CN108456317A - A kind of method that low temperature plasma prepares polar polymeric powder - Google Patents
A kind of method that low temperature plasma prepares polar polymeric powder Download PDFInfo
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- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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Abstract
The present invention provides a kind of methods that low temperature plasma prepares polar polymeric powder, and apolar polymeric powder is placed in reactor, the OH that can shock by electricity out is filled in reactor‑、NH2 ‑、CL‑Or F‑In one or more plasmas gas, apolar polymeric powder and the plasma reaction to shock by electricity out make polymer powder surface have polar group that is stronger and stablizing, is more conducive to polymer powder and is added in matrix be modified.Surface prepared by method using the present invention carries polar polymer powder, and microcosmic surface is porous structure and grafting reactivity active function groups, effect of the invention be it is permanent modified, will not because of high temperature, use environment, condition of storage and lose modified effect.Material prepared by the present invention can be used as additive and be added in polar material, and forming good interface with base material connect, as skeleton reinforcing material, promoted material it is wear-resisting, stretch, tear the specific or comprehensive performance such as anticorrosive.
Description
Technical field
The invention belongs to polymeric additive preparing technical fields, and in particular to a kind of low temperature plasma preparation polarity is poly-
The method for closing powder.
Background technology
Some polymer materials, such as ultra-high molecular weight polyethylene, high density polyethylene (HDPE), polypropylene, polyester, polychlorostyrene second
Alkene, nylon etc. have preferable physics and chemical property, such as compared with low-friction coefficient, high molecular weight, wear-resisting, resistance to chemical attack,
Ageing-resistant performance, powder as other materials (such as rubber, coating etc.) additive theoretically can reinforcing material correlation
Performance (such as 10%-20% additives are added, rubber material wearability 50%, corrosion resistance 30%, tear resistance can be improved
30%, prolong the service life 300%), but these polymer powders are non-polar materials, is not easy to disperse in polar substrates, with
The interface performance of base material is poor, easy to fall off even if the interface performance being added in base material with base material is poor, can not play predictive role,
The physical and mechanical property of other materials may be more destroyed instead.And some polymer architectures are particularly stable, graft modification
It is relatively difficult.It is very limited so being applied to be modified in other materials by these polymer materials in the prior art.
Currently used additive surface modification mode includes following several：Silane-modified, modified by maleic acid anhydride graft is total to
Gather the modes such as modified in the cladding of additive surface with polar functional group.But above several modified effects are unstable, in height
It under warm environment or when condition of storage is bad, is easily broken off with polar functional group in cladding, modified failure.
In view of the deficienciess of the prior art, proposing the present invention.
Invention content
The object of the present invention is to provide a kind of method that low temperature plasma prepares polar polymeric powder, the present invention passes through
It chooses several specific plasmas to be modified related polymer, achieves good effect.With conventional crosslinking technology phase
Than the graft effect that the method obtains is good, and wetting property raising degree is big, and effect is lasting.
For achieving the above object, the technical scheme is that：A kind of low temperature plasma prepares polar polymer
The method of powder, includes the following steps：
Apolar polymeric powder is added in vacuum reactor and heats, is heated to 80-400 DEG C by step (1)；
Step (2) ,≤- 0.09MPA is evacuated to after heating to vacuum reactor；
Step (3) is filled with reaction gas to -0.08MPA to 0.1MAP, the reaction gas after vacuumizing into reactor
Body, which is that electric shock is lower, generates OH-、NH2 -、CL-Or F-In one or more plasmas gas.
Step (4) after being filled with reaction gas, generates electricity to reactor with radio flow discharge electrode, discharge voltage 20-
200
Kilovolt, discharge power is 2~5W/m3, the duration is 10 minutes to 5 hours；
Step (5) after the completion of electric discharge, carries out reactor to be evacuated to≤- 0.09MPA, indifferent gas is filled with after vacuumizing
Body is to normal pressure.
Further, the reaction gas in step (3) is mixed gas, which is first kind gas and the second class
The mixed gas of gas, the first kind gas are carbon tetrachloride, monochloro methane, carbon tetrafluoride, sulfur hexafluoride or Nitrogen trifluoride
In one kind, the second class gas be ammonia or alcohol vapor, can be methanol, ethyl alcohol or other alcohols gases one kind
Or it is several.
Further, the first kind gas in step (3) and the second class gas volume ratio are less than 10：1.
