CN115819788A - Preparation method of high-adhesion high-wear-resistance lightweight nylon powder - Google Patents
Preparation method of high-adhesion high-wear-resistance lightweight nylon powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 57
- 239000004677 Nylon Substances 0.000 title claims abstract description 44
- 229920001778 nylon Polymers 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000011347 resin Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 238000007306 functionalization reaction Methods 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims description 16
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 15
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- GAQUIYRRYYKVMJ-UHFFFAOYSA-M tetrahydroxyazanium;hydroxide Chemical compound [OH-].O[N+](O)(O)O GAQUIYRRYYKVMJ-UHFFFAOYSA-M 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 6
- 229920000299 Nylon 12 Polymers 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 229920000571 Nylon 11 Polymers 0.000 claims description 4
- 229920002292 Nylon 6 Polymers 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007792 addition Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229920000572 Nylon 6/12 Polymers 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000000227 grinding Methods 0.000 abstract description 7
- 125000003277 amino group Chemical group 0.000 abstract 1
- 239000002981 blocking agent Substances 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 229910021389 graphene Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229920001169 thermoplastic Polymers 0.000 description 6
- 239000004416 thermosoftening plastic Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Abstract
The invention relates to lightweight nylon powder with high wear resistance and high adhesion performance and a preparation method thereof. The method comprises the following steps: first, ti is added 3 AlC 2 Functionalization to obtain MXene material containing amino group which can be used as a blocking agent; secondly, adding the functionalized MXene serving as an end-capping agent into a nylon polymerization process to obtain MXene end-capped nylon resin; and finally, processing the obtained nylon resin into powder by a cryogenic grinding method to obtain the lightweight nylon powder with high strength and high adhesive force.
Description
Technical Field
The invention relates to lightweight nylon powder with high adhesion and high wear resistance, belonging to the field of special engineering plastics.
Background
MXene, a new two-dimensional material consisting of a transition metal carbide, nitride or carbonitride of several atomic layer thicknesses, originally appeared in 2011. MXene materials have hydroxyl groups or terminal oxygen on the surface, so that the MXene materials have metal conductivity of transition metal carbide, and are more and more widely applied to supercapacitors, batteries, electromagnetic interference shielding, composite materials and the like. Different from the surfaces of two-dimensional materials such as graphene and transition carbon dihalide, the functional group can also be chemically modified, and the surface of the material can contain active groups through functional design, so that the adhesive force between the powder and metal can be conveniently improved; meanwhile, compared with graphene, no hydrogen bond exists between layers, the graphene has good interlayer sliding performance, and the wear resistance of the graphene is improved conveniently.
Powder coatings can be divided into thermoplastic and thermosetting powder coatings, where thermosetting powder coatings have the advantage of good levelling and strong coating compared to thermoplastic powder coatings, but inevitably they cannot be reused, which is the greatest hurdle limiting their application. The thermoplastic powder does not increase the molecular weight, so the initial requirement of the thermoplastic powder is higher molecular weight to ensure the mechanical property of the coating, but the leveling property of the coating is limited, and the thermoplastic powder which can ensure the mechanical property of the material and can be well leveled has great market prospect.
Nylon powder, as one of the thermoplastic powders, has an increasing market share in the powder coating field, based on the lower density, excellent mechanical properties, low temperature properties, corrosion resistance of nylon materials.
The nylon powder coating is mainly applied to household and automobiles, so that the nylon powder coating has high requirements on the adhesion, the wear-resisting effect and the light weight of the material.
Disclosure of Invention
The invention aims to provide light nylon powder with high adhesive force and high wear resistance, which can meet the adhesive force performance of powder coating, has the characteristics of high wear resistance and light weight, and has a great application prospect in the field of functional materials.
The invention adopts the following technical scheme:
a lightweight nylon powder with high adhesive force and high wear resistance is prepared by the following steps:
[1]mixing Ti 3 AlC 2 Functionalizing to obtain amino functionalized MXene;
[2] adding the functionalized MXene serving as an end-capping agent into a nylon polymerization process to obtain MXene end-capped nylon resin;
[3] the obtained nylon resin is processed into powder by a cryogenic grinding method, and the lightweight nylon powder with high wear resistance and high adhesive force is obtained.
