CN108384187A - A kind of preparation method of reinforced polyether ether ketone resin new material - Google Patents
A kind of preparation method of reinforced polyether ether ketone resin new material Download PDFInfo
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- CN108384187A CN108384187A CN201810334757.2A CN201810334757A CN108384187A CN 108384187 A CN108384187 A CN 108384187A CN 201810334757 A CN201810334757 A CN 201810334757A CN 108384187 A CN108384187 A CN 108384187A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
Present invention relates particularly to a kind of preparation method of reinforced polyether ether ketone resin new material, method includes：The tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law chloride, polyoxy isobutylene/methylene urea copolymer of 0.01 0.05 parts by weight, 15 parts by weight of 35 60 parts by weight of copolymer of 90 120 parts by weight of polyether-ether-ketone resin, caprolactone and dimethyl siloxane, 25 35 parts by weight of polyamic acid, 20 25 parts by weight of maleic anhydride, 10 15 parts by weight of dioctyl phthalate and 0.01 0.05 parts by weight are added in mixing device to the mixing for carrying out material, the heating of mixed material is melted, by the molding materials curing molding to get to the new material.
Description
Technical field
The invention belongs to polyether-ether-ketone preparing technical fields；More particularly to a kind of system of reinforced polyether ether ketone resin new material
Preparation Method.
Background technology
Polyether-ether-ketone resin (PEEK) is a kind of special engineering plastics haveing excellent performance, and is had compared with Other Engineering plastics
Many advantages, such as high temperature resistant, mechanical performance is excellent, self-lubricating property is good, chemicals-resistant burn into is fire-retardant, peel resistance, radiation resistance
Property, insulating properties stablize, hydrolysis and easy processing etc..
CN105482050B discloses a kind of preparation method of polyether-ether-ketone resin, including polymerisation and reaction product
Precipitating and purification process, precipitating processing are：Reaction temperature is first down to 210-230 DEG C after polymerisation, accelerating stirring makes
Polyether-ether-ketone resin system is uniformly precipitated, and trimethylbenzene is added after reactor temperature stabilization, stirring to reaction system it is uniform after
Reaction temperature is down to 90-110 DEG C again, makes polyether-ether-ketone resin all homogeneously crystallized precipitations；The white that precipitating is handled
Slurry recycles dehydrating agent, diphenyl sulphone (DPS) successively, then can be obtained polyether-ether-ketone resin by washing, drying.The method overcome existing
There is product in polyether-ether-ketone resin production process to need the discontinuous problem of technological process caused by crushing, also overcomes simultaneously
The inorganic salt particle that product particle wraps up in traditional handicraft cleans the problem for not causing totally macromolecule product purity not high.
CN103709406B discloses a kind of method preparing light color polyethersulfone/polresinr-ether-ketone resinr-ether-ketone, including step：It will contain
There is polyether sulfone/polyether-ether-ketone resin crushed after being dried of impurity at toner；Toner is placed in fat extractor, then
Extractant is added, the temperature in container is adjusted to 100-250 DEG C, pressure controls within the scope of 0.1-1MPa, is heated to boiling,
Pressure release filters out extractant and puts into distiller after keeping at least 30min, and heating makes extractant boil, and to be extracted dose of steam is cold
It is solidifying flow back into fat extractor and reach to pressurize after certain liquid level extract again, so repeat extracting 24-48 hour, taking-up sample
After product drying to obtain the final product.This method is notable to the purification effect of polyether sulfone/polyether-ether-ketone resin, reduce residual solvents and toluene or
Xylene content can be obviously improved color of resin, improve product quality.
CN103467681B discloses a kind of synthetic method of high thermal stability polyether-ether-ketone resin, using 4,4- difluoros two
Benzophenone and hydroquinone carry out nucleophilic condensation polymerization as polymerization chain reactant, and salt forming agent is sodium bicarbonate in this method,
Using 4,4- dihydroxy benaophenonels as molecular weight regulator, end-capping reagent is 4- fluorine biphenyl.The present invention selects sodium bicarbonate to make
So that the pH value of reaction system is reduced for salt forming agent, is conducive to inhibit hydroquinone oxidation.
The method that the above patent of invention provides, the intensity of material is poor, limits the application range of material.
