CN108456317B - Method for preparing polar polymer powder by low-temperature plasma - Google Patents
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Abstract
The invention provides a method for preparing polar polymer powder by low-temperature plasma, which comprises the steps of placing nonpolar polymer powder into a reactor, and charging OH which can be electrically shocked out into the reactor‑、NH2 ‑、CL‑Or F‑The non-polar polymer powder reacts with the plasma which is struck out, so that the surface of the polymer powder has stronger and stable polar groups, and the modification by adding the polymer powder into a matrix is facilitated. The polymer powder with polarity on the surface prepared by the method has a porous structure on the microscopic surface and is grafted with reactive active functional groups, and the effect of the method is permanent modification, so that the modification effect cannot be lost due to high temperature, use environment and storage conditions. The material prepared by the invention can be used as an additive to be added into a polar material,and the material and the base material form good interface connection, and the material is used as a framework reinforcing material to improve specific or comprehensive properties of the material, such as wear resistance, tensile property, tearing property, corrosion resistance and the like.
Description
Technical Field
The invention belongs to the technical field of polymer additive preparation, and particularly relates to a method for preparing polar polymer powder by using low-temperature plasma.
Background
Some polymer materials, such as ultra-high molecular weight polyethylene, high density polyethylene, polypropylene, polyester, polyvinyl chloride, nylon, etc., have good physical and chemical properties, such as low coefficient of friction, high molecular weight, abrasion resistance, chemical resistance, aging resistance, the powder can theoretically strengthen the related performance of the material (for example, 10 to 20 percent of additive can improve the wear resistance of the rubber material by 50 percent, the corrosion resistance by 30 percent, the tear resistance by 30 percent and the service life by 300 percent) as the additive of other materials (for example, rubber, paint and the like), however, these polymer powders are non-polar materials, are not easily dispersed in polar substrates, have poor interfacial properties with substrates, even if the material is added into a base material, the material is easy to fall off and cannot play the expected role, and the physical and mechanical properties of other materials can be damaged. Moreover, some polymers have particularly stable structures, and the graft modification of the polymers is difficult. The application of these polymeric materials to other materials for modification is very limited in the prior art.
The surface modification methods of the additives commonly used at present comprise the following steps: silane modification, maleic anhydride grafting modification, copolymerization modification and other modes are adopted to coat the surface of the additive with a polar functional group. However, the above modification effects are unstable, and in a high-temperature environment or under poor storage conditions, the coated functional group with polarity is easily broken, and modification is ineffective.
The invention provides a method for solving the defects in the prior art.
Disclosure of Invention
The invention aims to provide a method for preparing polar polymer powder by low-temperature plasma, and the method obtains good effect by selecting a plurality of specific plasmas to modify related polymers. Compared with the conventional grafting technology, the method has the advantages of good grafting effect, high infiltration performance improvement degree and lasting effect.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for preparing polar polymer powder by low-temperature plasma comprises the following steps:
step (1), adding the nonpolar polymer powder into a vacuum reactor for heating, and heating to 80-400 ℃;
step (2), after heating, vacuumizing the vacuum reactor to be less than or equal to-0.09 MPA;
step (3), after vacuumizing, filling reaction gas into the reactor until the reaction gas reaches-0.08 MPA to 0.1MAP, wherein the reaction gas
The body generates OH under electric shock-、NH2 -、CL-Or F-One or more plasma gases.
Step (4), after reaction gas is filled, generating electricity for the reactor by using a radio frequency discharge electrode, wherein the discharge voltage is 20-200
Kilovolt, discharge power of 2-5W/m3For a duration of 10 minutes to 5 hours;
step (5), after the discharge is finished, vacuumizing the reactor to be less than or equal to-0.09 MPA, and filling inert gas into the reactor after the vacuum is vacuumized
The temperature is reduced to normal pressure.
Further, the reaction gas in the step (3) is a mixed gas, the mixed gas is a mixed gas of a first gas and a second gas, the first gas is one of carbon tetrachloride, methane chloride, carbon tetrafluoride, sulfur hexafluoride and nitrogen trifluoride, and the second gas is ammonia gas or alcohol vapor, and may be one or more of methanol, ethanol and other alcohol gases.
Further, the volume ratio of the first type gas to the second type gas in the step (3) is less than 10: 1.
further, the vacuum reactor in the step (1) is a static reactor, and the thickness of the nonpolar polymer powder added into the reactor is not more than 3 mm.
