CN112662052A - Polypropylene modified material and preparation method thereof - Google Patents
Polypropylene modified material and preparation method thereof Download PDFInfo
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- CN112662052A CN112662052A CN202011344913.7A CN202011344913A CN112662052A CN 112662052 A CN112662052 A CN 112662052A CN 202011344913 A CN202011344913 A CN 202011344913A CN 112662052 A CN112662052 A CN 112662052A
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- -1 Polypropylene Polymers 0.000 title claims abstract description 207
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 116
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 116
- 239000000463 material Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 92
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 92
- 239000000843 powder Substances 0.000 claims abstract description 91
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 84
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 37
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 30
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 7
- 238000012986 modification Methods 0.000 claims abstract description 7
- 239000003365 glass fiber Substances 0.000 claims description 60
- 239000000203 mixture Substances 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 23
- RZQUPONQZIRTME-UHFFFAOYSA-N 1-(4-bicyclo[4.2.0]octa-1(6),2,4,7-tetraenyl)pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=C(C=C2)C2=C1 RZQUPONQZIRTME-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 238000005507 spraying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000010559 graft polymerization reaction Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 32
- 239000011259 mixed solution Substances 0.000 description 24
- 238000009832 plasma treatment Methods 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 230000007306 turnover Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 9
- 239000003063 flame retardant Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000001307 helium Substances 0.000 description 6
- 229910052734 helium Inorganic materials 0.000 description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229910052901 montmorillonite Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 206010000369 Accident Diseases 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005629 polypropylene homopolymer Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a polypropylene modified material and a preparation method thereof, wherein the polypropylene modified material comprises the following raw materials in percentage by mass: 0.5-15% of modified magnesium hydroxide, 0.05-10% of polytetrafluoroethylene micro powder and the balance of polypropylene; the modified magnesium hydroxide is prepared by dry modification of magnesium hydroxide by adopting a silane coupling agent. In the invention, the modified magnesium hydroxide prepared by dry modification of magnesium hydroxide by adopting the silane coupling agent has simple components, convenient manufacture and good flame retardance, can be uniformly dispersed in the polypropylene material, has high compatibility and can improve the mechanical strength of the polypropylene material; the added polytetrafluoroethylene micro powder can not only synergistically enhance the anti-dripping performance of the polypropylene material with the modified magnesium hydroxide, but also reduce the friction coefficient of the polypropylene material, so that the polypropylene material is more wear-resistant.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a polypropylene modified material and a preparation method thereof.
Background
The polypropylene material has excellent comprehensive performance and good chemical resistance, so the polypropylene material is widely used in the industries of packaging, textiles, building materials and the like. However, polypropylene is extremely easy to burn, and strong oxidative cracking can be generated in the burning process, so that molten drops are generated in the burning process, and fire accidents are extremely easy to cause; not only has low safety performance, but also becomes one of the main factors limiting the wider application of polypropylene materials.
In order to make the polypropylene material have flame retardant property, the chinese patent application with publication number CN107383623A discloses a polypropylene flame retardant material and a preparation method thereof, wherein the polypropylene flame retardant material comprises the following raw materials in parts by weight: 350-400 parts of co-polypropylene, 250-300 parts of homo-polypropylene, 80-90 parts of composite flame retardant, 40-60 parts of compatilizer and 5-15 parts of antioxidant; the composite flame retardant is prepared from magnesium hydroxide, nano-montmorillonite, a silane coupling agent and fatty acid, and the preparation method of the composite flame retardant comprises the following steps: mixing magnesium hydroxide and nano montmorillonite, heating to 100-120 ℃, adding a silane coupling agent, reacting while stirring for 10-15 min, cooling to 50-60 ℃, adding fatty acid, stirring uniformly, and cooling to room temperature.
The polypropylene flame-retardant material has the following defects: (1) the adopted composite coupling agent has more complex components and more complicated preparation process; (2) the material has poor anti-dripping performance, so that the flame retardant effect is poor.