Further, vacuum reactor is batch reactor, the non-polar polymer powder being added in reactor in step (1)
Body thickness is no more than 3mm.
Further, vacuum reactor is rotary kiln reactor in step (1).
Further, reactor rotates in step (4).
Further, punching press is filled with inert gas to an atmospheric pressure under step (1) heating temperature, then is evacuated to step
Suddenly the pressure in (2), be repeated in punching press, vacuumize 2-3 times after enter back into step (3).
Further, step (5) repeats 1-3 times.
Further, the apolar polymeric powder in step (1) be polypropylene (PP) powder, it is polyethylene (PE) powder, highly dense
Spend polyethylene (HDPE) powder, ultra-high molecular weight polyethylene (UHMPWE) powder, low density polyethylene (LDPE) (LDPE) powder, aramid fiber powder or poly-
The average grain diameter of acid imide powder, the apolar polymeric powder of selection is less than 150 μm.
Further, the heating temperature in step (1) is less than and adds higher than the boiling point for the reaction gas being filled in step (3)
The melting point of the apolar polymeric powder entered.
The beneficial effects of the invention are as follows：
Surface prepared by method using the present invention carries polar polymer powder, and microcosmic surface is porous structure and connects
The reactive active function groups of branch, effect of the invention be it is permanent modified, will not because of high temperature, use environment, condition of storage and lose
Lose modified effect.Material prepared by the method for the present invention can be used as additive and be added in polar material, be formed well with base material
Interface connection, as skeleton reinforcing material, promoted material it is wear-resisting, stretch, tear the specific or comprehensive performance such as anticorrosive.
Description of the drawings
Fig. 1 is that a kind of method processing polymer powder preparing polar polymeric powder using low temperature plasma is forward and backward
Effect of impregnation comparison diagram；
Fig. 2 is that a kind of method processing polymer powder preparing polar polymeric powder using low temperature plasma is forward and backward
Scanning electron microscope micro-structure diagram；
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention.
A kind of method that low temperature plasma prepares polar polymeric powder, includes the following steps：
Apolar polymeric powder is added in vacuum reactor and heats by step (1), heating temperature 80-400
℃；Specific reaction temperature is determined according to the reaction gas being next added, and the boiling point such as carbon tetrachloride of certain reaction gas connects
Nearly 80 DEG C, 80 DEG C or more can guarantee that reactive material is vaporized state, and the activity of plasma at a higher temperature is higher, can
React fully progress, but reaction temperature will be less than the melting point of powder, such as the melting point of PP is about 165 DEG C, and HDPE melting points are about
140 DEG C, polyimides melting point is up to 400 DEG C or more ...；
Step (2) ,≤- 0.09MPA is evacuated to after heating to vacuum reactor；This step can both extract vacuum reaction out
Residual gas in device, or reactor provides vacuum state；
Step (3) is filled with reaction gas to -0.08MPA to 0.1MPA after vacuumizing into reactor, and reaction gas is electricity
Hit lower generation OH-, NH2, CL- or one or more plasmas in F- gas.The anti-of above-mentioned plasma can be generated
It is one kind or alcohols gas in carbon tetrachloride, monochloro methane, carbon tetrafluoride, sulfur hexafluoride or Nitrogen trifluoride, ammonia to answer gas
Gas；It is furthermore preferred that the reaction gas in step (3) is mixed gas, which is first kind gas and the second class gas
Mixed gas, the first kind gas be carbon tetrachloride, monochloro methane, carbon tetrafluoride, sulfur hexafluoride or Nitrogen trifluoride in
One kind, the second class gas be alcohols gas or ammonia, you can with for methanol, ethyl alcohol or other alcohols gases one kind or
It is several；It is general to be filled with gas to normal pressure to be exactly reactor inside and outside differential pressure 0MPA or so be charged to if reactor allowable stress
0.1MPA, to guarantee to generate the plasma active of higher concentration；
It carries out needing to carry out reactor when step (2) and step (3) to continue heated at constant temperature, for reaction gas is next added
Body provides reaction temperature condition.