Further, the vacuum reactor in the step (1) is a rotary kiln reactor.
Further, in the step (4), the reactor is rotated.
Further, the step (1) is carried out under the heating temperature, namely, inert gas is filled to one atmospheric pressure, then, the vacuum pumping is carried out until the pressure in the step (2), and the step (3) is carried out after the steps of stamping and the vacuum pumping are sequentially repeated for 2-3 times.
Further, the step (5) is repeated 1 to 3 times.
Further, the nonpolar polymer powder in the step (1) is polypropylene (PP) powder, Polyethylene (PE) powder, high-density polyethylene (HDPE) powder, ultra-high molecular weight polyethylene (UHMPWE) powder, low-density polyethylene (LDPE) powder, aramid powder or polyimide powder, and the average particle size of the selected nonpolar polymer powder is less than 150 μm.
Further, the heating temperature in the step (1) is higher than the boiling point of the reaction gas charged in the step (3) and lower than the melting point of the charged nonpolar polymer powder.
The invention has the beneficial effects that:
the polymer powder with polar surface prepared by the method has a porous structure on the microscopic surface and is grafted with reactive active functional groups, and the effect of the method is permanent modification, so that the modification effect cannot be lost due to high temperature, use environment and storage condition. The material prepared by the method can be used as an additive to be added into a polar material to form good interface connection with a base material, and can be used as a framework reinforcing material to improve specific or comprehensive properties of the material, such as wear resistance, tensile property, tearing resistance, corrosion resistance and the like.
Drawings
FIG. 1 is a graph showing a comparison of wetting effects before and after processing a polymer powder by a method of preparing a polar polymer powder using a low temperature plasma;
FIG. 2 is a scanning electron microscope microstructure before and after processing polymer powder by using low temperature plasma to prepare polar polymer powder.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below.
A method for preparing polar polymer powder by low-temperature plasma comprises the following steps:
step (1), adding the nonpolar polymer powder into a vacuum reactor for heating, wherein the heating temperature is 80-400 ℃; the specific reaction temperature is determined according to the reaction gases added next, the boiling points of some reaction gases, such as carbon tetrachloride, are close to 80 ℃, the reaction substances can be ensured to be in a gasification state at the temperature of more than 80 ℃, the activity of the plasma at higher temperature is higher, the reaction can be fully carried out, but the reaction temperature is lower than the melting point of powder, such as the melting point of PP (polypropylene) is about 165 ℃, the melting point of HDPE (high-density polyethylene) is about 140 ℃, and the melting point of polyimide is … … as high as more than 400 ℃;
step (2), after heating, vacuumizing the vacuum reactor to be less than or equal to-0.09 MPA; the step can not only extract residual gas in the vacuum reactor, but also provide a vacuum state for the reactor;
step (3), after vacuumizing, filling reaction gas into the reactor to-0.08 MPA to 0.1MPA, wherein the reaction gas is OH-NH generated under electric shock2One or more of CL-, or F-, of the plasma. The reaction gas capable of generating the plasma is one of carbon tetrachloride, methane chloride, carbon tetrafluoride, sulfur hexafluoride or nitrogen trifluoride, or alcohol gas and ammonia gas; more preferably, the reaction gas in the step (3) is a mixed gas, the mixed gas is a mixed gas of a first gas and a second gas, the first gas is one of carbon tetrachloride, methyl chloride, carbon tetrafluoride, sulfur hexafluoride and nitrogen trifluoride, and the second gas is an alcohol gas or ammonia gas, i.e. one or more of methanol, ethanol and other alcohol gases; generally, the pressure difference between the inside and the outside of the reactor is about 0MPA when the gas is filled to the normal pressure, and if the reactor can bear the pressure, the pressure can be filled to 0.1MPA so as to ensure that the active plasma with higher concentration can be generated;
when the step (2) and the step (3) are carried out, the reactor needs to be heated continuously at constant temperature, and reaction temperature conditions are provided for adding reaction gas next time.
