CN115746500A - Organic silicon modified PEEK heat-shrinkable tube and preparation method thereof - Google Patents
Organic silicon modified PEEK heat-shrinkable tube and preparation method thereof Download PDFInfo
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- CN115746500A CN115746500A CN202211436975.XA CN202211436975A CN115746500A CN 115746500 A CN115746500 A CN 115746500A CN 202211436975 A CN202211436975 A CN 202211436975A CN 115746500 A CN115746500 A CN 115746500A
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- shrinkable tube
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 16
- 239000010703 silicon Substances 0.000 title claims abstract description 16
- -1 silicon modified PEEK Chemical class 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000004696 Poly ether ether ketone Substances 0.000 claims abstract description 33
- 229920002530 polyetherether ketone Polymers 0.000 claims abstract description 33
- 238000004132 cross linking Methods 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 19
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 6
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 claims abstract 7
- 238000001125 extrusion Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000011265 semifinished product Substances 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- AHWDQDMGFXRVFB-UHFFFAOYSA-N 1,3,5-trimethyl-1,3,5-triazinane-2,4,6-trione Chemical compound CN1C(=O)N(C)C(=O)N(C)C1=O AHWDQDMGFXRVFB-UHFFFAOYSA-N 0.000 claims description 2
- MPJPKEMZYOAIRN-UHFFFAOYSA-N 1,3,5-tris(2-methylprop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound CC(=C)CN1C(=O)N(CC(C)=C)C(=O)N(CC(C)=C)C1=O MPJPKEMZYOAIRN-UHFFFAOYSA-N 0.000 claims description 2
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 2
- GUTLYIVDDKVIGB-OUBTZVSYSA-N Cobalt-60 Chemical compound [60Co] GUTLYIVDDKVIGB-OUBTZVSYSA-N 0.000 claims description 2
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 2
- 230000005251 gamma ray Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims 1
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 claims 1
- 230000005855 radiation Effects 0.000 claims 1
- 239000000805 composite resin Substances 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000008602 contraction Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 229920006258 high performance thermoplastic Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention provides an organic silicon modified PEEK heat-shrinkable tube which comprises the following raw materials: PEEK resin: 70-95 parts of toughening precursor: 5-30 parts of crosslinking accelerator: 0.1-5 parts of antioxidant: 0.1-1 part, performing cross-linking reaction on a toughening precursor in the composite resin through high-energy ray irradiation to form a rubber phase, improving the toughness of the material, obviously reducing the pipe expanding processing temperature of the heat-shrinkable pipe by more than 80 ℃, and improving the shrinkage ratio of the PEEK heat-shrinkable pipe.
Description
Technical Field
The invention belongs to the field of processing of polymer composite materials, and particularly relates to an organic silicon modified PEEK heat-shrinkable tube and a preparation method thereof.
Background
PEEK (polyether ether ketone) is a wholly aromatic semi-crystalline high-performance thermoplastic resin containing ether bonds and carbonyl groups, has heat resistance, and has excellent friction resistance, high strength, high toughness, high dimensional stability, irradiation resistance, chemical corrosion resistance and fatigue resistance, and the long-term use temperature reaches 260 ℃. PEEK can be produced into products such as molded parts, pipes, bars, films and the like by means of injection molding, extrusion, mould pressing and the like through thermoforming, wherein PEEK heat-shrinkable tubes are products which are rapidly developed in recent years and can be used as connecting pieces or pipe sleeves for harsh environments or working conditions, such as nuclear-grade wire and cable connection or providing protective layers for key components in high-point equipment such as petroleum exploration, electronics, medical treatment and the like.
The conventional preparation method of the PEEK heat shrinkable tube is that a semi-finished tube is heated to a temperature above the glass transition temperature, and at the moment, PEEK resin shows partial high-elasticity property, expands and deforms the tube and keeps the state to be rapidly cooled and shaped; when in use, the heat shrinkable tube is heated to a high elastic state, so that the tube can automatically return to the original shape. The PEEK resin has high crystallinity (30 to 40 percent), and the crystallized part still has strong binding effect on PEEK macromolecules when heated to a high elastic state, so that the PEEK resin is difficult to deform and has poor toughness, and is easy to crack and break if the PEEK resin is expanded and deformed greatly, so that the expansion temperature of the heat-shrinkable tube prepared from the PEEK resin is high (300 to 330 ℃), and the product shrinkage ratio is only 1.1. The toughening agent is added in the formula, so that the toughness of the heat-shrinkable tube can be improved, the tube expansion processing temperature is reduced, the expansion rate is improved, and the shrinkage ratio is improved; however, common toughening agents such as POE, SEBS and the like cannot tolerate the processing temperature (350 to 400 ℃) of PEEK, and are decomposed or even carbonized in a large amount at high temperature.