Invention content
Insufficient present in background technology in order to overcome, the present invention provides a kind of system of reinforced polyether ether ketone resin new material
Preparation Method
Technical solution used in the present invention is：
A kind of preparation method of reinforced polyether ether ketone resin new material, the preparation method include the following steps：
（1）By the copolymer of polyether-ether-ketone resin 90-120 parts by weight, caprolactone and dimethyl siloxane that the degree of polymerization is 60-80
35-60 parts by weight, polyamic acid 25-35 parts by weight, maleic anhydride 20-25 parts by weight, dioctyl phthalate 10-15 weight
Part and the tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law chlorides of 0.01-0.05 parts by weight, 0.01-0.05 parts by weight it is poly-
The mixing for carrying out material is added in mixing device in oxygen isobutylene/methylene urea copolymer, 1-5 parts by weight, by mixed object
Material is placed in 160-170 DEG C of temperature environment to heat and be melted, and is stirred during heating to mixed material；
（2）After stirring 0.5-1 hours, enhancing component 67-110 parts by weight are divided 3-5 times and are added in mixed material, and after
Continuous stirring 2-3 hours, stops stirring, obtains molding materials；
（3）By the molding materials curing molding, then cooled to room temperature is to get to the new material；Wherein, it is solidified into
Profile bar part is：180-185 DEG C of heat preservation 30-50 min, 200-220 DEG C of heat preservation 0.5-1h, 250-280 DEG C of heat preservation 3-6h.
The enhancing component is prepared by the following method：
By vinal 35-45 parts by weight, urea 5-10 parts by weight, citric acid 8-15 parts by weight, potassium titanate crystal whisker 5-10
Parts by weight, methylcellulose 5-10 parts by weight, polyethylene glycol 5-10 parts by weight and feldspar in powder 3-5 parts by weight are put into batch mixer
In, batch mixing is carried out under high speed rate of rotation, high speed rate of rotation is 400-500 revs/min；
After stirring 0.5-1 hours, material is uniformly mixed, and lubricant 1-5 parts by weight are then added to uniformly mixed material again
In, the rotating speed of batch mixer is adjusted, batch mixing is carried out under low speed rate of rotation, wherein low speed rate of rotation is 80-120 revs/min, 30-40 points
Zhong Hou, material are uniformly mixed, and are stopped operating to get to the enhancing component.
The lubricant is in glycerine monofatty ester, dimer (fatty acid) yl diisocyanate, methyl sodiosul foaliphatate
It is any.
The mixing device is batch mixer.
In step（1）In, the rate for controlling the stirring is 100-200 revs/min.
The invention has the advantages that compared with the prior art,：It is added using vinal as the enhancing of key component
Material so that the tensile strength and bending strength of resin material are improved, and extend the application range of material.
Specific implementation mode
Below by specific embodiment, the invention will be further described：
Embodiment 1
A kind of preparation method of reinforced polyether ether ketone resin new material, the preparation method include the following steps：
（1）115 parts by weight of polyether-ether-ketone resin, 50 weight of copolymer of caprolactone and dimethyl siloxane by the degree of polymerization for 70
Part, 30 parts by weight of polyamic acid, 23 parts by weight of maleic anhydride, 13 parts by weight of dioctyl phthalate and 0.01-0.05 weight
The tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law chloride of part, polyoxy isobutylene/methylene of 0.01-0.05 parts by weight
The mixing for carrying out material is added in batch mixer in urea copolymer, 3 parts by weight, and mixed material is placed in 165 DEG C of temperature environment
Middle heating is melted, and is stirred during heating to mixed material, and the rate of stirring is 150 revs/min；
（2）After stirring 0.8 hour, enhancing 88 parts by weight of component are divided 4 times and are added in mixed material, and continue to stir
2.5 hour stops stirring, obtains molding materials；
The enhancing component is prepared by the following method：
By 40 parts by weight of vinal, 8 parts by weight of urea, 12 parts by weight of citric acid, 8 parts by weight of potassium titanate crystal whisker, methyl
8 parts by weight of cellulose, 8 parts by weight of polyethylene glycol and 4 parts by weight of feldspar in powder are put into batch mixer, are mixed under high speed rate of rotation
Material, high speed rate of rotation are 450 revs/min；
After stirring 0.8 hour, material is uniformly mixed, and is then again added to 3 parts by weight of glycerine monofatty ester uniformly mixed
In material, the rotating speed of batch mixer is adjusted, batch mixing is carried out under low speed rate of rotation, wherein low speed rate of rotation is 100 revs/min, 35 minutes
Afterwards, material is uniformly mixed, and is stopped operating to get to the enhancing component；
（3）By the molding materials curing molding, then cooled to room temperature is to get to the new material；Wherein, it is solidified into
Profile bar part is：183 DEG C of heat preservations 40min, 210 DEG C of heat preservations 0.8h, 265 DEG C of heat preservation 4.5h.