Disclosure of Invention
The invention aims to provide a polypropylene modified material with simple components, strong anti-dripping performance and good flame retardant effect and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the polypropylene modified material comprises the following raw materials in percentage by mass: 0.5-15% of modified magnesium hydroxide, 0.05-10% of polytetrafluoroethylene micro powder and the balance of polypropylene;
the modified magnesium hydroxide is prepared by dry modification of magnesium hydroxide by adopting a silane coupling agent.
In the polypropylene modified material, the silane coupling agent is adopted to carry out dry modification on the magnesium hydroxide to prepare the modified magnesium hydroxide, so that the modified magnesium hydroxide has the advantages of simple components, convenient manufacture and good flame retardance, can be uniformly dispersed in the polypropylene material, has oleophylic surface and higher compatibility with polypropylene, and can improve the mechanical strength of the polypropylene material; the added polytetrafluoroethylene micro powder can not only synergistically enhance the anti-dripping performance of the polypropylene material with the modified magnesium hydroxide, but also reduce the friction coefficient of the polypropylene material, so that the polypropylene material is more wear-resistant.
Preferably, in the polypropylene modified material, the modified magnesium hydroxide comprises the following raw materials in percentage by mass: 97-99.9% of magnesium hydroxide and 0.1-3% of silane coupling agent.
Preferably, in the polypropylene modified material, the preparation method of the modified magnesium hydroxide comprises the following steps: preparing the silane coupling agent into a solution, spraying the solution on magnesium hydroxide, and then placing the solution at the temperature of 60-150 ℃ for bridging for 0.5-5 h to obtain the modified magnesium hydroxide. When in use, the silane coupling agent can be prepared into a solution with the volume fraction of 20 percent by adopting absolute ethyl alcohol and then sprayed on the magnesium hydroxide.
Preferably, in the polypropylene-modified material, the silane coupling agent is KH 550.
In the polypropylene modified material, the polytetrafluoroethylene micro powder is modified polytetrafluoroethylene micro powder, and the modified polytetrafluoroethylene micro powder is obtained by grafting the polytetrafluoroethylene micro powder subjected to plasma treatment and N- (benzocyclobutene-4-yl) maleimide under ultraviolet irradiation.
The N- (benzocyclobutene-4-yl) maleimide monomer is grafted on the surface of the polytetrafluoroethylene micro powder, so that the surface activity of the polytetrafluoroethylene micro powder can be improved, the surface free energy of the polytetrafluoroethylene micro powder is enhanced, and the compatibility of the obtained modified polytetrafluoroethylene micro powder and polypropylene is higher.
The polytetrafluoroethylene micro powder can be directly subjected to graft polymerization after being subjected to plasma treatment, so that the step of introducing peroxy radicals by exposing the polytetrafluoroethylene micro powder in the air is omitted; under ultraviolet irradiation, the N- (benzocyclobutene-4-yl) maleimide is not only a photoinitiator for graft polymerization reaction, but also a polymerization monomer, and no additional photoinitiator is required to be introduced into a reaction system, so that the reaction system is simpler, and the post-treatment step is simpler and more convenient.
Preferably, in the polypropylene modified material, the modified polytetrafluoroethylene micro powder is obtained by graft polymerization of the plasma-treated polytetrafluoroethylene micro powder and N- (benzocyclobutene-4-yl) maleimide under 200-400 nm ultraviolet irradiation for 2-120 min.
Preferably, in the polypropylene modified material, the modified polytetrafluoroethylene micro powder comprises the following raw materials in percentage by mass: 95-99.9% of polytetrafluoroethylene micro powder and 0.1-5% of N- (benzocyclobutene-4-yl) maleimide.
Preferably, the polypropylene modified material also comprises 0.5-15% of modified glass fiber in percentage by mass, and the modified glass fiber is prepared by modifying the glass fiber by adopting a silane coupling agent in a dry method. The addition of the glass fiber can improve the hardness, mechanical strength and wear resistance of the polypropylene material, but the glass fiber is not melted in a polypropylene system, so that the silane coupling agent is adopted to modify the glass fiber by a dry method, and the obtained modified glass fiber can be melted in the polypropylene material while the hardness, mechanical strength and wear resistance of the polypropylene material are greatly improved, and the compatibility between the two is higher.