Said step [1]In (1), the above-mentioned 3 AlC 2 Functionalization, comprising:
ti treated by hydrofluoric acid solution 3 AlC 2 Reacting the powder with tetrahydroxyammonium hydroxide (TPAOH) to obtain Ti 3 C 2 T X ；
Then Ti is added 3 C 2 T X Adding into mixed solution of cetyltrimethylammonium chloride (CTAC) and Triethanolamine (TEA), stirring for a while, adding Tetraethoxysilane (TEOS) for reaction to obtain intermediate product MXene @ mSiO 2 ；
Finally, 3-Aminopropyltrimethoxysilane (APTES) is added to MXene @ mSiO 2 In the ethanol solution, refluxing and reacting for a period of time to obtain the amino-functionalized MXene end-capping agent;
wherein, the concentration of the hydrofluoric acid solution is 30-50wt%, and the treatment time is 2-4 days;
the mass fraction of the tetrahydroxy ammonium hydroxide (TPAOH) solution is 20-40wt%;
tetrahydroxy ammonium hydroxide (TPAOH) volume of Ti 3 AlC 2 3-10 times of the powder;
Ti 3 AlC 2 stirring the powder and tetrahydroxy ammonium hydroxide (TPAOH) at room temperature for 2-4 days;
the solvent used in the mixed solution of cetyltrimethylammonium chloride (CTAC) and Triethanolamine (TEA) is water, and the mass fractions of the cetyltrimethylammonium chloride (CTAC) and the Triethanolamine (TEA) are respectively 5-20wt%; volume of the mixed solution is Ti 3 C 2 T X 5-20 times of the powder;
Ti 3 C 2 T X stirring in a mixed solution of cetyltrimethylammonium chloride (CTAC) and Triethanolamine (TEA) for 1-2 hours;
tetraethoxysilane (TEOS) and Ti 3 C 2 T X The mass ratio of the powder is 1:50-200, preferably in a mass ratio of 1:80-150 parts of;
adding Tetraethoxysilane (TEOS) at 60-100 deg.C, preferably 70-90 deg.C for 0.5-2 hr;
3-Aminopropyltrimethoxysilane (APTES) and MXene @ mSiO 2 The mass ratio of (1): 30-100, preferably 1:50-80 parts of;
3-Aminopropyltrimethoxysilane (APTES) and MXene @ mSiO 2 The reaction temperature is 70-90 ℃, and the reaction time is 8-10h.
In the step [2 ]: the nylon monomer can be one or more of nylon 6, nylon 12, nylon 612, nylon 11, nylon 1012 and the like;
the mass ratio of the nylon monomer to the functionalized MXene is 1000:1-10;
the nylon polymerization process of the step [2] can adopt the conventional reaction conditions in the field; in a specific embodiment, in the step [2], the nylon monomer, the functionalized MXene and the water are added into a reaction kettle to react for 4 hours at 280 ℃ to realize ring opening of the nylon monomer; and then cooling to 260 ℃, vacuumizing to negative pressure, reacting for 3 hours under the negative pressure, filling nitrogen to normal pressure, and discharging to obtain MXene end-capped nylon resin.
In the step [3], the cryogenic grinding method is a conventional process.
The invention has the beneficial effects that:
the light nylon powder with high adhesion and high wear resistance prepared by the invention can be used for preparing powder coating, and compared with the existing powder coating, the end group of the nylon powder contains active groups, so that the adhesion between the powder and metal is improved; meanwhile, compared with graphene, no hydrogen bond exists between layers, the graphene has good interlayer sliding performance, and the wear resistance of the graphene is improved conveniently; in addition, the method benefits from larger intermolecular acting force, has the characteristics of less entanglement, fluffy powder, higher density and light weight.
The powder coating prepared from the nylon powder has great advantages in adhesion, wear resistance and light weight, and is a powder coating with excellent performance.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative of the invention and are not to be construed as limiting the scope of the invention.
The raw materials used in the examples of the present invention may be commercially available, unless otherwise specified.