Embodiment 2
A kind of preparation method of reinforced polyether ether ketone resin new material, the preparation method include the following steps：
（1）90 parts by weight of polyether-ether-ketone resin, 35 weight of copolymer of caprolactone and dimethyl siloxane by the degree of polymerization for 60
Part, 25 parts by weight of polyamic acid, 20 parts by weight of maleic anhydride, 10 parts by weight of dioctyl phthalate and 0.01-0.05 weight
The tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law chloride of part, polyoxy isobutylene/methylene of 0.01-0.05 parts by weight
The mixing for carrying out material is added in batch mixer in urea copolymer, 1 parts by weight, and mixed material is placed in 160 DEG C of temperature environment
Middle heating is melted, and is stirred during heating to mixed material, and the rate of stirring is 100 revs/min；
（2）After stirring 0.5 hour, enhancing 67 parts by weight of component are added three times in mixed material, and continue stirring 2
Hour, stop stirring, obtains molding materials；
The enhancing component is prepared by the following method：
35 parts by weight of vinal, 5 parts by weight of urea, 8 parts by weight of citric acid, 5 parts by weight of potassium titanate crystal whisker, methyl is fine
Plain 5 parts by weight of dimension, 5 parts by weight of polyethylene glycol and 3 parts by weight of feldspar in powder are put into batch mixer, are mixed under high speed rate of rotation
Material, high speed rate of rotation are 400 revs/min；
After stirring 0.5 hour, material is uniformly mixed, and 1 parts by weight of dimer (fatty acid) yl diisocyanate are then added to mixing again
In uniform material, the rotating speed of batch mixer is adjusted, carries out batch mixing under low speed rate of rotation, wherein low speed rate of rotation is 80 revs/min, 30
After minute, material is uniformly mixed, and is stopped operating to get to the enhancing component；
（3）By the molding materials curing molding, then cooled to room temperature is to get to the new material；Wherein, it is solidified into
Profile bar part is：180 DEG C of heat preservations 30 min, 200 DEG C of heat preservations 0.5h, 250 DEG C of heat preservation 3h.
Embodiment 3
A kind of preparation method of reinforced polyether ether ketone resin new material, the preparation method include the following steps：
（1）120 parts by weight of polyether-ether-ketone resin, 60 weight of copolymer of caprolactone and dimethyl siloxane by the degree of polymerization for 80
Part,Polyamic acid35 parts by weight, 25 parts by weight of maleic anhydride, 15 parts by weight of dioctyl phthalate and 0.01-0.05 weight
The tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law chloride of part, polyoxy isobutylene/methylene of 0.01-0.05 parts by weight
The mixing for carrying out material is added in batch mixer in urea copolymer, 5 parts by weight, and mixed material is placed in 170 DEG C of temperature environment
Middle heating is melted, and is stirred during heating to mixed material, and the rate of stirring is 200 revs/min；
（2）After stirring 1 hour, enhancing 110 parts by weight of component are divided 5 times and are added in mixed material, and it is small to continue stirring 3
When, stop stirring, obtains molding materials；
The enhancing component is prepared by the following method：
By 45 parts by weight of vinal, 10 parts by weight of urea, 15 parts by weight of citric acid, 10 parts by weight of potassium titanate crystal whisker, first
10 parts by weight of base cellulose, 10 parts by weight of polyethylene glycol and 5 parts by weight of feldspar in powder are put into batch mixer, under high speed rate of rotation into
Row batch mixing, high speed rate of rotation are 500 revs/min；
After stirring 1 hour, material is uniformly mixed, and is then again added to 5 parts by weight of methyl sodiosul foaliphatate uniformly mixed
In material, the rotating speed of batch mixer is adjusted, batch mixing is carried out under low speed rate of rotation, wherein low speed rate of rotation is 120 revs/min, 40 minutes
Afterwards, material is uniformly mixed, and is stopped operating to get to the enhancing component；
（3）By the molding materials curing molding, then cooled to room temperature is to get to the new material；Wherein, it is solidified into
Profile bar part is：185 DEG C of heat preservations 50 min, 220 DEG C of heat preservations 1h, 280 DEG C of heat preservation 6h.
Comparative example 1
It is not added with vinal, the other the same as in Example 1.
Comparative example 2
It is not added with potassium titanate crystal whisker, the other the same as in Example 1.
