CN118420960A - Novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process - Google Patents
Novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process Download PDFInfo
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- CN118420960A CN118420960A CN202410214380.2A CN202410214380A CN118420960A CN 118420960 A CN118420960 A CN 118420960A CN 202410214380 A CN202410214380 A CN 202410214380A CN 118420960 A CN118420960 A CN 118420960A
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 35
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 35
- KDFQYGBJUYYWDJ-UHFFFAOYSA-N azane;sodium Chemical compound N.[Na] KDFQYGBJUYYWDJ-UHFFFAOYSA-N 0.000 claims description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
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- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
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- URXNVXOMQQCBHS-UHFFFAOYSA-N naphthalene;sodium Chemical compound [Na].C1=CC=CC2=CC=CC=C21 URXNVXOMQQCBHS-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention relates to a novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process, and belongs to the field of polytetrafluoroethylene surface modification. The novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process comprises the following steps of: preparing treatment liquid, ammoniating polytetrafluoroethylene, drying the ammoniated polytetrafluoroethylene and bonding the polytetrafluoroethylene. The invention provides a polytetrafluoroethylene surface ammoniation preparation process with simple preparation process and high treatment efficiency, which solves the technical bottleneck and difficult problems of polytetrafluoroethylene surface treatment by optimally designing a polytetrafluoroethylene treatment reagent and a preparation process, wherein the treatment reagent is environment-friendly and can be recycled, and the treated polytetrafluoroethylene can be bonded with stainless steel, carbon steel, aluminum plates, titanium steel, titanium alloy, copper plates, polytetrafluoroethylene, polypropylene, polyethylene, polyurethane and polystyrene.
Description
Technical Field
The invention belongs to the field of polytetrafluoroethylene surface modification, and particularly relates to a novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process.
Background
Polytetrafluoroethylene, commonly known as "plastic king", is a high molecular polymer prepared by polymerizing tetrafluoroethylene as a monomer, and can be used for a long time at-180-260 ℃. The polytetrafluoroethylene has excellent chemical medium resistance, self-lubrication and dielectric property, and has wide application in the aspects of chemical corrosion resistance, electrical appliance insulation and mechanical sealing. However, polytetrafluoroethylene is difficult to bond, and if bonding is desired, a surface treatment is required. There are many methods for surface treatment of polytetrafluoroethylene, such as solution chemistry, plasma treatment and biomimetic modification.
The solution chemical modification has been widely used with the advantages of simple operation and good modification effect. Chemical solutions for polytetrafluoroethylene modification include furan alkali solutions, sodium naphthalene solutions, strong acids and strong oxidizing salts. The mechanism of the solution chemistry modified polytetrafluoroethylene membrane is based on the reaction between the solution and polytetrafluoroethylene. The solution chemical method for treating the polytetrafluoroethylene has the advantages of simple operation, simple equipment, obvious treatment effect, lasting surface activity and the like, but has the risks of introducing impurities, enhancing surface toxicity, reducing mechanical strength and the like in some methods.
The plasma treatment method comprises the steps of ion surface activation, plasma induced grafting, plasma polymerization and the like, wherein the plasma assisted surface activation and grafting are two main modification modes of the polytetrafluoroethylene film. Plasma-assisted surface activation is achieved by reactive gas plasma treatment, creating a hydrophilic surface. Surface plasmon grafting and surface polymerization effectively change the surface properties of the film. When the polymeric material is exposed to plasma, free radicals are generated in the polymer chains, which initiate the polymerization reaction when they come into contact with the monomer in the liquid or gas phase. The graft copolymer is formed on the surface. In plasma-assisted copolymerization, the polymer is first exposed to a plasma to generate radicals at the surface, and inelastic collisions between electrons in the plasma and the polymer surface generate radicals in the polymer chains. Thereafter, the polymer is exposed to a vapor of the monomer or an aqueous or organic solution of the monomer. Plasma graft copolymerization occurs at the surface. The plasma technology modified polytetrafluoroethylene has the advantages of short treatment time and no change of mechanical properties and other self properties of the polytetrafluoroethylene body. Different characteristic surfaces can be obtained according to different gases and different excitation modes, and the device has operability. However, the excitation equipment is complex, the treatment process is complex, polytetrafluoroethylene aging is caused after treatment, the efficiency is possibly insufficient due to low-power treatment, and surface fiber breakage is caused at high power. Meanwhile, the effect time of maintaining the plasma treatment is short, the function cannot be maintained for a long time, and the defects limit the application of the plasma.