And (4) after reaction gas is filled, discharging the reactor by using a radio frequency discharge electrode, wherein the discharge voltage is 20-200 kilovolts, and the discharge power is 2-5W/m3For a duration of 10 minutes to 5 hours; in the step, the reaction gas generates plasma under the electric shock, and the plasma reacts with the nonpolar polymer powder under the temperature and the pressure kept by the reactor to generate a required product;
the principle is as follows: namely, the reactor is ionized to contain OH after electric shock-、NH2 -、CL-Or F-One or more kinds of plasma (depending on the kind of reaction gas); these plasmas have strong activity and electronegativity, especially OH-Or NH2 -Can promote some C-H bonds on the surface of the polymer to be broken, and the broken C-H bonds and plasma are formedReactive C-OH, C-NH2，CL-Or F-Bonds with strong bond energy such as C-Cl, C-F and the like can be generated on the surface of the polymer, and the newly generated bonds have strong polarity, so that the surface of the polymer can be polarized.
Meanwhile, the plasma also has an etching effect on the surface of the powder, so that the specific surface area of the powder is increased (the specific surface area can be observed from a microstructure, and an electron microscope picture 2 is provided), and the wetting performance of the powder and a base material in the future can be further improved;
and (5) after the discharge is finished, vacuumizing the reactor to be less than or equal to-0.09 MPA, and filling inert gas to be normal pressure after vacuumizing. The step is to remove gas impurities remained in the reaction, and overflow when the reactor is opened in the reaction to pollute the environment.
Preferably, the reaction gas in the step (3) is a mixed gas, the mixed gas is a mixed gas of a first gas and a second gas, the first gas is one of carbon tetrachloride, methyl chloride, carbon tetrafluoride, sulfur hexafluoride and nitrogen trifluoride, and the second gas is one or more of alcohol vapor, methanol, ethanol, other alcohol gas or ammonia gas. The first type of gas can produce CL in ionization-Or F-Plasma, the second type of gas can generate OH in ionization-Or NH2 -Plasma is generated.
Preferably, the volume ratio of the first type gas to the second type gas in the step (3) is not less than 10: 1. ensuring CL-or F-Plasma and OH-Or NH2 -The concentration ratio of the plasma is constant, and OH grafted on the surface of the powder is ensured-Or NH2 -The plasma is not excessive. If OH is present-Or NH2 -Excessive plasma concentration will affect the reactivity of the modified powder and thus the further use of the product.
In the technical scheme, the vacuum reactor in the step (1) can be a static reactor, and in order to increase the contact area of the polymer powder and the reaction gas, the thickness of the polymer powder added into the reactor is not more than 3 mm.
Or in the step (1), the vacuum reactor is selected from a rotary kiln reactor. The rotary kiln reactor has the advantages that the powder can be turned over in the reactor to fully react with the plasma, and the rotary kiln reactor is suitable for industrial production;
if a rotary kiln reactor is selected, the rotary kiln reactor is rotated in step (4).
Preferably, the stamping is carried out at the heating temperature in the step (1), namely, inert gas is filled to one atmosphere, then the vacuum pumping is carried out until the pressure in the step (2), and the step (3) is carried out after the stamping and the vacuum pumping are sequentially repeated for 2-3 times. Namely, the heating state in the step (1) is kept during the stamping and the vacuum pumping, and the constant temperature of the reactor is controlled as much as possible. The operation of punching and vacuumizing for many times in the scheme can more fully remove residual gas impurities in the reactor.
Preferably, step (5) is repeated 1-3 times. And (3) repeating the step (5) for multiple times can better remove residual reaction gas in the reactor.
In the above technical scheme, the nonpolar polymer powder in step (1) may be selected from PP powder, PE powder, HDPE powder, UHMPWE powder, LDPE powder, aramid powder or polyimide powder, and the average particle size of the nonpolar polymer powder may be selected to be less than 150 μm. If the particle size of the powder is larger than 150 μm, the powder can be used as an additive to affect the appearance or performance of downstream products.
In the above technical solution, the heating temperature in step (1) is higher than the boiling point of the reaction gas charged in step (3), i.e. higher than the boiling point of the gas with the highest boiling point in the mixed gas, and lower than the melting point of the added non-polar polymer powder.
The first embodiment is as follows: modification of ultra-high molecular weight polyethylene (UHMWPE) powder
Raw materials: ultra-high molecular weight polyethylene powder brand: the Mitsui chemical trade mark 240S has an average particle size of 120 μm and a molecular weight of 200 ten thousand.