Preferably, in the polypropylene modified material, the preparation method of the modified glass fiber comprises the following steps: preparing the silane coupling agent into a solution, spraying the solution on glass fibers, and then placing the glass fibers at the temperature of 60-150 ℃ for bridging for 0.5-5 hours to obtain the modified glass fibers;
the modified glass fiber comprises the following raw materials in percentage by mass: 97-99.9% of glass fiber and 0.1-3% of silane coupling agent.
Preferably, the polypropylene modified material comprises the following raw materials in percentage by mass: 3.5-8% of modified magnesium hydroxide, 5-10% of modified glass fiber, 3-7% of polytetrafluoroethylene micro powder, and the balance of polypropylene.
The invention also provides a preparation method of the polypropylene modified material, which comprises the following steps:
(1) uniformly mixing the raw materials according to a preset mass percentage, then drying the mixture for 4 to 12 hours at a temperature of between 70 and 110 ℃, and cooling the mixture for later use;
the drying aims at removing moisture and low molecular substances in the raw material mixture, cooling the raw material mixture after drying is finished, and placing the raw material mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into an extruder, blending at the temperature of 250 ℃ and 280 ℃, extruding and granulating to obtain the polypropylene modified material.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the polypropylene modified material, the silane coupling agent is adopted to carry out dry modification on the magnesium hydroxide to prepare the modified magnesium hydroxide, so that the modified magnesium hydroxide has the advantages of simple components, convenient manufacture, good flame retardance, uniform dispersion in the polypropylene material, high compatibility and capability of improving the mechanical strength of the polypropylene material; the added polytetrafluoroethylene micro powder can not only synergistically enhance the anti-dripping performance of the polypropylene material with the modified magnesium hydroxide, but also reduce the friction coefficient of the polypropylene material, so that the polypropylene material is more wear-resistant.
(2) The polytetrafluoroethylene micro powder adopted in the invention is modified polytetrafluoroethylene micro powder, the modified polytetrafluoroethylene micro powder is obtained by grafting the polytetrafluoroethylene micro powder subjected to plasma treatment and N- (benzocyclobutene-4-yl) maleimide under ultraviolet irradiation, and compared with the polytetrafluoroethylene micro powder, the modified polytetrafluoroethylene micro powder has higher compatibility with polypropylene.
(3) The polypropylene modified material also contains modified glass fiber, and the modified glass fiber is prepared by modifying the glass fiber by adopting a silane coupling agent in a dry method; the addition of the glass fiber can improve the hardness, mechanical strength and wear resistance of the polypropylene material, but the glass fiber is not melted in a polypropylene system, so that the silane coupling agent is adopted to modify the glass fiber by a dry method, and the obtained modified glass fiber can be melted in the polypropylene material while the hardness, mechanical strength and wear resistance of the polypropylene material are greatly improved, and the compatibility between the two is higher.
Detailed Description
The technical means of the present invention will be described in further detail below with reference to specific embodiments.
Example 1
The polypropylene modified material comprises the following raw materials in percentage by mass: 6% of modified magnesium hydroxide, 7% of modified glass fiber, 5% of modified polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of magnesium hydroxide was spread in a pan and the solution was sprayed on the magnesium hydroxide; the discs were then placed in an oven and bridged at 100 ℃ for 2h to obtain the modified magnesium hydroxide of this example.
The preparation method of the modified glass fiber comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of glass fiber is spread in a plate, and the solution is sprayed on the glass fiber; the tray was then placed in an oven and bridged at 100 ℃ for 2h to obtain the modified glass fiber of this example.