Step (4) after being filled with reaction gas, discharges to reactor with radio flow discharge electrode, discharge voltage 20-
200 kilovolts, discharge power is 2~5W/m3, the duration is 10 minutes to 5 hours；Reaction gas is under electric shock in this step
Plasma is generated, plasma reacts under the temperature and pressure that reactor is kept needed for generation with apolar polymeric powder
Product；
Principle：It shocks by electricity and ionizes out containing including OH in post-reactor-、NH2 -、CL-Or F-In one or more plasmas
Body (type of visual response gas)；These plasmas have strongly active and electronegativity, especially OH-Or NH2 -It can promote to polymerize
Some c h bonds fracture of object surface, C-OH, C-NH with reactivity are formed after fracture with plasma2, CL-Or F-It can be
Polymer surfaces generate C-Cl, and there is C-F etc. the key compared with strong bond energy, these newly-generated keys to have more highly polar, so that it may with
Make polymer surfaces polarity.
Meanwhile plasma also has corrasion to powder surface, increases the specific surface area of powder, it (can be from micro-
See and observe and obtain in structure, electromicroscopic photograph Fig. 2 is provided), can further improve in this way powder in future in addition with the leaching of base material
Lubricant nature energy；
Step (5) after the completion of electric discharge, carries out reactor to be evacuated to≤- 0.09MPA, indifferent gas is filled with after vacuumizing
Body is to normal pressure.The step is to remove the remaining gaseous impurity of reaction, and pollution environment is overflowed in reaction when opening reactor.
More preferably, the reaction gas in step (3) is mixed gas, which is first kind gas and the second class gas
The mixed gas of body, the first kind gas are in carbon tetrachloride, monochloro methane, carbon tetrafluoride, sulfur hexafluoride or Nitrogen trifluoride
One kind, the second class gas is one kind or several that alcohol vapor can be methanol, ethyl alcohol or other alcohols gases or ammonia
Kind.First kind gas can generate CL in ionization-Or F-Plasma, the second class gas can generate OH in ionization-Or NH2 -Deng
Gas ions.
More preferably, the first kind gas in step (3) and the second class gas volume ratio are not less than 10：1.Ensure CL-Or F-Deng
Gas ions and OH-Or NH2 -The concentration ratio of plasma always, while ensureing the OH for being grafted on powder surface-Or NH2 -Plasma
It will not be excessive.If OH-Or NH2 -Plasma density is excessive, it will the reactivity for influencing modified powder, to influence product
It is further to use.
In the above-mentioned technical solutions, vacuum reactor can select batch reactor in step (1), in order to increase polymer
The contact area of powder and reaction gas, the polymer powder body thickness being added in reactor are no more than 3mm.
Or vacuum reactor selects rotary kiln reactor in step (1).The advantages of rotary kiln reactor is can to allow powder
Overturning is suitble to industrialized production with to fully be reacted with gas ions in the reactor；
If selecting rotary kiln reactor, rotary kiln reactor rotates in step (4).
More preferably, punching press is filled with inert gas to an atmospheric pressure under the step (1) heating temperature, then vacuumizes
Pressure into step (2), be repeated in punching press, vacuumize 2-3 times after enter back into step (3).I.e. in punching press and when vacuumizing
The heated condition in step (1) is kept, controls reactor steady temperature as possible.Multi-step forming and the operation vacuumized in the program
The residual gas impurity in reactor can more fully be removed.
More preferably, step (5) repeats 1-3 times.Multiplicating step (5) can preferably remove remaining in reactor
Reaction gas.
In the above technical solution, the apolar polymeric powder in step (1) can select PP powder, PE powder, HDPE
The average grain diameter of powder, UHMPWE powder, LDPE powder, aramid fiber powder or polyimides powder, optional negated polar polymeric powder is small
In 150 μm.If diameter of particle is more than 150 μm, as additive, it will generate the influence of appearance or performance to downstream product.
In the above technical solution, the heating temperature wherein in step (1) is higher than the reaction gas being filled in step (3)
Boiling point, that is, be higher than the boiling temperature of mixed gas mid-boiling point highest gas, less than the apolar polymeric powder being added
Melting point.
Embodiment one：The modification of ultra-high molecular weight polyethylene (UHMWPE) powder
Raw material：Ultra-high molecular weight polyethylene powder brand：Mitsui Chemicals trade mark 240S 120 μm of molecular weight 200 of average grain diameter
Ten thousand.
