materials in parts by weight: 80-140 parts of organic solvent, 20-50 parts of triisocyanate modified anhydride, 18-50 parts of diamine monomer, 2-5 parts of catalyst and 2-4 parts of dehydrating agent;
The preparation method of the triisocyanate modified anhydride comprises the following steps: under the protection of nitrogen, reacting dianhydride monomer, triisocyanate and dimethylformamide for 3-5 hours at 100-150 ℃ to obtain triisocyanate modified anhydride, wherein the mass ratio of the dianhydride monomer to the triisocyanate to the dimethylformamide is 5-25: 5-30: 50-75 parts;
The preparation method of the nickel screen coating material comprises the following steps: placing triisocyanate modified anhydride and diamine monomer into an organic solvent under the protection of nitrogen, uniformly stirring, performing polycondensation reaction at 20-40 ℃ for 1-2 h, adding a catalyst and a dehydrating agent, stirring for 2-4 h, performing defoaming treatment by ultrasonic for 30min, coating on the surface of a printing nickel screen matrix, and performing curing treatment in a vacuum drying oven at each temperature point of 100 ℃, 150 ℃ and 250 ℃ for 2h respectively;
The preparation method of the printed nickel screen matrix comprises the following steps: performing magnetron sputtering on the surface of the printed nickel screen substrate by a magnetron sputtering method to form a metal M layer with the thickness of 5-15 nm, and performing heat treatment for 1-2 hours at the temperature of 1200-1400 ℃ in a hydrogen environment to obtain a printed nickel screen substrate;
The preparation method of the printed nickel screen comprises the following steps: placing the printing nickel screen matrix into a mixed solution of organic amine and toluene with the volume ratio of (10-50) 100 for reaction for 5-10 hours, and then cleaning with deionized water to obtain the printing nickel screen matrix subjected to amino grafting treatment; coating a nickel screen coating material on the surface of the printing nickel screen substrate subjected to the amino grafting treatment; the organic amine is one or more of triethylamine, isopropylamine and ethylenediamine.
2. The printed nickel screen of claim 1, wherein the diamine monomer is one or more of m-phenylenediamine, p-xylylenediamine, p-phenylenediamine;
The catalyst is one or more of trimethylamine, N-diethyl ethylenediamine, N-phenylpyrrolidine and N, N-diisopropyl ethylenediamine;
the dehydrating agent is one or more of benzoic anhydride and phthalic anhydride.
3. The printed nickel screen of claim 1, wherein the dianhydride monomer is one or more of 3,3', 4' -diphenyl tetracarboxylic dianhydride, 3', 4' -diphenyl sulfone tetracarboxylic dianhydride.
4. The printed nickel screen according to claim 1, wherein the thickness of the nickel/metal M solid solution alloy layer is 20-30 nm, and the solid solubility of the metal M in the nickel/metal M solid solution alloy layer is 25% -50%;
the thickness of the nickel screen coating layer material is 5-20 mu m.
5. The printed nickel screen according to claim 1, wherein the printed nickel screen substrate is a pretreated printed nickel screen substrate, the pretreatment comprising the steps of: respectively ultrasonically cleaning the printed nickel screen substrate by using acetone and deionized water for 5-10 min to remove surface impurities; and then, immersing the printed nickel screen substrate in a mixed solution of 20% hydrofluoric acid and 25% nitric acid in a volume ratio of 1:1 for 10-20 min, and polishing to remove the oxide layer.
6. Use of a printed nickel screen according to any one of claims 1-5 in a textile printing process.
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| WO2015074913A1 (en) * | 2013-11-21 | 2015-05-28 | Basf Se | Cross-linked polymeric materials based on polyimides, production and use thereof |
| CN109762166A (en) * | 2018-12-26 | 2019-05-17 | 哈尔滨工程大学 | A kind of preparation method of polyimide precursor and Kapton |
| CN116218357A (en) * | 2022-12-09 | 2023-06-06 | 航天科工(长沙)新材料研究院有限公司 | Cyanate in-situ modified polyimide high-temperature-resistant coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015074913A1 (en) * | 2013-11-21 | 2015-05-28 | Basf Se | Cross-linked polymeric materials based on polyimides, production and use thereof |
| CN109762166A (en) * | 2018-12-26 | 2019-05-17 | 哈尔滨工程大学 | A kind of preparation method of polyimide precursor and Kapton |
| CN116218357A (en) * | 2022-12-09 | 2023-06-06 | 航天科工(长沙)新材料研究院有限公司 | Cyanate in-situ modified polyimide high-temperature-resistant coating and preparation method thereof |
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