The bionic modification is to graft bioactive substances such as macromolecular amino acid, biological polysaccharide, extracellular matrix and the like on the surface of the material, so that the implant material has a bioactive surface layer, reduces immune rejection and is quickly suitable for the surrounding environment. The bionic modification does not change the property of the material, but the current use frequency on the surface of polytetrafluoroethylene is not very high, mainly the strong hydrophobicity of polytetrafluoroethylene, and the active substances are difficult to combine with a base and are easy to fall off due to low surface energy. This disadvantage greatly limits its application.
Therefore, the surface treatment method of the polytetrafluoroethylene-based material is efficient, environment-friendly and simple in process, does not damage the modification of the polytetrafluoroethylene surface, facilitates the adhesion of polytetrafluoroethylene and other materials, and expands the application field of polytetrafluoroethylene.
Disclosure of Invention
Aiming at the defects of low efficiency, complex process, easy inactivation, damage to polytetrafluoroethylene base materials, toxicity of treated polytetrafluoroethylene caused by using toxic reagents and the like in the surface modification of polytetrafluoroethylene, the invention provides a polytetrafluoroethylene surface ammoniation preparation process with green and environment-friendly treatment reagents and recycling use, simple preparation process and high treatment efficiency, which solves the technical bottleneck and difficult problems of polytetrafluoroethylene surface treatment, and the treated polytetrafluoroethylene can be bonded with stainless steel, polytetrafluoroethylene, polypropylene, polyethylene, polyurethane and polystyrene.
The invention provides a novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process, which comprises the following steps:
S1, preparing a treatment fluid: and adding metal sodium into the liquid ammonia solution to prepare a sodium ammonia solution, and reacting for 1-3 hours at the temperature of-30-0 0 ℃ until the sodium is completely dissolved.
S2 ammoniation of polytetrafluoroethylene: immersing the polytetrafluoroethylene workpiece to be treated in a sodium ammonia solution for soaking, taking out, and then soaking in a methanol or ethanol solution for 5-10 minutes.
S3, drying polytetrafluoroethylene after ammoniation: and taking out the workpiece from the methanol or ethanol solution, rinsing the workpiece with clear water, and then placing the workpiece in a brown reagent bottle at 20-30 0 ℃ for drying until no liquid remains on the surface of the polytetrafluoroethylene.
S4, bonding polytetrafluoroethylene: and uniformly coating the adhesive on the surface to be bonded of the polytetrafluoroethylene, immediately bonding, and standing for 20-40 hours at 24-30 0 ℃ to firmly bond.
In some embodiments, in the step S1, the mass ratio of the sodium metal to the liquid ammonia solution is 1: 19-99.
In some of these embodiments, the ratio of the surface area of polytetrafluoroethylene to be treated in step S2 to the sodium ammonia solution is1 cm 2: 5-20 g.
In some embodiments, the soaking time of the polytetrafluoroethylene to be treated in the step S2 in the sodium ammonia solution is 10-30S.
In some embodiments, the sodium ammonia solution treated in the step S2 is put into a polypropylene bottle for recycling, sealed and stored under the condition of-30-0 0 C, and can not be discarded at random to prevent environment pollution.
In some embodiments, the adhesive in step S4 is one or more of epoxy, silicone, and polyurethane.
In some of these embodiments, the polytetrafluoroethylene coated with the adhesive in the step S4 may be bonded with stainless steel, polytetrafluoroethylene, polypropylene, polyethylene, polyurethane, polystyrene.
(1) The polytetrafluoroethylene treatment reagent, namely the sodium ammonia solution, has the advantage of environmental protection, and the treated polytetrafluoroethylene has no toxicity, can be used in the biological field, and does not limit the application field of polytetrafluoroethylene;
(2) The polytetrafluoroethylene treatment reagent, namely the sodium ammonia solution, can be recycled for multiple times, so that the pollution to the environment is reduced;
(3) The optimal volume-mass ratio of the surface area of the polytetrafluoroethylene to be treated to the sodium ammonia solution treatment is explored, so that the polytetrafluoroethylene surface treatment efficiency can be ensured, and the sodium ammonia solution waste can be avoided.