The preparation method of the modified polytetrafluoroethylene micro powder comprises the following steps: taking 1000g of polytetrafluoroethylene micro powder, and carrying out plasma treatment on the polytetrafluoroethylene micro powder under the atmosphere of helium, wherein the treatment power is 100W, and the treatment time is 90 s; placing the polytetrafluoroethylene micro powder subjected to plasma treatment in a reactor, introducing nitrogen into the reactor to discharge oxygen, and introducing a mixed solution of anhydrous tetrahydrofuran and N- (benzocyclobutene-4-yl) maleimide (5g) into the reactor after the oxygen is exhausted, wherein the introduction amount of the mixed solution is based on the immersion of the polytetrafluoroethylene micro powder;
and after the introduction of the mixed solution is finished, opening an ultraviolet lamp of the reactor, allowing the polytetrafluoroethylene micro powder and the mixed solution to react for 1h under the irradiation of ultraviolet light with the wavelength of 365nm, taking out, washing with deionized water for at least three times, and naturally drying to obtain the modified polytetrafluoroethylene micro powder.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the modified glass fiber, the modified polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to the preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 8 hours to remove moisture and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Example 2
The polypropylene modified material comprises the following raw materials in percentage by mass: 3.5 percent of modified magnesium hydroxide, 10 percent of modified glass fiber, 7 percent of modified polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of magnesium hydroxide was spread in a pan and the solution was sprayed on the magnesium hydroxide; the discs were then placed in an oven and bridged at 60 ℃ for 5h to obtain the modified magnesium hydroxide of this example.
The preparation method of the modified glass fiber comprises the following steps: preparing 30g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; placing 970g of glass fiber in a pan, and spraying the solution on the glass fiber; the tray was then placed in an oven and bridged for 5h at 60 ℃ to obtain the modified glass fiber of this example.
The preparation method of the modified polytetrafluoroethylene micro powder comprises the following steps: taking 1000g of polytetrafluoroethylene micro powder, and carrying out plasma treatment on the polytetrafluoroethylene micro powder under the atmosphere of helium, wherein the treatment power is 100W, and the treatment time is 90 s; placing the polytetrafluoroethylene micro powder subjected to plasma treatment in a reactor, introducing nitrogen into the reactor to discharge oxygen, and introducing a mixed solution of anhydrous tetrahydrofuran and N- (benzocyclobutene-4-yl) maleimide (5g) into the reactor after the oxygen is exhausted, wherein the introduction amount of the mixed solution is based on the immersion of the polytetrafluoroethylene micro powder;
and after the introduction of the mixed solution is finished, opening an ultraviolet lamp of the reactor, allowing the polytetrafluoroethylene micro powder and the mixed solution to react for 1h under the irradiation of ultraviolet light with the wavelength of 365nm, taking out, washing with deionized water for at least three times, and naturally drying to obtain the modified polytetrafluoroethylene micro powder.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the modified glass fiber, the modified polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to the preset mass percentage, uniformly mixing, then placing the mixture into an oven at 70 ℃ for drying for 12 hours to remove moisture and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 250 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Example 3
The polypropylene modified material comprises the following raw materials in percentage by mass: 8% of modified magnesium hydroxide, 5% of modified glass fiber, 3% of modified polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 1g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; spreading 999g of magnesium hydroxide in a pan, and spraying the solution on the magnesium hydroxide; the disc was then placed in an oven and bridged at 150 ℃ for 0.5h to obtain the modified magnesium hydroxide of this example.
The preparation method of the modified glass fiber comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of glass fiber is spread in a plate, and the solution is sprayed on the glass fiber; the tray was then placed in an oven and bridged at 150 ℃ for 0.5h to obtain the modified glass fiber of this example.
The preparation method of the modified polytetrafluoroethylene micro powder comprises the following steps: taking 1000g of polytetrafluoroethylene micro powder, and carrying out plasma treatment on the polytetrafluoroethylene micro powder under the atmosphere of helium, wherein the treatment power is 100W, and the treatment time is 90 s; placing the polytetrafluoroethylene micro powder subjected to plasma treatment in a reactor, introducing nitrogen into the reactor to discharge oxygen, and introducing a mixed solution of anhydrous tetrahydrofuran and N- (benzocyclobutene-4-yl) maleimide (5g) into the reactor after the oxygen is exhausted, wherein the introduction amount of the mixed solution is based on the immersion of the polytetrafluoroethylene micro powder;
and after the introduction of the mixed solution is finished, opening an ultraviolet lamp of the reactor, allowing the polytetrafluoroethylene micro powder and the mixed solution to react for 1h under the irradiation of ultraviolet light with the wavelength of 365nm, taking out, washing with deionized water for at least three times, and naturally drying to obtain the modified polytetrafluoroethylene micro powder.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the modified glass fiber, the modified polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to the preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 110 ℃ for baking for 4 hours to remove moisture and low molecular substances, cooling after baking, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 280 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Example 4
The polypropylene modified material comprises the following raw materials in percentage by mass: 15% of modified magnesium hydroxide, 15% of modified glass fiber, 10% of modified polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of magnesium hydroxide was spread in a pan and the solution was sprayed on the magnesium hydroxide; the discs were then placed in an oven and bridged at 80 ℃ for 2h to obtain the modified magnesium hydroxide of this example.