1) it is 20L that 100g raw material, which are positioned over tiling in pallet and are placed in reactor volume in batch reactor,；
2) reactor is heated to 100 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) it is filled in reactor such as helium to normal pressure；
5) step 3) and step 4) are repeated in twice；The process keeps heating target temperature to reactor continuous heating
It is 100 DEG C；The temperature for keeping reactor provides temperature environment for next reaction；
6) reactor is carried out being evacuated to -0.09MPa；
7) Nitrogen trifluoride (NF is filled with into reactor3) (purity>99.99%) gas and ammonia (NH3) (purity>
99.99%) mixed gas NF here3：NH3Mixed gas volume ratio be 10:1, until normal pressure；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/m3, 20 minutes duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) step 9 and step 10 are repeated in twice；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, ultra-high molecular weight polyethylene powder can be numbered 52 dyne at this time
Liquid infiltrates, and illustrates the surface energy of powder>52mN/m.
Embodiment two：The modification of high density polyethylene (HDPE) (HDPE) powder
Raw material：High density polyethylene (HDPE) powder brand：Mitsui Chemicals trade mark 1105A density 0.99g/cc fusing points
137℃。
1) 100g raw material are positioned over tiling in pallet and are placed in rotary kiln reactor, reactor volume 20L；
2) reactor is heated to 100 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) it is filled in reactor such as helium to normal pressure；
5) it is repeated in step 3) and step 4) is primary；The process keeps heating target temperature to reactor continuous heating
It is 100 DEG C, keeps the temperature of reactor, temperature environment is provided for next reaction；
6) reactor is carried out being evacuated to -0.09MPa；
7) it is filled with reactor monochloro methane (CH3CL) (purity>And methanol steam (CH 99.99%)3OH) (purity>
99.99%) to normal pressure, the molal weight ratio of the monochloro methane and methanol that are filled with is 10:1；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/cm3,10 minutes duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) it is repeated in step 9 and step 10 is primary；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, high density polyethylene (HDPE) micro mist can be numbered 52 dyne liquid leaching at this time
Profit, illustrates the surface energy of powder>52mN/m.
Embodiment three：The modification of polyethylene (PE) wax powder
Raw material：Polyethylene wax powder brand：Its poem trade mark PEW-0202 16 μm of average grain diameter, 110 DEG C of fusing points.
1) it is 20L that 100g raw material, which are positioned over tiling in pallet and are placed in reactor volume in batch reactor,；
2) reactor is heated to 80 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) helium is filled in reactor to normal pressure；
5) step 3 and step 4 are repeated in twice；The process keeps the heating target temperature to be reactor continuous heating
80 DEG C, the temperature of reactor is kept, temperature environment is provided for next reaction；
6) reactor is carried out being evacuated to -0.09MPa；
7) it is filled with reactor Nitrogen trifluoride (NF3) (purity>And ammonia (NH 99.99%)3) (purity>99.99%) mixed
Gas is closed to normal pressure, the molal weight ratio of the Nitrogen trifluoride and ammonia that are filled with is 10:1；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/m3, 40 minutes duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) it is primary to repeat step 9-10；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, polyethylene powder can be numbered 52 dyne liquid infiltration, explanation at this time
The surface energy of powder>46mN/m.
Example IV：The modification of polyimides (PI) powder
Raw material：Polyimide powder brand：Du Pont trade mark TP2875.
1) it is 20L that 100g raw material, which are positioned over tiling in pallet and are placed in reactor volume in batch reactor,；
2) reactor is heated to 400 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) helium is filled in reactor to normal pressure；
5) step 3 and step 4 are repeated in twice；The process keeps the heating target temperature to be reactor continuous heating
400 DEG C, the temperature of reactor is kept, temperature environment is provided for next reaction；
6) reactor is carried out being evacuated to -0.09MPa；
7) it is filled with reaction gas sulfur hexafluoride (purity>And methanol steam (purity 99.99%)>99.99%) to reactor pressure
Power is 0.1MAP, and the molal weight ratio of the sulfur hexafluoride and methanol that are filled with is 10:1；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/cm3, 5 hours duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) it is primary to repeat step 9-10；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, polyimides powder can be numbered 52 dyne liquid infiltration at this time, say
The surface energy of bright powder>52mN/m.
Embodiment five：The modification of aramid fiber (Aramid) micro mist
Raw material：Aramid fiber brand：Du Pont's Kev draws trade mark 8F1857.