(4) The conditions for treating the polytetrafluoroethylene are mild, the time is short, the polytetrafluoroethylene base material cannot be damaged, and the aging and the mechanical strength reduction of the polytetrafluoroethylene in the treatment process are avoided.
(5) The treated polytetrafluoroethylene surface is grafted with relatively stable primary amino groups, so that the polytetrafluoroethylene can be stably stored for a long time and is not easy to inactivate.
Drawings
FIG. 1 shows XPS scans of polytetrafluoroethylene before and after treatment in example 1;
FIG. 2 shows XPS scans of polytetrafluoroethylene before and after treatment in example 2;
FIG. 3 shows XPS scans of polytetrafluoroethylene before and after the treatment of example 3;
FIG. 4 shows the water contact angle of polytetrafluoroethylene before and after the treatment of example 1;
FIG. 5 shows the water contact angle of polytetrafluoroethylene before and after the treatment of example 2;
FIG. 6 shows the water contact angle of polytetrafluoroethylene before and after the treatment of example 3;
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will clearly and completely describe the technical process steps, specific implementation conditions and materials in conjunction with the drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing a treatment fluid: 1 part by weight of metallic sodium is added into 19 parts of liquid ammonia solution to prepare sodium ammonia solution, and the sodium ammonia solution is reacted for 2 hours at the temperature of-20 0 ℃ until the sodium is completely dissolved.
Ammoniation of polytetrafluoroethylene: accurately testing the surface area of polytetrafluoroethylene to be treated, soaking the polytetrafluoroethylene to be treated in a sodium ammonia solution, wherein the volume-mass ratio of the polytetrafluoroethylene to the sodium ammonia solution is 1 cm 2: 10g, soaking time is 10 seconds, the treated sodium ammonia solution is put into a polypropylene bottle for recycling, sealing and preserving under the condition of-10 0 C, and the sodium ammonia solution cannot be discarded at random to prevent environment pollution. Then the treated polytetrafluoroethylene is soaked in ethanol solution for 10 minutes.
Drying of the aminated polytetrafluoroethylene: and taking out the workpiece from the methanol or ethanol solution, rinsing the workpiece with clear water, and then placing the workpiece in a brown reagent bottle at 30 0 ℃ for drying until no liquid remains on the surface of the polytetrafluoroethylene.
To prove that the surface ammonification of the polytetrafluoroethylene is successful, XPS scanning characterization is carried out on polytetrafluoroethylene before and after treatment, as shown in figure 1, the surface of the polytetrafluoroethylene before treatment is free of nitrogen elements, the peak of N1s in figure 1, the surface of the polytetrafluoroethylene after treatment is provided with obvious nitrogen elements, the peak of N1s in figure 1, and the surface ammonification of the polytetrafluoroethylene is successful. The contact angle of polytetrafluoroethylene before and after treatment was measured by means of a surface contact angle meter, as shown in fig. 4, the contact angle of water before treatment was about 129.1 °, the contact angle of water after treatment was 15.6 °, and the results further demonstrate that the surface ammoniation modification of polytetrafluoroethylene was successful. The tensile strength of polytetrafluoroethylene before and after treatment is tested by a universal tensile testing machine, the strength of polytetrafluoroethylene before treatment is 71.81 +/-0.97 Mpa, the tensile strength of polytetrafluoroethylene after treatment is 70.21+/-0.69 Mpa, and the mechanical strength of a surface polytetrafluoroethylene substrate is not affected.
Example 2
Preparing a treatment fluid: adding 1 part by weight of metallic sodium into 99 parts of liquid ammonia solution to prepare sodium ammonia solution, and reacting for 1 hour at the temperature of-10 0 ℃ until sodium is completely dissolved.
Ammoniation of polytetrafluoroethylene: accurately testing the surface area of polytetrafluoroethylene to be treated, soaking the polytetrafluoroethylene to be treated in a sodium ammonia solution, wherein the volume-mass ratio of the polytetrafluoroethylene to the sodium ammonia solution is 1 cm 2: 20g, soaking time is 20 seconds, the treated sodium ammonia solution is put into a polypropylene bottle for recycling, sealing and preserving under the condition of-20 0 ℃ and can not be discarded randomly to prevent environment pollution. Then the treated polytetrafluoroethylene is soaked in ethanol solution for 8 minutes.