1)100g of raw materials are placed in a tray, flatly laid in a static reactor and 20L of reactor volume;
2) the reactor was heated to 100 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium into the reactor to normal pressure;
5) repeating the step 3) and the step 4) twice in sequence; the reactor is continuously heated in the process, and the heating target temperature is kept at 100 ℃; maintaining the temperature of the reactor to provide a temperature environment for the subsequent reaction;
6) evacuating the reactor to-0.09 MPa;
7) charging nitrogen trifluoride (NF) into the reactor3) (purity of>99.99%) gas and ammonia (NH)3) (purity of>99.99%) of mixed gas here NF3：NH3The volume ratio of the mixed gas is 10:1 to normal pressure;
8) the radio frequency power supply electrode discharges in the reactor with the discharge power of 2W/m3For a duration of 20 minutes;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9 and the step 10 twice in sequence;
12) opening the reactor and taking out the materials;
13) the wettability test is carried out by the dyne liquid, and at this time, the ultra-high molecular weight polyethylene powder can be wetted by the dyne liquid with the reference number of 52, which shows that the surface energy of the powder is more than 52 mN/m.
Example two: modification of High Density Polyethylene (HDPE) powder
Raw materials: high density polyethylene powder brand: mitsui chemical designation 1105A has a density of 0.99g/cc melting point of 137 deg.C.
1)100g of raw materials are placed in a tray, flatly laid and placed in a rotary kiln reactor, and the volume of the reactor is 20L;
2) the reactor was heated to 100 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium into the reactor to normal pressure;
5) repeating the step 3) and the step 4) in sequence once; the reactor is continuously heated in the process, the heating target temperature is kept at 100 ℃, the temperature of the reactor is kept, and a temperature environment is provided for the next reaction;
6) evacuating the reactor to-0.09 MPa;
7) charging into reactor to obtain monochloromethane (CH)3CL) (purity)>99.99%), and methanol vapor (CH)3OH) (purity)>99.99 percent) to normal pressure, and the molar mass ratio of the charged methane chloride and the methanol is 10: 1;
8) discharging the radio frequency power supply electrode in the reactor, wherein the discharge power is 2W/cm3, and the duration is 10 minutes;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9 and the step 10 in sequence once;
12) opening the reactor and taking out the materials;
13) the wettability test is carried out by the dyne liquid, and at this time, the high-density polyethylene micropowder can be wetted by the dyne liquid with the reference number of 52, which shows that the surface energy of the powder is greater than 52 mN/m.
Example three: modification of Polyethylene (PE) wax powder
Raw materials: polyethylene wax powder brand: the Tianshi brand PEW-0202 has an average particle size of 16 mu m and a melting point of 110 ℃.
1)100g of raw materials are placed in a tray, flatly laid in a static reactor and 20L of reactor volume;
2) the reactor was heated to 80 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium gas into the reactor to normal pressure;
5) repeating the step 3 and the step 4 in sequence twice; the reactor is continuously heated in the process, the heating target temperature is kept at 80 ℃, the temperature of the reactor is kept, and a temperature environment is provided for the next reaction;
6) evacuating the reactor to-0.09 MPa;
7) charging into a reactor nitrogen trifluoride (NF)3) (purity of>99.99%), and ammonia (NH)3) (purity of>99.99%) to normal pressure, and the molar mass ratio of the charged nitrogen trifluoride and ammonia gas is 10: 1;
8) the radio frequency power supply electrode discharges in the reactor with the discharge power of 2W/m3Hand holdingThe time is prolonged for 40 minutes;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9-10 once;
12) opening the reactor and taking out the materials;
13) the wettability test with a dyne liquid was carried out, at which time the polyethylene powder was wettable with a dyne liquid numbered 52, indicating that the surface energy of the powder was >46 mN/m.
Example four: modification of Polyimide (PI) powder
Raw materials: polyimide powder brand: dupont brand TP 2875.
1)100g of raw materials are placed in a tray, flatly laid in a static reactor and 20L of reactor volume;
2) the reactor was heated to 400 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium gas into the reactor to normal pressure;
5) repeating the step 3 and the step 4 in sequence twice; the reactor is continuously heated in the process, the heating target temperature is kept at 400 ℃, the temperature of the reactor is kept, and a temperature environment is provided for the next reaction;
6) evacuating the reactor to-0.09 MPa;
7) filling reaction gas sulfur hexafluoride (purity is more than 99.99%) and methanol steam (purity is more than 99.99%) to a reactor pressure of 0.1MAP, wherein the molar mass ratio of the filled sulfur hexafluoride to the methanol is 10: 1;
8) discharging the radio frequency power supply electrode in the reactor with the discharge power of 2W/cm3Lasting for 5 hours;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9-10 once;
12) opening the reactor and taking out the materials;
13) the wettability test was carried out with a dyne solution, at which time the polyimide powder was wettable with a dyne solution numbered 52, indicating that the surface energy of the powder was >52 mN/m.