1) it is 20L that 100g raw material, which are positioned over tiling in pallet and are placed in reactor volume in batch reactor,；
2) reactor is heated to 300 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) it is filled in reactor such as helium to normal pressure；
5) step 3 and step 4 are repeated twice；
6) reactor is carried out being evacuated to -0.09MPa；
7) it is filled with reactor carbon tetrafluoride (CF4) (purity>And alcohol vapour (C 99.99%)2H5OH) (purity>
99.99%) for pressure to 0.1MAP, the molal weight ratio of the carbon tetrafluoride and ethyl alcohol that are filled with is 10:1；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/m3,3 hours duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) it is primary to repeat step 9-10；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, aramid fiber powder can be numbered 52 dyne liquid infiltration at this time, illustrate powder
The surface energy of body>52mN/m.
Embodiment six：The modification of polypropylene (PP) micro mist
1) it is 20L that 100g raw material, which are positioned over tiling in pallet and are placed in reactor volume in batch reactor,；
2) reactor is heated to 100 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) helium is filled in reactor to normal pressure；
5) step 3 and step 4 are repeated twice；
6) reactor is carried out being evacuated to -0.09MPa；
7) Nitrogen trifluoride (NF is filled with into reactor3) (purity>99.99%) gas and ammonia (NH3) (purity>
99.99%) to normal pressure, the molal weight ratio of the Nitrogen trifluoride and ammonia that are filled with is 10:1；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/m3, 40 minutes duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) it is primary to repeat step 9-10；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, polypropylene powder can be numbered 46 dyne liquid infiltration, explanation at this time
The surface energy of powder>46mN/m.
Embodiment seven：The modification of low density polyethylene (LDPE) (LDPE) micro mist
Raw material：Low density polyethylene (LDPE) micro mist brand：Tao Shi trade mark 330E 20 microns of average grain diameter, 120 DEG C of fusing points.
1) it is 20L that 100g raw material, which are positioned over tiling in pallet and are placed in reactor volume in batch reactor,；
2) reactor is heated to 100 DEG C；
3) reactor is evacuated, until -0.09MPa；
4) helium is filled in reactor to normal pressure；
5) step 3 and step 4 are repeated twice；
6) reactor is carried out being evacuated to -0.09MPa；
7) it is filled with reactor carbon tetrachloride CCl4(purity>And methanol steam (CH 99.99%)3OH) to normal pressure, be filled with four
The molal weight of chlorination carbon and methanol ratio is 10:1；
8) radio-frequency power supply electrode discharges in the reactor, discharge power 2W/m3, 30 minutes duration；
9) reactor is carried out being evacuated to -0.09MPA；
10) nitrogen is filled with to normal pressure；
11) it is primary to repeat step 9-10；
12) reactor is opened, material is taken out；
13) wellability test is carried out with dyne liquid, low density polyethylene (LDPE) micro mist powder can be numbered 46 dyne at this time
Liquid infiltrates, and illustrates the surface energy of powder>46mN/m.
Powder after taking out reaction in the reactor in above-mentioned each embodiment, powder surface at this time are provided with centainly
Polarity and favorable dispersibility, as polar material additive have preferable processability.
We examine modified effect by measuring the wellability of powder herein, are surveyed using dyne drop test method
The wellability of powder is measured, dyne liquid can be used for surface tension of the reaction material to water, in printing industry, through commonly using dyne liquid
Or whether a dyne test material surface can firmly be printed；
As one is had at a certain temperature and determine that a dyne drop for such as 46 dynes of numerical value enters by the above work by Fig. 1
In the polyethylene powder that skill is modified, dyne liquid can infiltrate powder (see the right sides Fig. 1), and the not polyethylene Jing Guo this process modification
Powder dyne liquid is then conglobulated on powder (see the left sides Fig. 1), can not infiltrate powder, and the front and back comparison diagram of powder infiltration is shown in Fig. 1, then
Illustrate surface tension of the modified polyethylene powder to water>46mN/m, and not surface of the modified polyethylene powder to water
Tension<46mN/m learns that common polythene is 31N mN/m, the wetting property of powder to the surface tension of water by inspection information
It improves, according to similar compatibility principle, the polarity raising degree of material is larger；
Fig. 2 be using the above method before modified after polymer powder scanning electron microscope (SEM) photograph, the left side is that we are modified
Scanning electron microscope microstructure, the right Fig. 2 is that before modified, the left sides Fig. 2 are modified, is under different amplification from top to bottom
Structure chart, as can be seen from Figure modified product become porous structure from microcosmic, the base material with particle contact can
With penetrating particle, so after particle is added to other base materials, the associativity dispersibility of system can all reach better state.
