CN106009430A - Polytetrafluoroethylene powder material based on selective laser sintering and preparation method thereof - Google Patents
Polytetrafluoroethylene powder material based on selective laser sintering and preparation method thereof Download PDFInfo
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- CN106009430A CN106009430A CN201610422671.6A CN201610422671A CN106009430A CN 106009430 A CN106009430 A CN 106009430A CN 201610422671 A CN201610422671 A CN 201610422671A CN 106009430 A CN106009430 A CN 106009430A
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
Abstract
A polytetrafluoroethylene powder material based on selective laser sintering is characterized by being prepared from, by weight, 100 parts of polytetrafluoroethylene, 30 parts of high-density polyethylene, 0.5-2 parts of carbon, 0.2-2 parts of bronze, 0.05-0.5 part of carbon black, 0.1-2 parts of a flow promoting agent, 101-120 parts of a solvent, 0.5-1 part of an antioxidant, 0.2-2 parts of a silane coupling agent, 5-10 parts of a plasticizer, 0.5-2 parts of a light absorber and 0.2-0.5 part of a nucleating agent. The production cost is lowered by adding the high-density polyethylene with the melt index being 0.5-2 into the polytetrafluoroethylene, the defect that a powder material preparation technology is high in difficulty is overcome by adding the flow promoting agent, the antioxidant and the like, and the physical mechanical performance such as the shock resistance of the product is improved by adopting a reaction kettle and reasonably controlling technological parameters such as temperature and pressure.
Description
Technical field
The present invention relates to polymeric material field, particularly to a kind of polytetrafluorethylepowder powder material based on selective laser sintering and preparation method thereof.
Background technology
Selective laser sintering rapid forming technology (SLS) is to utilize dusty material principle of sintering under laser irradiates, and piles up molding the most layer by layer.SLS can shape multiple material, including polymer, metal and pottery etc..The crystalline state polymer being presently used for SLS mainly has nylon, wax, polyethylene etc., and owing to crystalline state polymer viscosity in sintering process is little, sintering rate is fast, thus its sintered part density is big, but can produce bigger mould shrinkage, causes its dimensional accuracy relatively low.And politef has the chemical-resistant of excellence, excellent in cushion effect, viscosity is high, can form the fine powder of 0.5 micron, well be applicable to the material of SLS.Visible, need to find a kind of SLS material, solve original SLS material preparation technology difficulty height, complex process, the defect of the aspect such as expensive.
Summary of the invention
The purpose of the present invention solves the above-mentioned problems in the prior art exactly, it is provided that a kind of polytetrafluorethylepowder powder material based on selective laser sintering and preparation method thereof.
Technical scheme is as follows:
A kind of polytetrafluorethylepowder powder material based on selective laser sintering, it is characterised in that: each composition weight number is as follows: politef: 100 parts；High density polyethylene (HDPE): 30 parts；Carbon: 0.5-2 part；Bronze: 0.2-2 part；White carbon black: 0.05-0.5 part；Flow promortor: 0.1-2 part；Solvent: 101-120 part；Antioxidant: 0.5-1 part；Silane coupler: 0.2-2 part；Plasticizer: 5-10 part；Light absorber: 0.5-2 part；Nucleator: 0.2-0.5 part.
The mean diameter of described politef is 0.1nm ~ 20nm.
The melt index of described high density polyethylene (HDPE) is the high density polyethylene (HDPE) of 0.5 ~ 2.
Described flow promortor is nano silicon, nano aluminium oxide or nano-calcium carbonate.
In described solvent, each volume components number is: ethanol 80-120 part；Butanone 10-15 part；Diethylene glycol 1-5 part；Water 10-15 part.
Described antioxidant is made up of with sulfur vinegar class with phosphorous acid lipid or phenols phenols.
Described plasticizer be hexylene glycol, glycerol, to the mixture of one or more in light yl benzoic acid vinegar, sulfonephthalein amine.
Described light absorber is benzophenone class, benzotriazole, triazines and one or more in hindered amines light absorber；Wherein benzophenone class light absorber is: 2,4-DihydroxyBenzophenone or 2-hydroxyl, 4-methoxy benzophenone, benzotriazole light absorber is 2-(2 ＇ hydroxyl-3 ＇, the 5 tertiary phenyl of ＇-two)-5-chlorination benzotriazole, triazines light absorber is 2,4,6-tri-(2 ＇-n-butoxyphenyl)-1,3,5 one triazines, hindered amines light absorber is two (2,2,6,6-tetramethyl-4-piperidyls) sebacate or double (1,2,2,6,6-pentamethyl-4-piperidyls) sebacate.