Example five: modification of Aramid (Aramid) micropowder
Raw materials: aramid brand: dupont Kevlar number 8F 1857.
1)100g of raw materials are placed in a tray, flatly laid in a static reactor and 20L of reactor volume;
2) the reactor was heated to 300 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium into the reactor to normal pressure;
5) repeating the step 3 and the step 4 twice;
6) evacuating the reactor to-0.09 MPa;
7) carbon tetrafluoride (CF) charged to the reactor4) (purity of>99.99%), and ethanol vapor (C)2H5OH) (purity)>99.99%) to 0.1MAP, and the molar mass ratio of the charged carbon tetrafluoride to the charged ethanol is 10: 1;
8) discharging the radio frequency power supply electrode in the reactor, wherein the discharge power is 2W/m3, and the duration is 3 hours;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9-10 once;
12) opening the reactor and taking out the materials;
13) and (3) performing a wettability test by using the dyne liquid, wherein the aramid powder can be wetted by the dyne liquid with the reference number of 52, and the surface energy of the powder is more than 52 mN/m.
Example six: modification of polypropylene (PP) micropowder
1)100g of raw materials are placed in a tray, flatly laid in a static reactor and 20L of reactor volume;
2) the reactor was heated to 100 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium gas into the reactor to normal pressure;
5) repeating the step 3 and the step 4 twice;
6) evacuating the reactor to-0.09 MPa;
7) charging nitrogen trifluoride (NF) into the reactor3) (purity of>99.99%) gas and ammonia (NH)3) (purity of>99.99%) to normal pressure, and the molar mass ratio of the charged nitrogen trifluoride and ammonia gas is 10: 1;
8) the radio frequency power supply electrode discharges in the reactor with the discharge power of 2W/m3For a duration of 40 minutes;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9-10 once;
12) opening the reactor and taking out the materials;
13) the wettability test was carried out with a dyne liquid, at which time the polypropylene powder was wetted with a dyne liquid numbered 46, indicating that the surface energy of the powder was >46 mN/m.
Example seven: modification of Low Density Polyethylene (LDPE) micropowder
Raw materials: low density polyethylene micropowder brand: the Dow brand 330E has an average particle size of 20 microns and a melting point of 120 ℃.
1)100g of raw materials are placed in a tray, flatly laid in a static reactor and 20L of reactor volume;
2) the reactor was heated to 100 ℃;
3) evacuating the reactor to-0.09 MPa;
4) filling helium gas into the reactor to normal pressure;
5) repeating the step 3 and the step 4 twice;
6) evacuating the reactor to-0.09 MPa;
7) carbon tetrachloride CCl charged into the reactor4(purity of>99.99%) and methanol vapor (CH)3OH) to normal pressure, wherein the molar mass ratio of the charged carbon tetrachloride to the methanol is 10: 1;
8) the radio frequency power supply electrode discharges in the reactor with the discharge power of 2W/m3For a duration of 30 minutes;
9) evacuating the reactor to-0.09 MPA;
10) filling nitrogen to normal pressure;
11) repeating the step 9-10 once;
12) opening the reactor and taking out the materials;
13) the wettability test is carried out by the dyne liquid, and the low-density polyethylene micropowder can be wetted by the dyne liquid with the number of 46 at the moment, which shows that the surface energy of the micropowder is more than 46 mN/m.
After the reaction, the powder was taken out from the reactor in each of the above examples, and the surface of the powder had a certain polarity and good dispersibility, and had good processability as an additive for a polar material.
The modification effect is tested by measuring the wettability of the powder, the wettability of the powder is measured by adopting a dyne drop test method, a dyne liquid can be used for reacting the surface tension of the material to water, and in the printing industry, the surface of the material can be often tested by using a dyne liquid or a dyne pen to determine whether the surface of the material can be firmly printed;
as shown in fig. 1, at a certain temperature, a dyne liquid with a determined value, for example, 46 dynes is dripped into a polyethylene powder modified by the above process, the dyne liquid can infiltrate the powder (see fig. 1 right), while a polyethylene powder dyne liquid which is not modified by the process polymerizes into a sphere on the powder (see fig. 1 left), the powder cannot infiltrate, and comparing the graph before and after the powder infiltration with the graph shown in fig. 1, the surface tension of the modified polyethylene powder to water is greater than 46mN/m, while the surface tension of the unmodified polyethylene powder to water is less than 46mN/m, the surface tension of common polyethylene to water is 31NmN/m, the infiltration performance of the powder is improved, and the polarity of the material is improved greatly according to the principle of similar compatibility;
fig. 2 is a scanning electron microscope image of the polymer powder before and after modification by the above method, the left side is the microstructure of the modified polymer powder, the right side of fig. 2 is before modification, the left side of fig. 2 is after modification, and the structure diagram is from top to bottom under different magnifications.