Disclosure of Invention
Aiming at the defects in the field, the invention provides the organic silicon modified PEEK heat-shrinkable tube, wherein a toughening precursor of a polysiloxane component is added in the formula of the organic silicon modified PEEK heat-shrinkable tube, the organic silicon resin has excellent high-temperature resistance and can completely resist the PEEK processing temperature, the precursor resin has no obvious toughening effect, but the structure of the precursor resin has methyl-CH 3 Or vinyl-CH = CH 2 The active groups of the isoelectric rays can be excited by ionizing radiation such as gamma rays or electron beams to generate a crosslinking reaction, and the crosslinked organic silicon as rubber has a remarkable toughening effect compared with PEEK, so that the temperature required by pipe expanding processing is reduced, and the shrinkage ratio of a finished product is improved.
An organic silicon modified PEEK heat-shrinkable tube and a preparation method thereof are characterized by comprising the following raw materials in parts by mass:
PEEK resin: 70 to 95 portions of
Toughening a precursor: 5 to 30 portions of
Crosslinking accelerator: 0.1 to 5 portions
Antioxidant: 0.1 to 1 portion
The crosslinking accelerator is selected from at least one of trimethyl isocyanurate TMAIC and triallylisocyanurate oligomer.
The antioxidant is the combination of a main antioxidant and an auxiliary antioxidant.
The primary antioxidant is at least one selected from an antioxidant 1098 and an antioxidant 1010;
the secondary antioxidant is at least one of antioxidant 9228 and antioxidant 626;
the invention also provides a preparation method of the organic silicon modified PEEK heat-shrinkable tube, which comprises the process steps of extrusion granulation, extrusion molding, irradiation crosslinking and tube expansion shaping.
Preferably, the extrusion granulation process comprises: adding the PEEK resin, the toughening precursor, the crosslinking accelerator, the antioxidant and the lubricant into a high-speed mixer according to a ratio, uniformly mixing, adding into a double-screw extruder, and extruding and granulating to obtain heat-shrinkable tube resin particles;
further preferably, the temperature of the double-screw extruder is 340 to 380 ℃, the screw rotating speed is 400 to 600 r/min, and the feeding frequency is 8 to 15 Hz.
Preferably, the extrusion molding process comprises: drying the resin particles prepared by the extrusion granulation process, then performing melt extrusion by using a single-screw extruder, and molding by using a sizing sleeve and a vacuum cooling water tank to obtain a semi-finished product of the heat-shrinkable tube;
further preferably, the drying temperature of the resin particles is 140 ℃, and the drying time is 2-4h;
the temperature of the single-screw extruder is 350 to 390 ℃, and the extrusion speed is 2 to 8m/min.
Preferably, the irradiation crosslinking process comprises: performing irradiation crosslinking on the semi-finished product of the heat shrinkable tube by gamma rays or electron beams according to a certain dose;
further preferably, the gamma ray is generated by a cobalt 60 source, and the irradiation dose is 25 to 200 kGy;
the electron beam energy is 3 to 10 MeV, and the irradiation dose is 25 to 200 kGy.
Preferably, the pipe expanding and sizing process comprises the following steps: conveying the semi-finished product of the heat shrinkable tube after irradiation crosslinking to a heating chamber, simultaneously applying pressure to expand the heat shrinkable tube, controlling the expansion ratio of the outer diameter by a shaping device, and quickly cooling by a water tank to obtain a finished product of the heat shrinkable tube;
further preferably, the temperature of the heating chamber is 200 to 260 ℃, and the length of the heating chamber is 500 to 1500mm;
the expansion ratio is 1.5 to 1 to 2.5.