[ example 1 ]
[1]10g of Ti treated with 30% hydrofluoric acid solution for 2 days 3 AlC 2 Reacting the powder with 5 times volume of tetrahydroxy ammonium hydroxide with the mass fraction of 40% for 2 days to obtain Ti 3 C 2 T X (ii) a Then 10g of Ti 3 C 2 T X Adding the mixture into a mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine with the mass fraction of 20 percent in 5 times of volume, reacting for 1.5 hours at normal temperature, heating to 70 ℃, adding 100mg of tetraethoxysilane, and stirring for 0.5 hour to obtain an intermediate product MXene @ mSiO2; finally 200mg of 3-aminopropyltrimethoxysilane was added to MXene @ mSiO at 70 deg.C 2 Refluxing for 10 hours in the ethanol solution to obtain the amino-functionalized MXene end-capping agent;
[2] adding 1kg of nylon 12 monomer, 5g of functionalized MXene and 5g of water into a reaction kettle, reacting for 4 hours at 280 ℃, then cooling to 260 ℃, vacuumizing to negative pressure, reacting for 3 hours under the negative pressure, filling nitrogen to normal pressure, and discharging to obtain MXene-terminated nylon 12 resin;
[3] the obtained nylon resin is processed into powder by a cryogenic grinding method.
[ example 2]
[1]10g of Ti treated with 30% hydrofluoric acid solution for 2 days 3 AlC 2 Reacting the powder with 5 times of ammonium tetrahydroxy hydroxide with the mass fraction of 20% for 2 days to obtain Ti 3 C 2 T X (ii) a Then 10g of Ti 3 C 2 T X Adding the mixture into a mixed solution of 5% hexadecyl trimethyl ammonium chloride and triethanolamine with the mass fraction of 10 times of the volume of the mixture, reacting for 1 hour at normal temperature, heating to 90 ℃, adding 60mg tetraethoxysilane, and stirring for 1 hour to obtain an intermediate product MXene @ mSiO2; finally 130mg of 3-aminopropyltrimethoxysilane were added to MXene @ mSiO at 90 deg.C 2 Refluxing for 8 hours in the ethanol solution to obtain the amino-functionalized MXene end-capping agent;
[2] adding 1kg of nylon 6 monomer, 9g of functionalized MXene and 5g of water into a reaction kettle, reacting for 4 hours at 280 ℃, then cooling to 260 ℃, vacuumizing to negative pressure, reacting for 3 hours under the negative pressure, filling nitrogen to normal pressure, and discharging to obtain MXene-terminated nylon 6 resin;
[3] the obtained nylon resin is processed into powder by a cryogenic grinding method.
[ example 3]
[1]10g of Ti treated with 30% hydrofluoric acid solution for 2 days 3 AlC 2 Reacting the powder with 5 times of volume of 30% tetrahydroxy ammonium hydroxide for 2 days to obtain Ti 3 C 2 T X (ii) a Then 10g of Ti 3 C 2 T X Adding into the mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine with the mass fraction of 10 percent respectively in 20 times of volume, reacting for 2 hours at normal temperature, heating to 80 ℃, adding 80mg tetraethoxysilane, stirring for 1.5 hours to obtain an intermediate product MXene @ mSiO 2 (ii) a Finally 150mg of 3-aminopropyltrimethoxysilane were added to MXene @ mSiO at 80 deg.C 2 Refluxing for 9 hours in the ethanol solution to obtain the amino-functionalized MXene end-capping agent;
[2] adding 1kg of nylon 11 monomer, 1g of functionalized MXene and 5g of water into a reaction kettle, reacting for 4 hours at 280 ℃, then cooling to 260 ℃, vacuumizing to negative pressure, reacting for 3 hours under the negative pressure, filling nitrogen to normal pressure, and discharging to obtain MXene-terminated nylon 11 resin;
[3] the obtained nylon resin is processed into powder by a cryogenic grinding method.
[ COMPARATIVE EXAMPLES ]
Adding 1kg of nylon 12 monomer, 5g of adipic acid and 5g of water into a reaction kettle, reacting at 280 ℃ for 4 hours, then cooling to 260 ℃, vacuumizing to negative pressure, reacting for 3 hours under the negative pressure, filling nitrogen to normal pressure, and discharging to obtain nylon 12 resin with an adipic acid end cap;
the obtained nylon resin is processed into powder by a cryogenic grinding method.
