CN115819788B - 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 56
- 239000004677 Nylon Substances 0.000 title claims abstract description 43
- 229920001778 nylon Polymers 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 claims abstract description 21
- 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 12
- 230000001070 adhesive effect Effects 0.000 claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 239000002981 blocking agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 14
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 14
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- GAQUIYRRYYKVMJ-UHFFFAOYSA-M tetrahydroxyazanium;hydroxide Chemical compound [OH-].O[N+](O)(O)O GAQUIYRRYYKVMJ-UHFFFAOYSA-M 0.000 claims description 9
- 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
- 229920000571 Nylon 11 Polymers 0.000 claims description 4
- 229920002292 Nylon 6 Polymers 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 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 10
- 238000000227 grinding Methods 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 238000007306 functionalization reaction Methods 0.000 abstract description 3
- 125000003277 amino group Chemical group 0.000 abstract 1
- 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 10
- 239000011248 coating agent Substances 0.000 description 10
- 229910021389 graphene Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 229920001169 thermoplastic Polymers 0.000 description 6
- 239000004416 thermosoftening plastic Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000005299 abrasion Methods 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
- 238000010992 reflux Methods 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 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
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 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
- 238000013461 design Methods 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
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003902 lesion Effects 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
- 238000011056 performance test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
The invention relates to a lightweight nylon powder with high wear resistance and high adhesive force performance and a method for preparing the powder. The method comprises the following steps: first, ti is 3 AlC 2 Functionalization to obtain an amino group-containing MXene material which can be used as a capping agent; secondly, adding the functionalized MXene serving as a blocking agent into a nylon polymerization process to obtain MXene blocked 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 adhesive force and high wear resistance, belonging to the category of special engineering plastics.
Background
MXene, a new two-dimensional material, is composed of several atomic layer thick transition metal carbides, nitrides or carbonitrides, which was originally present in 2011. Because of the hydroxyl groups or terminal oxygen on the surface of the MXene materials, the MXene materials have metal conductivity of transition metal carbide, and are increasingly widely applied to supercapacitors, batteries, electromagnetic interference shielding, composite materials and the like. Different from the surface of two-dimensional materials such as graphene and transition dihalide carbon, the functional groups of the two-dimensional materials can be chemically modified, and the surface of the two-dimensional materials can be provided with active groups through functional design, so that the adhesive force between powder and metal can be improved conveniently; meanwhile, compared with graphene, the graphene has no hydrogen bond between layers, so that the graphene has good interlayer sliding performance, and the abrasion resistance of the graphene is improved conveniently.
Powder coatings can be classified into thermoplastic and thermosetting powder coatings, wherein thermosetting powder coatings have the advantage of being well leveled and strongly coated compared to thermoplastic powder coatings, but cannot be reused inevitably, which is the most hard lesion limiting its application. The thermoplastic powder is not increased in molecular weight, so that the thermoplastic powder is required to have larger molecular weight initially to ensure the mechanical property of the coating, but the leveling property of the coating is limited, and the preparation of the thermoplastic powder which can ensure the mechanical property of the material and can be well leveled has great market prospect.
Nylon powder, which is one of thermoplastic powders, occupies an increasing market share in the powder coating field, which is based on the lower density, excellent mechanical properties, low temperature properties, and corrosion resistance of nylon materials.
The nylon powder coating is mainly applied to household appliances and automobiles, so that the nylon powder coating has high requirements on the adhesive force, the wear-resisting effect and the light weight of materials.
Disclosure of Invention
The invention aims to provide the light nylon powder with high adhesive force and high wear resistance, which meets the adhesive force performance of powder coating, has the characteristics of high wear resistance and light weight, and has 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]ti is mixed with 3 AlC 2 Functionalization to obtain amino-functionalized MXene;
[2] adding the functionalized MXene as a blocking agent into a nylon polymerization process to obtain MXene blocked nylon resin;
[3] the obtained nylon resin is processed into powder by a cryogenic grinding method, so that the lightweight nylon powder with high wear resistance and high adhesive force performance is obtained.