Table 1 is the accessible surface tension of part powder body material after this process：
* expert data is not found, and our unit tests real income data with dyne liquid.
Table 1
It is less than dyne liquid polarity in polymer powder, such as polymer powder polarity with dyne drop of opposed polarity, then droplets float
(left side in such as Fig. 2) cannot be infiltrated on polymer powder surface, if polymer powder polarity is more than dyne liquid polarity, then drop is infiltrated to poly-
It closes in object powder (right in such as Fig. 2).
In conclusion surface prepared by method using the present invention carries polar polymer powder, microcosmic surface is porous
Structure and grafting reactivity active function groups, effect of the invention are permanently to be modified, will not be because of high temperature, use environment, storage
It deposits condition and loses modified effect.Material prepared by the method for the present invention can be used as additive and be added in polar material, with base
Material forms the connection of good interface, as skeleton reinforcing material, promoted material it is wear-resisting, stretch, tear it is anticorrosive etc. specific or
Comprehensive performance.
Claims (10)
1. a kind of method that low temperature plasma prepares polar polymeric powder, which is characterized in that include the following steps：
Apolar polymeric powder is added in vacuum reactor and heats, is heated to 80-400 DEG C by step (1)；Step
(2) ,≤- 0.09MPA is evacuated to vacuum reactor after heating；
Step (3) is filled with reaction gas to -0.08MPA to 0.1MAP after vacuumizing into reactor, and the reaction gas is electricity
Hit lower generation OH-、NH2 -、CL-Or F-In one or more plasmas gas；
Step (4) after being filled with reaction gas, generates electricity to reactor with radio flow discharge electrode, and discharge voltage is 20-200 thousand
Volt, discharge power are 2~5W/m3, the duration is 10 minutes to 5 hours；
Step (5) after the completion of electric discharge, carries out reactor to be evacuated to≤- 0.09MPA, inert gas is filled with after vacuumizing extremely
Normal pressure.
2. the method that a kind of low temperature plasma according to claim 1 prepares polar polymeric powder, which is characterized in that
Reaction gas in the step (3) is mixed gas, which is the gaseous mixture of first kind gas and the second class gas
Body, the first kind gas is one kind in carbon tetrachloride, monochloro methane, carbon tetrafluoride, sulfur hexafluoride or Nitrogen trifluoride, described
Second class gas is ammonia or alcohol vapor.
3. the method that a kind of low temperature plasma according to claim 2 prepares polar polymeric powder, which is characterized in that
First kind gas and the second class gas volume ratio in the step (3) are less than or equal to 10：1.
4. the method that a kind of low temperature plasma according to claim 1 prepares polar polymeric powder, which is characterized in that
Vacuum reactor is batch reactor in the step (1), and the non-polar polymer powder thickness being added in reactor is no more than
3mm。
5. the method that a kind of low temperature plasma according to claim 1 prepares polar polymeric powder, which is characterized in that
Vacuum reactor is rotary kiln reactor in the step (1).
6. the method that a kind of low temperature plasma according to claim 5 prepares polar polymeric powder, which is characterized in that
Reactor rotates in the step (4).
7. according to the method that a kind of low temperature plasma of claim 1-6 any one of them prepares polar polymeric powder,
It is characterized in that, punching press is filled with inert gas to an atmospheric pressure under the step (1) heating temperature, then is evacuated to step
(2) pressure in, be repeated in punching press, vacuumize 2-3 times after enter back into step (3).
8. the method that a kind of low temperature plasma according to claim 7 prepares polar polymeric powder, which is characterized in that
The step (5) repeats 1-3 times.
9. according to the method that a kind of low temperature plasma of claim 1-6 any one of them prepares polar polymeric powder,
It is characterized in that, the apolar polymeric powder in the step (1) is polypropylene (PP) powder, polyethylene (PE) powder, high density are poly-
Ethylene (HDPE) powder, ultra-high molecular weight polyethylene (UHMPWE) powder, low density polyethylene (LDPE) (LDPE) powder, aramid fiber powder or polyamides are sub-
Amine powder.
10. the method that a kind of low temperature plasma according to claim 9 prepares polar polymeric powder, feature exist
In the heating temperature in the step (1) is less than the nonpolarity being added higher than the boiling point for the reaction gas being filled in step (3)
The melting point of polymer powder.
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