And (4) performance testing:
the nylon powders prepared in the above examples and comparative examples were tested for abrasion resistance by paint film abrasion test (GB/T15102) (500 times, 0.5 kg), and the results are shown in Table 1 below,
TABLE 1
| Sample (I) | Comparative example | Example 1 | Example 2 | Example 3 |
| Loss case (g) | 0.05 | 0.02 | 0.01 | 0.02 |
It can be seen that the example products have a significant wear advantage over the comparative example products.
The nylon powders prepared in the above examples and comparative examples were tested for adhesion by ISO4624-2016, with the results shown in Table 2:
TABLE 2
| Sample (I) | Comparison ofExample (b) | Example 1 | Example 2 | Example 3 |
| Adhesion (MPa) | 1.52 | 2.27 | 2.36 | 2.05 |
It can be seen that the example products have a clear adhesion advantage over the comparative example products.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and additions can be made without departing from the method of the present invention, and these modifications and additions should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of light nylon powder with high adhesive force and high wear resistance comprises the following steps:
(1) Mixing Ti 3 AlC 2 Functionalizing to obtain amino functionalized MXene;
(2) Adding MXene with functionalized amino as a terminating agent into a nylon polymerization process to obtain MXene terminated nylon resin;
(3) The obtained nylon resin is processed into powder to obtain light nylon powder with high adhesive force and high wear resistance.
2. The method of claim 1, wherein the subjecting Ti 3 AlC 2 Functionalization, comprising:
ti treated by hydrofluoric acid solution 3 AlC 2 Reacting the powder with tetrahydroxy ammonium hydroxide to obtain Ti 3 C 2 T X ；
Mixing Ti 3 C 2 T X Adding the mixture into a mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine, stirring for a period of time, adding tetraethoxysilane for reaction to obtain an intermediate product MXene @ mSiO 2 ；
Addition of 3-aminopropyltrimethoxysilane to MXene @ mSiO 2 And in the solution, refluxing and reacting for a period of time to obtain the amino-functionalized MXene end-capping agent.
3. The method according to claim 2, wherein the concentration of the hydrofluoric acid solution is 30-50wt%, and the treatment time is 2-4 days;
Ti 3 AlC 2 the powder and the tetrahydroxy ammonium hydroxide are stirred and react for 2 to 4 days at room temperature.
4. The method according to claim 2 or 3, wherein the solvent used in the mixed solution of cetyltrimethylammonium chloride and triethanolamine is water, and the mass fractions of the cetyltrimethylammonium chloride and the triethanolamine are 5-20wt% respectively;
preferably, the volume of the mixed solution is Ti 3 C 2 T X 5-20 times of the powder;
preferably, ti 3 C 2 T X Stirring in the mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine for 1-2 hr.
5. The method of any of claims 2-4, wherein tetraethoxysilane is reacted with Ti 3 C 2 T X The mass ratio of the powder is 1:50-200, preferably 1:80-150 parts of;
preferably, the tetraethoxysilane is added at a reaction temperature of 60 to 100 ℃ for a reaction time of 0.5 to 2 hours.
6. The process according to any one of claims 2 to 5, wherein 3-aminopropyltrimethoxysilane is reacted with MXene @ mSiO 2 The mass ratio of (1): 30-100, preferably 1:50-80 parts;
preferred, 3-aminopropyltrimethoxysilane and MXene @ mSiO 2 The reaction temperature is 70-90 ℃, and the reaction time is 8-10h.
7. The method as claimed in any one of claims 1 to 6, wherein in the step (2), the nylon monomer is one or more of nylon 6, nylon 12, nylon 612, nylon 11 and nylon 1012.
8. The method according to any one of claims 1 to 7, wherein in the step (2), the mass ratio of the nylon monomer to the functionalized MXene is 1000:1-10.
9. A nylon powder prepared according to the process of any one of claims 1-8.
10. Use of the nylon powder of claim 9 in the field of powder coatings.
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