Comparative example 3
It is not added with the copolymer of caprolactone and dimethyl siloxane, the other the same as in Example 1.
Comparative example 4
It is not added with tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law's chloride, the other the same as in Example 1.
Comparative example 5
It is not added with polyoxy isobutylene/methylene urea copolymer, the other the same as in Example 1.
Comparative example 6
It is not added with perfluoroalkyl silicyl mica, the other the same as in Example 1.
Table：The tensile strength of polyetheretherketonematerials materials made from different process and the comparing result of bending strength
| Number | Tensile strength/MPa | Bending strength/MPa |
| Embodiment 1 | 187 | 235 |
| Embodiment 2 | 185 | 232 |
| Embodiment 3 | 188 | 239 |
| Comparative example 1 | 161 | 207 |
| Comparative example 2 | 160 | 205 |
| Comparative example 3 | 158 | 199 |
| Comparative example 4 | 172 | 223 |
| Comparative example 5 | 169 | 211 |
| Comparative example 6 | 163 | 206 |
Claims (5)
1. a kind of preparation method of reinforced polyether ether ketone resin new material, which is characterized in that the preparation method includes following step
Suddenly：
（1）By the copolymer of polyether-ether-ketone resin 90-120 parts by weight, caprolactone and dimethyl siloxane that the degree of polymerization is 60-80
35-60 parts by weight, polyamic acid 25-35 parts by weight, maleic anhydride 20-25 parts by weight, dioctyl phthalate 10-15 weight
Part and tall oil alkyl benzyl hydroxyethyl imidazole quinoline nitrogen father-in-law chloride 0.01-0.05 parts by weight, polyoxy isobutylene/methylene urea
Copolymer 0.01-0.05 parts by weight, perfluoroalkyl silicyl mica 1-5 parts by weight, which are added in mixing device, carries out the mixed of material
Close, mixed material, which is placed in 160-170 DEG C of temperature environment heating, to be melted, and during heating to mixing after
Material be stirred；
（2）After stirring 0.5-1 hours, enhancing component 67-110 parts by weight are divided 3-5 times and are added in mixed material, and after
Continuous stirring 2-3 hours, stops stirring, obtains molding materials；
（3）By the molding materials curing molding, then cooled to room temperature is to get to the new material；Wherein, it is solidified into
The process conditions of type are：180-185 DEG C of heat preservation 30-50 min, 200-220 DEG C of heat preservation 0.5-1h, 250-280 DEG C of heat preservation 3-6h.
2. preparation method according to claim 1, which is characterized in that the enhancing component be prepared as follows and
At：
By vinal 35-45 parts by weight, urea 5-10 parts by weight, citric acid 8-15 parts by weight, potassium titanate crystal whisker 5-10
Parts by weight, methylcellulose 5-10 parts by weight, polyethylene glycol 5-10 parts by weight and feldspar in powder 3-5 parts by weight are put into batch mixer
In, batch mixing is carried out under high speed rate of rotation, high speed rate of rotation is 400-500 revs/min；
After stirring 0.5-1 hours, material is uniformly mixed, and lubricant 1-5 parts by weight are then added to uniformly mixed material again
In, the rotating speed of batch mixer is adjusted, batch mixing is carried out under low speed rate of rotation, wherein low speed rate of rotation is 80-120 revs/min, 30-40 points
Zhong Hou, material are uniformly mixed, and are stopped operating to get to the enhancing component.
3. preparation method according to claim 2, which is characterized in that the lubricant is glycerine monofatty ester, dimerization
Any one of aliphatic acid diisocyanate, methyl sodiosul foaliphatate.
4. preparation method according to claim 1, which is characterized in that the mixing device is batch mixer.
5. preparation method according to claim 1, which is characterized in that in step（1）In, the rate for controlling the stirring is
100-200 revs/min.
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| CN201810334757.2A CN108384187A (en) | 2018-04-15 | 2018-04-15 | A kind of preparation method of reinforced polyether ether ketone resin new material |
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| CN201810334757.2A CN108384187A (en) | 2018-04-15 | 2018-04-15 | A kind of preparation method of reinforced polyether ether ketone resin new material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109608823A (en) * | 2018-12-31 | 2019-04-12 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of composite material and preparation method for fan blade |
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2018
- 2018-04-15 CN CN201810334757.2A patent/CN108384187A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109608823A (en) * | 2018-12-31 | 2019-04-12 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of composite material and preparation method for fan blade |
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Application publication date: 20180810 |