The preparation method of the modified glass fiber comprises the following steps: preparing 1g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; spreading 999g of glass fiber in a plate, and spraying the solution on the glass fiber; the tray was then placed in an oven and bridged at 80 ℃ for 2h to obtain the modified glass fiber of this example.
The preparation method of the modified polytetrafluoroethylene micro powder comprises the following steps: taking 1000g of polytetrafluoroethylene micro powder, and carrying out plasma treatment on the polytetrafluoroethylene micro powder under the atmosphere of helium, wherein the treatment power is 100W, and the treatment time is 90 s; placing the polytetrafluoroethylene micro powder subjected to plasma treatment in a reactor, introducing nitrogen into the reactor to discharge oxygen, and introducing a mixed solution of anhydrous tetrahydrofuran and N- (benzocyclobutene-4-yl) maleimide (5g) into the reactor after the oxygen is exhausted, wherein the introduction amount of the mixed solution is based on the immersion of the polytetrafluoroethylene micro powder;
and after the introduction of the mixed solution is finished, opening an ultraviolet lamp of the reactor, allowing the polytetrafluoroethylene micro powder and the mixed solution to react for 1h under the irradiation of ultraviolet light with the wavelength of 365nm, taking out, washing with deionized water for at least three times, and naturally drying to obtain the modified polytetrafluoroethylene micro powder.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the modified glass fiber, the modified polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to the preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 3 hours to remove moisture and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Example 5
The polypropylene modified material comprises the following raw materials in percentage by mass: 15 percent of modified magnesium hydroxide, 0.5 percent of modified glass fiber, 0.05 percent of modified polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of magnesium hydroxide was spread in a pan and the solution was sprayed on the magnesium hydroxide; the discs were then placed in an oven and bridged at 80 ℃ for 2h to obtain the modified magnesium hydroxide of this example.
The preparation method of the modified glass fiber comprises the following steps: preparing 30g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; placing 970g of glass fiber in a pan, and spraying the solution on the glass fiber; the tray was then placed in an oven and bridged at 80 ℃ for 2h to obtain the modified glass fiber of this example.
The preparation method of the modified polytetrafluoroethylene micro powder comprises the following steps: taking 1000g of polytetrafluoroethylene micro powder, and carrying out plasma treatment on the polytetrafluoroethylene micro powder under the atmosphere of helium, wherein the treatment power is 100W, and the treatment time is 90 s; placing the polytetrafluoroethylene micro powder subjected to plasma treatment in a reactor, introducing nitrogen into the reactor to discharge oxygen, and introducing a mixed solution of anhydrous tetrahydrofuran and N- (benzocyclobutene-4-yl) maleimide (5g) into the reactor after the oxygen is exhausted, wherein the introduction amount of the mixed solution is based on the immersion of the polytetrafluoroethylene micro powder;
and after the introduction of the mixed solution is finished, opening an ultraviolet lamp of the reactor, allowing the polytetrafluoroethylene micro powder and the mixed solution to react for 1h under the irradiation of ultraviolet light with the wavelength of 365nm, taking out, washing with deionized water for at least three times, and naturally drying to obtain the modified polytetrafluoroethylene micro powder.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the modified glass fiber, the modified polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to the preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 3 hours to remove moisture and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Example 6
The polypropylene modified material comprises the following raw materials in percentage by mass: 6 percent of modified magnesium hydroxide, 5 percent of modified polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of magnesium hydroxide was spread in a pan and the solution was sprayed on the magnesium hydroxide; the discs were then placed in an oven and bridged at 100 ℃ for 2h to obtain the modified magnesium hydroxide of this example.