Said step [1 ]]In the above, theTi is mixed with 3 AlC 2 Functionalization, comprising:
ti to be treated with hydrofluoric acid solution 3 AlC 2 Reacting the powder with tetra-hydroxy ammonium hydroxide (TPAOH) to obtain Ti 3 C 2 T X ;
Then Ti is added 3 C 2 T X Adding into a mixed solution of Cetyl Trimethyl Ammonium Chloride (CTAC) and Triethanolamine (TEA), stirring for a period of time, and adding Tetraethoxysilane (TEOS) to react to obtain an intermediate product MXene@mSiO 2 ;
Finally, 3-aminopropyl trimethoxysilane (APTES) is added to MXene@mSiO 2 Reflux-reacting for a period of time to obtain an 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%;
the volume of the tetrahydroxy ammonium hydroxide (TPAOH) is Ti 3 AlC 2 3-10 times of powder;
Ti 3 AlC 2 reacting the powder with tetrahydroxy ammonium hydroxide (TPAOH) at room temperature under stirring for 2-4 days;
the solvent used in the mixed solution of Cetyl Trimethyl Ammonium Chloride (CTAC) and Triethanolamine (TEA) is water, and the mass fractions of the Cetyl Trimethyl Ammonium Chloride (CTAC) and the Triethanolamine (TEA) are 5-20wt% respectively; the volume of the mixed solution is Ti 3 C 2 T X 5-20 times of powder;
Ti 3 C 2 T X stirring in a mixture 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 with a mass ratio of 1:80-150;
the reaction temperature of Tetraethoxysilane (TEOS) is 60-100 ℃, preferably 70-90 ℃ and the reaction time is 0.5-2 hours;
3-aminopropyl trimethoxysilane (APTES) with MXene@mSiO 2 The mass ratio of (2) is 1:30-100, preferably 1:50-80;
3-aminopropyl trimethoxysilane (APTES) with 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;
step [2] the nylon polymerization process may employ reaction conditions conventional in the art; in a specific embodiment, in the step [2], nylon monomer, functionalized MXene and water are added into a reaction kettle to react for 4 hours at 280 ℃ so as to realize the ring opening of the nylon monomer; then cooling to 260 ℃, vacuumizing to negative pressure, keeping the reaction for 3 hours under the negative pressure, charging nitrogen to normal pressure, and discharging to obtain the 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 invention prepares the high-adhesion high-wear-resistance light nylon powder, can be used for preparing powder coating, and compared with the existing powder coating, the end group of the powder coating contains active groups, so that the adhesion between the powder and metal is improved; meanwhile, compared with graphene, the graphene has no hydrogen bond between layers, so that the graphene has good interlayer sliding performance, and the abrasion resistance of the graphene is improved conveniently; in addition, the powder is benefited by larger intermolecular acting force, less entanglement, fluffy powder, larger density and light weight.
The powder coating prepared from the nylon powder has great advantages in adhesive force, wear resistance and light weight, and is excellent in performance.
Detailed Description
The invention will now be further illustrated by means of specific examples which are given solely by way of illustration of the invention and do not limit the scope thereof.
The raw materials used in the examples of the present invention are 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 tetrahydroxy ammonium hydroxide with a mass fraction of 40% by volume of 5 times for 2 days to obtain Ti 3 C 2 T X The method comprises the steps of carrying out a first treatment on the surface of the Then 10g of Ti 3 C 2 T X Adding the mixture into a mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine, wherein the mass fraction of the mixture is 20% in volume and the volume of the mixture is respectively, 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-aminopropyl trimethoxysilane are added to MXene@mSiO at 70 DEG C 2 Refluxing for 10 hours to obtain an 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, keeping the negative pressure for reacting for 3 hours, charging nitrogen to normal pressure, and discharging to obtain MXene-terminated nylon 12 resin;
[3] the nylon resin obtained was processed into powder by cryogenic grinding.
[ 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 tetrahydroxy ammonium hydroxide with mass fraction of 20% for 2 days to obtain Ti 3 C 2 T X The method comprises the steps of carrying out a first treatment on the surface of the Then 10g of Ti 3 C 2 T X Adding the mixture into mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine, wherein the mass fraction of the mixture is 5% of that of the mixture, reacting for 1 hour at normal temperature, heating to 90 ℃, adding 60mg of tetraethoxysilane, and stirring for 1 hour to obtain an intermediate product MXene@mSiO2; finally 130mg of 3-aminopropyl trimethoxysilane are added to MXene@mSiO at 90 ℃ 2 Refluxing for 8 hours to obtain an 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, keeping the negative pressure for reacting for 3 hours, charging nitrogen to normal pressure, and discharging to obtain MXene-terminated nylon 6 resin;
[3] the nylon resin obtained was processed into powder by cryogenic grinding.
[ 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 tetrahydroxy ammonium hydroxide with mass fraction of 30% for 2 days to obtain Ti 3 C 2 T X The method comprises the steps of carrying out a first treatment on the surface of the Then 10g of Ti 3 C 2 T X Adding into mixed solution of hexadecyl trimethyl ammonium chloride and triethanolamine with the mass fraction of 10% of 20 times of the volume of the mixed solution, reacting for 2 hours at normal temperature, heating to 80 ℃, adding 80mg of tetraethoxysilane, and stirring for 1.5 hours to obtain an intermediate product MXene@mSiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Finally 150mg of 3-aminopropyl trimethoxysilane were added to MXene@mSiO at 80 ℃ 2 Refluxing for 9 hours to obtain an 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 to react for 4 hours at 280 ℃, then cooling to 260 ℃, vacuumizing to negative pressure, keeping the negative pressure to react for 3 hours, charging nitrogen to normal pressure, and discharging to obtain MXene-terminated nylon 11 resin;
[3] the nylon resin obtained was processed into powder by cryogenic grinding.