Table 1 shows the surface tension achievable for a portion of the powder material after treatment by the process:
no professional data was found, and this unit tested the actual data with dyne fluid.
TABLE 1
If the polarity of the polymer powder is less than that of the dyne liquid, the liquid drop floats on the surface of the polymer powder and cannot be soaked (as shown in the left part of figure 2), and if the polarity of the polymer powder is more than that of the dyne liquid, the liquid drop is soaked into the polymer powder (as shown in the right part of figure 2).
In summary, the polymer powder prepared by the method of the present invention has a polar surface, a porous structure on the microscopic surface and reactive active functional groups grafted thereon, and the effect of the present invention is permanent modification, and the modification effect is not lost due to high temperature, use environment and storage conditions. The material prepared by the method can be used as an additive to be added into a polar material to form good interface connection with a base material, and can be used as a framework reinforcing material to improve specific or comprehensive properties of the material, such as wear resistance, tensile property, tearing resistance, corrosion resistance and the like.
Claims (6)
1. A method for preparing polar polymer powder by low-temperature plasma is characterized by comprising the following steps:
step (1), adding the nonpolar polymer powder into a vacuum reactor for heating, and heating to 80-400 ℃;
step (2), after heating, vacuumizing the vacuum reactor to less than or equal to-0.09 MPa;
step (3), after vacuumizing, filling reaction gas into the reactor to-0.08 MPa to 0.1MPa, wherein the reaction gas is OH generated under electric shock-、NH2 -、CL-Or F-One or more plasma gases;
step (4), after reaction gas is filled, discharging the reactor by using a radio frequency discharge electrode, wherein the discharge voltage is 20-200 kilovolts, and dischargingThe power is 2-5W/m3The duration is 10min-5 h;
step (5), after the discharge is finished, vacuumizing the reactor to be less than or equal to-0.09 MPa, and filling inert gas to be normal pressure after vacuumizing;
wherein the nonpolar polymer powder in the step (1) is polypropylene (PP) powder, Polyethylene (PE) powder, High Density Polyethylene (HDPE) powder, ultra-high molecular weight polyethylene (UHMPWE) powder, Low Density Polyethylene (LDPE) powder, aramid powder or polyimide powder;
wherein, the heating temperature in the step (1) is higher than the boiling point of the reaction gas filled in the step (3) and lower than the melting point of the added non-polar polymer powder;
the reaction gas in the step (3) is a mixed gas, the mixed gas is a mixed gas of a first gas and a second gas, the first gas is one of carbon tetrachloride, methane chloride, carbon tetrafluoride, sulfur hexafluoride or nitrogen trifluoride, and the second gas is ammonia gas or alcohol steam; the volume ratio of the first type gas to the second type gas is not less than 10: 1.
2. the method for preparing polar polymer powder by using low-temperature plasma as claimed in claim 1, wherein the vacuum reactor in step (1) is a static reactor, and the thickness of the nonpolar polymer powder added into the reactor is not more than 3 mm.
3. The method for preparing polar polymer powder by using low-temperature plasma as claimed in claim 1, wherein the vacuum reactor in step (1) is a rotary kiln reactor.
4. The method of claim 3, wherein the reactor is rotated in step (4).
5. A method for preparing polar polymer powder according to any one of claims 1-4, characterized in that, the heating temperature in step (1) is pressurized by filling inert gas to one atmosphere, then the pressure in step (2) is vacuumized, and the pressurizing and vacuuming are repeated for 2-3 times, and then step (3) is proceeded.
6. The method of claim 5, wherein step (5) is repeated 1-3 times.
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| CN111808419B (en) * | 2020-07-10 | 2023-06-20 | 江苏集萃先进高分子材料研究所有限公司 | Wear-resistant plastic with high friction coefficient and preparation method thereof |
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