The preparation method of the modified polytetrafluoroethylene micro powder comprises the following steps: taking 1000g of polytetrafluoroethylene micro powder, and carrying out plasma treatment on the polytetrafluoroethylene micro powder under the atmosphere of helium, wherein the treatment power is 100W, and the treatment time is 90 s; placing the polytetrafluoroethylene micro powder subjected to plasma treatment in a reactor, introducing nitrogen into the reactor to discharge oxygen, and introducing a mixed solution of anhydrous tetrahydrofuran and N- (benzocyclobutene-4-yl) maleimide (5g) into the reactor after the oxygen is exhausted, wherein the introduction amount of the mixed solution is based on the immersion of the polytetrafluoroethylene micro powder;
and after the introduction of the mixed solution is finished, opening an ultraviolet lamp of the reactor, allowing the polytetrafluoroethylene micro powder and the mixed solution to react for 1h under the irradiation of ultraviolet light with the wavelength of 365nm, taking out, washing with deionized water for at least three times, and naturally drying to obtain the modified polytetrafluoroethylene micro powder.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the modified polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to the preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 8 hours to remove water and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Example 7
The polypropylene modified material comprises the following raw materials in percentage by mass: 15% of modified magnesium hydroxide, 5% of polytetrafluoroethylene micro powder and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; spreading 1000g of magnesium hydroxide in a pan, and spraying the solution on the magnesium hydroxide; the discs were then placed in an oven and bridged at 100 ℃ for 2h to obtain the modified magnesium hydroxide of this example.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to a preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 8 hours to remove water and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Comparative example 1
The polypropylene modified material comprises the following raw materials in percentage by mass: 15% of modified magnesium hydroxide, and the balance of polypropylene;
the preparation method of the modified magnesium hydroxide comprises the following steps: preparing 10g of silane coupling agent into a solution with the volume fraction of 20% by using absolute ethyl alcohol; 990g of magnesium hydroxide was spread in a pan and the solution was sprayed on the magnesium hydroxide; the discs were then placed in an oven and bridged at 100 ℃ for 2h to obtain the modified magnesium hydroxide of this example.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to a preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 8 hours to remove water and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
Comparative example 2
The polypropylene modified material comprises the following raw materials in percentage by mass: 15% magnesium hydroxide, the remainder being polypropylene.
The preparation method of the polypropylene modified material of the embodiment comprises the following steps:
(1) putting the modified magnesium hydroxide, the polytetrafluoroethylene micro powder and the polypropylene into a high-speed mixer according to a preset mass percentage, uniformly mixing, then placing the mixture into an oven at the temperature of 80 ℃ for drying for 8 hours to remove water and low molecular substances, cooling after drying, and placing the mixture into a turnover box to keep a dry state for later use;
(2) and (2) feeding the mixture obtained in the step (1) into a screw extruder, blending at 260 ℃, extruding and granulating to obtain the polypropylene modified material of the embodiment.
The polypropylene modified materials prepared in examples 1-7 and comparative examples 1-2 were tested for various properties, and the test results are shown in tables 1 and 2.