Compared with the prior art, the invention has the main advantages that:
1) According to the invention, the toughening precursor and the crosslinking accelerator are added into the formula, and the toughening precursor in the composite resin is subjected to crosslinking reaction to form a rubber phase through high-energy ray irradiation, so that the toughness of the material is improved, the pipe expansion processing temperature of the heat-shrinkable pipe can be obviously reduced by more than 80 ℃, and the shrinkage ratio of the PEEK heat-shrinkable pipe is improved.
2) According to the formula, the added toughening precursor is an organic silicon component, so that the flowability of the material can be improved and the processing temperature can be reduced without additionally adding a lubricating agent and a processing aid during screw extrusion processing, and the produced heat-shrinkable tube has smooth and smooth surface and good apparent quality.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are conducted under conditions not specified, usually according to conventional conditions, or according to conditions recommended by the manufacturer.
In the examples, the raw materials are shown in table 1 by weight, and the preparation method is as follows:
adding the raw material components into a high-speed mixer according to the proportion shown in the table 1, uniformly mixing, adding into a double-screw extruder, setting the temperature of the extruder to be 340-360 ℃, the rotating speed of a screw to be 400 r/min and the feeding frequency to be 10Hz, and extruding and granulating to obtain the heat-shrinkable tube resin particles.
And drying the resin particles at 140 ℃ for 4h, then adding the resin particles into a single-screw extruder, setting the temperature of the extruder to be 350-380 ℃, the extrusion speed to be 3m/min, melting and extruding the materials, and forming the materials through a sizing sleeve and a vacuum cooling water tank to obtain a semi-finished product of the heat-shrinkable tube.
And (3) performing irradiation crosslinking on the semi-finished product of the heat-shrinkable tube by using gamma rays or electron beams, and setting the irradiation dose to be 100 kGy.
And conveying the semi-finished product of the heat shrinkable tube after irradiation crosslinking to a heating chamber, setting the temperature of the heating chamber to be 220 ℃ and the length of the heating chamber to be 1200mm, applying pressure to expand the heat shrinkable tube, controlling the expansion ratio of the outer diameter by a shaping device, and quickly cooling by a water tank to obtain the finished product of the heat shrinkable tube.
TABLE 1
The raw material composition of the comparative example 1 is not added with toughening precursor, and the preparation method of the comparative example 1 is completely the same as the example.
The raw material composition of comparative example 2 was added with an excess amount of toughening precursor, and the preparation method was completely the same as in the examples.
Comparative example 3 the composition of the raw material was the same as that of example 2 except that no crosslinking accelerator was added and the preparation method of comparative example 3 was exactly the same as that of example.
The products obtained in the above examples and comparative examples were tested and the test results are shown in Table 2. The tensile strength and the elongation at break are tested according to GB/T1040.2; gradually increasing the expansion ratio when the maximum contraction ratio is produced until the heat shrinkable tube is cracked or damaged, wherein the contraction ratio corresponding to the maximum expansion ratio can be normally produced; the surface roughness of the pipe is tested according to GB/T14234.
TABLE 2
| Test item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Tensile Strength (MPa) | 73 | 81 | 75 | 67 | 61 | 70 | 85 | — | 72 |
| Elongation at Break (%) | 38 | 21 | 27 | 46 | 68 | 44 | 13 | — | 18 |
| Maximum shrinkage ratio | 2.1:1 | 1.8:1 | 1.6:1 | 2:1 | 2.5:1 | 2.4:1 | 1.1:1 | — | 1.4:1 |
| Surface roughness (Ra) | 0.75 | 0.82 | 0.86 | 0.87 | 0.61 | 0.68 | 1.02 | — | 0.79 |
According to the results in table 2, it can be known from examples 1 to 6 that the added toughening precursor has an obvious gain effect on the improvement of the PEEK heat shrinkable tube shrinkage ratio after irradiation crosslinking, and especially, when polymethyl vinyl siloxane containing unsaturated double bonds is added in example 5, the shrinkage ratio can reach 2.5; and the processing temperature can be reduced, and the prepared heat shrinkable tube product has smooth surface and low roughness.
Comparing comparative example 1 and the example, it is known that the expansion rate of the heat shrinkable tube under the same processing conditions is low without adding the toughening precursor, the final shrinkage ratio is only 1.1.
Comparative example 2 the strands were fluffy and foamed during extrusion granulation, and no subsequent production could be performed, due to the compatibility problem between silicone and PEEK resin, severe incompatibility occurred after addition of the amount of toughening precursor exceeding the compounding ratio.