Drying of the aminated polytetrafluoroethylene: and taking out the workpiece from the methanol or ethanol solution, rinsing the workpiece with clear water, and then placing the workpiece in a brown reagent bottle at the temperature of 27 0 ℃ for drying until no liquid remains on the surface of the polytetrafluoroethylene.
To prove that the surface ammonification of the polytetrafluoroethylene is successful, XPS scanning characterization is carried out on polytetrafluoroethylene before and after treatment, as shown in figure 2, the surface of polytetrafluoroethylene before treatment has no nitrogen element, the peak of N1s in figure 2, the surface of polytetrafluoroethylene after treatment has obvious nitrogen element, the peak of N1s in figure 2, and the surface ammonification of the polytetrafluoroethylene is successful. The contact angle of polytetrafluoroethylene before and after treatment was measured by means of a surface contact angle meter, as shown in fig. 4, the contact angle of water before treatment was about 133.6 °, the contact angle of water after treatment was 14.7 °, and the results further demonstrate that the surface ammoniation modification of polytetrafluoroethylene was successful. The tensile strength of polytetrafluoroethylene before and after treatment is tested by a universal tensile testing machine, the strength of polytetrafluoroethylene before treatment is 68.56+/-1.23 Mpa, the tensile strength of polytetrafluoroethylene after treatment is 66.79 +/-0.89 Mpa, and the mechanical strength of a surface polytetrafluoroethylene substrate is not affected.
Example 3
Preparing a treatment fluid: adding 1 part by weight of metallic sodium into 49 parts of liquid ammonia solution to prepare sodium ammonia solution, and reacting for 3 hours at the temperature of-30 0 ℃ until sodium is completely dissolved.
Ammoniation of polytetrafluoroethylene: accurately testing the surface area of polytetrafluoroethylene to be treated, soaking the polytetrafluoroethylene to be treated in a sodium ammonia solution, wherein the volume-mass ratio of the polytetrafluoroethylene to the sodium ammonia solution is 1 cm 2: 10g, soaking time is 30 seconds, and the treated sodium ammonia solution is put into a polypropylene bottle for recycling, sealed and stored under the condition of-20 0 ℃ and cannot be discarded randomly to prevent environment pollution. Then the treated polytetrafluoroethylene is soaked in ethanol solution for 10 minutes.
Drying of the aminated polytetrafluoroethylene: and taking out the workpiece from the methanol or ethanol solution, rinsing the workpiece with clear water, and then placing the workpiece in a brown reagent bottle at 30 0 ℃ for drying until no liquid remains on the surface of the polytetrafluoroethylene.
To prove that the surface ammonification of the polytetrafluoroethylene is successful, XPS scanning characterization is carried out on polytetrafluoroethylene before and after treatment, as shown in figure 3, the surface of polytetrafluoroethylene before treatment has no nitrogen element, the peak of N1s in figure 3, the surface of polytetrafluoroethylene after treatment has obvious nitrogen element, the peak of N1s in figure 3, and the surface ammonification of the polytetrafluoroethylene is successful. The contact angle of polytetrafluoroethylene before and after treatment was measured by means of a surface contact angle meter, as shown in fig. 4, the contact angle of water before treatment was about 131.8 °, the contact angle of water after treatment was 16.4 °, and the results further demonstrate that the surface ammoniation modification of polytetrafluoroethylene was successful. The tensile strength of polytetrafluoroethylene before and after treatment is tested by a universal tensile testing machine, the strength of polytetrafluoroethylene before treatment is 70.52+/-1.12 Mpa, the tensile strength of polytetrafluoroethylene after treatment is 71.33 +/-2.01 Mpa, and the mechanical strength of a surface polytetrafluoroethylene substrate is not affected.
Example 4
The portion of polytetrafluoroethylene treated in example 1 to be bonded was coated with an epoxy adhesive, the stainless steel to be bonded was bonded to the polytetrafluoroethylene coated with the epoxy adhesive, and the resultant was left to stand at 24 0 C for 20 hours, and the bonding force was measured to be 15.24N m -2.