TABLE 1
| Test items | Tensile strength | Bending strength | Density of |
| Test standard | GB/T1040.2-2006 | GB/T9341-2008 | GB/T 1033.1-2008 |
| Example 1 | 31.5MPa | 29.5MPa | 1.20g/cm3 |
| Example 2 | 28.1MPa | 26.3MPa | 1.02g/cm3 |
| Example 3 | 28.3MPa | 26.4MPa | 1.03g/cm3 |
| Example 4 | 27.9MPa | 26.1MPa | 1.01g/cm3 |
| Example 5 | 27.5MPa | 25.9MPa | 1.00g/cm3 |
| Example 6 | 22.1MPa | 21.3MPa | 0.99g/cm3 |
| Example 7 | 20.3MPa | 18.7MPa | 0.96g/cm3 |
| Comparative example 1 | 17.7MPa | 16.2MPa | 0.89g/cm3 |
| Comparative example 2 | 15.3MPa | 14.7MPa | 0.86g/cm3 |
TABLE 2
| Test items | Oxygen index | Amount of wear | Melt index |
| Test standard | GB/T2406.2-2009 | ASTM 4060-2014 | ASTM-D-1238 |
| Example 1 | 27.2％ | 143.8mg | 1.12g/min |
| Example 2 | 23.7％ | 147.6mg | 1.14g/min |
| Example 3 | 23.2％ | 147.9mg | 1.15g/min |
| Example 4 | 22.0％ | 152.3mg | 1.14g/min |
| Example 5 | 21.7％ | 153.1mg | 1.16g/min |
| Example 6 | 21.1％ | 159.4mg | 1.16g/min |
| Example 7 | 20.8％ | 164.8mg | 1.73g/min |
| Comparative example 1 | 18.8％ | 192.6mg | 3.37g/min |
| Comparative example 2 | 18.2％ | 214.8mg | 3.92g/min |
Claims (10)
1. The polypropylene modified material is characterized by comprising the following raw materials in percentage by mass: 0.5-15% of modified magnesium hydroxide, 0.05-10% of polytetrafluoroethylene micro powder and the balance of polypropylene;
the modified magnesium hydroxide is prepared by dry modification of magnesium hydroxide by adopting a silane coupling agent.
2. The polypropylene modified material of claim 1, wherein the modified magnesium hydroxide comprises the following raw materials in percentage by mass: 97-99.9% of magnesium hydroxide and 0.1-3% of silane coupling agent.
3. The polypropylene modified material of claim 1, wherein the modified magnesium hydroxide is prepared by a process comprising: preparing the silane coupling agent into a solution, spraying the solution on magnesium hydroxide, and then placing the solution at the temperature of 60-150 ℃ for bridging for 0.5-5 h to obtain the modified magnesium hydroxide.
4. The polypropylene modified material according to any one of claims 1 to 3, wherein the silane coupling agent is KH 550.
5. The polypropylene modified material according to any one of claims 1 to 3, wherein the polytetrafluoroethylene fine powder is modified polytetrafluoroethylene fine powder obtained by grafting plasma-treated polytetrafluoroethylene fine powder with N- (benzocyclobutene-4-yl) maleimide under ultraviolet irradiation.
6. The polypropylene modified material according to claim 5, wherein the modified polytetrafluoroethylene micro powder is obtained by graft polymerization of plasma-treated polytetrafluoroethylene micro powder and N- (benzocyclobutene-4-yl) maleimide under 200-400 nm ultraviolet irradiation for 2-120 min.
7. The polypropylene modified material of claim 5, wherein the modified polytetrafluoroethylene micropowder comprises the following raw materials in percentage by mass: 95-99.9% of polytetrafluoroethylene micro powder and 0.1-5% of N- (benzocyclobutene-4-yl) maleimide.
8. The polypropylene modified material according to any one of claims 1 to 3 and 6 to 7, further comprising 0.5 to 15 mass% of modified glass fiber, wherein the modified glass fiber is prepared by dry modification of glass fiber with a silane coupling agent.
9. The polypropylene modified material of claim 8, wherein the preparation method of the modified glass fiber comprises the following steps: preparing the silane coupling agent into a solution, spraying the solution on glass fibers, and then placing the glass fibers at the temperature of 60-150 ℃ for bridging for 0.5-5 hours to obtain the modified glass fibers;
the modified glass fiber comprises the following raw materials in percentage by mass: 97-99.9% of glass fiber and 0.1-3% of silane coupling agent.
10. The process for the preparation of polypropylene modified material according to any one of claims 1 to 9, comprising the steps of:
(1) uniformly mixing the raw materials according to a preset mass percentage, then drying the mixture for 4 to 12 hours at a temperature of between 70 and 110 ℃, and cooling the mixture for later use;
(2) and (2) feeding the mixture obtained in the step (1) into an extruder, blending at the temperature of 250 ℃ and 280 ℃, extruding and granulating to obtain the polypropylene modified material.
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