[ comparative example ]
Adding 1kg of nylon 12 monomer, 5g of adipic acid and 5g of water into a reaction kettle to react for 4 hours at 280 ℃, then cooling to 260 ℃, vacuumizing to negative pressure, keeping the negative pressure to react for 3 hours, charging nitrogen to normal pressure, and discharging to obtain adipic acid-terminated nylon 12 resin;
the nylon resin obtained was processed into powder by cryogenic grinding.
Performance test:
the nylon powders prepared in the above examples and comparative examples were tested for abrasion resistance by the paint film abrasion test (GB/T15102) (500 times, 0.5 kg), and the results are shown in Table 1 below,
TABLE 1
Sample of | Comparative example | Example 1 | Example 2 | Example 3 |
Loss condition (g) | 0.05 | 0.02 | 0.01 | 0.02 |
It can be seen that the example product has a significant wear advantage over the comparative example product.
The nylon powders prepared in the above examples and comparative examples were tested for adhesion by ISO4624-2016 and the results are shown in table 2:
TABLE 2
Sample of | Comparative example | Example 1 | Example 2 | Example 3 |
Adhesive force (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 foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and additions may be made to those skilled in the art without departing from the method of the present invention, which modifications and additions are also to be considered as within the scope of the present invention.
Claims (12)
1. A preparation method of high-adhesion and high-wear-resistance light nylon powder comprises the following steps:
(1) Ti to be treated with hydrofluoric acid solution 3 AlC 2 Reacting the powder with tetrahydroxy ammonium hydroxide to obtain Ti 3 C 2 T X ;
Ti is mixed with 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, and then adding tetraethoxysilane to react to obtain an intermediate product MXene@mSiO 2 ;
Adding 3-aminopropyl trimethoxysilane to MXene@mSiO 2 Reflux-reacting for a period of time in the solution to obtain amino-functionalized MXene;
(2) Adding an amino-functionalized MXene as a blocking agent into a nylon polymerization process to obtain an MXene-blocked nylon resin;
(3) And processing the obtained nylon resin into powder to obtain the light nylon powder with high adhesive force and high wear resistance.
2. The method according to claim 1, 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 was reacted with tetrahydroxy ammonium hydroxide at room temperature with stirring for 2-4 days.
3. The method according to claim 1, wherein the solvent used in the mixed solution of cetyltrimethylammonium chloride and triethanolamine is water, and the mass fractions of the two are 5-20wt% respectively.
4. A method according to claim 3, wherein the volume of the mixed liquor is Ti 3 C 2 T X 5-20 times of (3);
Ti 3 C 2 T X stirring in the mixture of cetyltrimethylammonium chloride and triethanolamine for 1-2 hours.
5. The method of claim 1, wherein tetraethoxysilane is combined with Ti 3 C 2 T X The mass ratio of (2) is 1:50-200 parts;
the reaction temperature of the tetraethoxysilane is 60-100 ℃ and the reaction time is 0.5-2 hours.
6. The method of claim 5, wherein tetraethoxysilane is used with Ti 3 C 2 T X The mass ratio of (2) is 1:80-150.
7. The method of claim 1, wherein 3-aminopropyl trimethoxysilane is reacted with MXene@mSiO 2 The mass ratio of (2) is 1:30-100;
3-aminopropyl trimethoxysilane with MXene@mSiO 2 The reaction temperature is 70-90 ℃ and the reaction time is 8-10h.
8. The method of claim 7, wherein 3-aminopropyl trimethoxysilane is mixed with MXene@mSiO 2 The mass ratio of (2) is 1:50-80.
9. The method of claim 1, wherein in step (2), the nylon monomer is one or more of nylon 6, nylon 12, nylon 612, nylon 11, and nylon 1012.
10. The method of any one of claims 1-9, wherein in step (2), the mass ratio of nylon monomer to functionalized MXene is 1000:1-10.
11. Nylon powder prepared according to the method of any one of claims 1-10.
12. Use of the nylon powder according to claim 11 in the field of powder coatings.
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CN114855442A (en) * | 2022-05-13 | 2022-08-05 | 青岛科技大学 | MXene-based conductive self-cleaning composite fabric for electromagnetic shielding and preparation method thereof |
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A novel coating with SiO2 anchored on MXene loading tannic acid for self-healing anticorrosive performance;Xiaoguang Sun,等;《Journal of Alloys and Compounds》;第928卷;第167202页 * |
MXene/SiO2杂化材料及其丁苯橡胶复合材料的研究;朱淑丽;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》(第02期);第B020-601页 * |
石墨烯与MXene的制备及石墨烯改性涂料性能的研究;李亚洲;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》(第12期);第B015-96页 * |
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