Example 5
The silicone adhesive was applied to the portion of the polytetrafluoroethylene treated in example 2 to be bonded, the polytetrafluoroethylene to be bonded was bonded to the silicone adhesive-applied polytetrafluoroethylene, and the resultant was allowed to stand at 30 0 C for 30 hours, and the bonding force was measured to be 18.33N m -2.
Example 6
The portion to be bonded of the polytetrafluoroethylene treated in example 3 was coated with a polyurethane adhesive, and the polyethylene to be bonded was bonded to the polyurethane adhesive-coated polytetrafluoroethylene, and the resultant was left standing at 30 0 C for 36 hours, and tested for its adhesion of 19.991N m -2.
Example 7
The portion to be bonded of the polytetrafluoroethylene treated in example 1 was coated with a polyurethane adhesive, and polypropylene to be bonded was bonded to the polyurethane adhesive-coated polytetrafluoroethylene, and the resultant was allowed to stand at 30 0 C for 40 hours, and the adhesion was measured to be 23.41N m -2.
Example 8
The portion of polytetrafluoroethylene treated in example 2 to be bonded was coated with an epoxy adhesive, the polystyrene to be bonded was bonded to the polytetrafluoroethylene coated with the epoxy adhesive, and the bonding force was measured to be 19.56N m -2 by standing at 30 0 C for 20 hours.
Example 9
The portion to be bonded of the polytetrafluoroethylene treated in example 3 was coated with a polyurethane adhesive, the stainless steel to be bonded was bonded with the polyurethane adhesive-coated polytetrafluoroethylene, and the resultant was left to stand at 35 0 C for 40 hours, and the adhesion was measured to be 24.71: 24.71N m -2.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. The novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process is characterized by comprising the following steps of:
S1, preparing a treatment fluid: adding metal sodium into liquid ammonia solution to prepare sodium ammonia solution, reacting for 1-3 hours at the temperature of-30-0 0 ℃ until sodium is completely dissolved,
S2 ammoniation of polytetrafluoroethylene: immersing the polytetrafluoroethylene workpiece to be treated in sodium ammonia solution for soaking, taking out and then soaking in methanol or ethanol solution for 5-10 minutes,
S3, drying polytetrafluoroethylene after ammoniation: taking out the workpiece from the methanol or ethanol solution, rinsing with clear water, placing in a brown reagent bottle at 20-30 0 ℃ for drying until no liquid residue exists on the surface of polytetrafluoroethylene,
S4, bonding polytetrafluoroethylene: and uniformly coating the adhesive on the surface to be bonded of the polytetrafluoroethylene, immediately bonding, and standing for 20-40 hours at 24-30 0 ℃ to firmly bond.
2. The novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process according to claim 1, wherein the mass ratio of the metal sodium to the liquid ammonia solution in the step S1 is 1: 19-99.
3. The novel environment-friendly polytetrafluoroethylene surface ammonification process according to claim 1, wherein the ratio of the surface area of polytetrafluoroethylene to be treated in the step S2 to the sodium ammonia solution is 1 cm 2: 5-20 g.
4. The novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process according to claim 1, wherein the soaking time of polytetrafluoroethylene to be treated in the step S2 in a sodium ammonia solution is 10-30S.
5. The novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process according to claim 1, wherein the sodium ammonia solution treated in the step S2 is placed in a polypropylene bottle for recycling, is sealed, is stored under the condition of-30-0 0 ℃ and cannot be discarded at random to prevent the environment from being polluted.
6. The novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process according to claim 1, wherein the adhesive in the step S4 is one or more of epoxy resin, organosilicon and polyurethane.
7. The novel environmental protection polytetrafluoroethylene surface ammoniation treatment process according to claim 1, wherein the polytetrafluoroethylene coated with the adhesive in the step S4 can be bonded with stainless steel, carbon steel, aluminum plate, titanium steel, titanium alloy, copper plate, polytetrafluoroethylene, polypropylene, polyethylene, polyurethane and polystyrene.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410214380.2A CN118420960A (en) | 2024-02-27 | 2024-02-27 | Novel environment-friendly polytetrafluoroethylene surface ammoniation treatment process |
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