As can be seen from comparison of comparative example 3 and example 2, direct irradiation crosslinking is also possible because the formulation contains unsaturated vinyl groups, but since the reaction efficiency is not as good as that of the crosslinking accelerator, the crosslinking is incomplete and the shrinkage ratio of the final product is not high.
According to the organic silicon modified PEEK heat-shrinkable tube and the preparation method thereof, organic silicon is added in a formula to serve as a toughening precursor, so that the fluidity of PEEK can be improved and the processing temperature is reduced by 10 to 30 ℃ when extrusion processing granulation and extrusion of a semi-finished tube are carried out; and the toughening precursor after irradiation crosslinking has excellent toughening effect as a rubber phase, can reduce the pipe expanding processing temperature by 80-100 ℃, and simultaneously remarkably improves the product shrinkage ratio. In addition, due to the characteristic of low surface energy of the organic silicon component, the prepared PEEK heat-shrinkable tube has smooth and smooth surface and good surface quality.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention as defined by the appended claims.
Claims (9)
1. An organic silicon modified PEEK heat-shrinkable tube is characterized by comprising the following raw materials in parts by mass:
PEEK resin: 70 to 95 portions of
Toughening a precursor: 5 to 30 portions of
Crosslinking accelerator: 0.1 to 5 portions of
Antioxidant: 0.1-1 part.
2. The silicone PEEK heat shrink tube of claim 1, wherein the toughening precursor is at least one of ultra-high molecular weight polydimethylsiloxane, polymethylvinylsiloxane, and polymethylphenylsiloxane.
3. The silicone-modified PEEK heat shrink tube according to claim 1, wherein the crosslinking accelerator is selected from at least one of trimethyl isocyanurate TMAIC and triallyl isocyanurate oligomer.
4. The silicone-modified PEEK heat shrinkable tube according to claim 1, wherein the antioxidant is a combination of a primary antioxidant and a secondary antioxidant;
the primary antioxidant is at least one of an antioxidant 1098 and an antioxidant 1010;
the auxiliary antioxidant is at least one of antioxidant 9228 and antioxidant 626.
5. The preparation method of the organic silicon modified PEEK heat shrinkable tube according to any one of claims 1 to 4, which is characterized by comprising the process steps of extrusion granulation, extrusion molding, irradiation crosslinking and tube expansion shaping.
6. The method of claim 5, wherein the extrusion granulation process comprises: adding the PEEK resin, the toughening precursor, the crosslinking accelerator and the antioxidant into a high-speed mixer according to a ratio, uniformly mixing, adding into a double-screw extruder, and extruding and granulating to obtain heat-shrinkable tube resin particles;
the temperature of the double-screw extruder is 340 to 380 ℃, the rotating speed of the screw is 400 to 600 r/min, and the feeding frequency is 8 to 15 Hz.
7. The method of manufacturing according to claim 5, wherein the extrusion molding process includes: drying the resin particles prepared by the extrusion granulation process, performing melt extrusion by using a single-screw extruder, and forming by using a sizing sleeve and a vacuum cooling water tank to obtain a semi-finished product of the heat shrinkable tube;
the drying temperature of the resin particles is 140 ℃, and the drying time is 2-4h;
the temperature of the single-screw extruder is 350 to 390 ℃, and the extrusion speed is 2 to 8m/min.
8. The method of claim 5, wherein the radiation crosslinking process comprises: performing irradiation crosslinking on the semi-finished product of the heat shrinkable tube by gamma rays or electron beams according to a certain dose;
the gamma ray is generated by a cobalt 60 source, and the irradiation dose is 25-200 kGy;
the electron beam energy is 0.5-10 MeV, and the irradiation dose is 25-200 kGy.
9. The method for preparing the pipe expanding and sizing material, wherein the pipe expanding and sizing process comprises the following steps: conveying the semi-finished product of the heat shrinkable tube after irradiation crosslinking to a heating chamber, simultaneously applying pressure to expand the heat shrinkable tube, controlling the expansion ratio of the outer diameter by a shaping device, and quickly cooling by a water tank to obtain a finished product of the heat shrinkable tube;
the temperature of the heating chamber is 200 to 260 ℃, and the length of the heating chamber is 500 to 1500mm;
the expansion ratio is 1.5 to 1 to 2.5.
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