Described nucleator is any one in silicon dioxide, aquadag, lithium fluoride, boron nitride, Alborex M 12.
A kind of preparation method of polytetrafluorethylepowder powder material based on selective laser sintering, it is characterised in that: comprise the following steps:
Step one, politef and high density polyethylene (HDPE), carbon, white carbon black, bronze mixs, uniformly load in reactor, solvent is added in reactor, sealing, evacuation, it is passed through carbon dioxide, and to make reactor initial pressure be 0.1-0.3MPa；
Step 2, heating, make reactor be gradually heating to 150 ~ 180 DEG C, opens stirring, it is continuously heating to 180 ~ 220 DEG C, open drain tap, pressure in still is down to 1.3 ~ 1.4MPa, keeps 0.5 ~ 0.6 hour, the most uniform blood pressure lowering, make reacting kettle inner pressure be down to normal pressure in 1.9 ~ 2.4 hours, keep at ambient pressure 0.5 ~ 0.8 hour, stop stirring, being taken out from reactor by product puts into cold rinse bank, dries and obtains product；
Step 3, above-mentioned product and antioxidant, silane coupler, plasticizer, light absorber, nucleator are put in reactor together, close kettle cover, reactor is carried out evacuation process, and is passed through nitrogen, reactor is to slowly warm up to 160 ~ 190 DEG C, and is incubated 4 ~ 5 hours；
Step 4, temperature of reaction kettle is down to room temperature, take out material, in material, add flow promortor after being dried in atmosphere 11 ~ 12 hours, carry out ball milling 4 ~ 5 hours, again the powder body that ball milling obtains is put in vacuum drying oven and dry 45-48 hour, obtain polytetrafluorethylepowder powder material.
As can be seen from the above technical solutions, the present invention is that 0.5 ~ 2 high density polyethylene (HDPE) reduces production cost by adding melt index in politef, by add the auxiliary agent such as flow promortor, antioxidant solve dusty material difficulty of preparation technology high, defect, by use reactor and and conservative control temperature, the technological parameters such as pressure, the physical and mechanical properties such as shock resistance that improve product.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment
1
:
A kind of preparation method of polytetrafluorethylepowder powder material based on selective laser sintering, it is characterised in that: comprise the following steps:
Step one, politef and high density polyethylene (HDPE), carbon, white carbon black, bronze mixs, uniformly load in reactor, solvent is added in reactor, sealing, evacuation, it is passed through carbon dioxide, and to make reactor initial pressure be 0.1MPa；
Step 2, heating, make reactor be gradually heating to 150 DEG C, opens stirring, it is continuously heating to 180 DEG C, open drain tap, pressure in still is down to 1.3MPa, keeps 0.5 hour, the most uniform blood pressure lowering, make reacting kettle inner pressure be down to normal pressure in 1.9 hours, keep 0.5 hour at ambient pressure, stop stirring, being taken out from reactor by product puts into cold rinse bank, dries and obtains product；
Step 3, above-mentioned product and antioxidant, silane coupler, plasticizer, light absorber, nucleator are put in reactor together, close kettle cover, reactor is carried out evacuation process, and is passed through nitrogen, reactor is to slowly warm up to 160 DEG C, and is incubated 4 hours；
Step 4, temperature of reaction kettle is down to room temperature, takes out material, in material, add flow promortor after being dried in atmosphere 11 hours, carry out ball milling 4 hours, then the powder body obtained by ball milling is put in vacuum drying oven and dried 45 hours, obtains polytetrafluorethylepowder powder material.
Each composition weight number is:
Politef: 100 parts；High density polyethylene (HDPE): 30 parts；Carbon: 0.5 part；Bronze: 0.2 part；White carbon black: 0.05 part；Flow promortor: 0.1 part；Solvent: 101 parts；Antioxidant: 0.5 part；Silane coupler: 0.2 part；Plasticizer: 5 parts；Light absorber: 0.5 part；Nucleator: 0.2 part.
Embodiment
2
:
A kind of preparation method of polytetrafluorethylepowder powder material based on selective laser sintering, it is characterised in that: comprise the following steps:
Step one, politef and high density polyethylene (HDPE), carbon, white carbon black, bronze mixs, uniformly load in reactor, solvent is added in reactor, sealing, evacuation, it is passed through carbon dioxide, and to make reactor initial pressure be 0.3MPa；
Step 2, heating, make reactor be gradually heating to 180 DEG C, opens stirring, it is continuously heating to 220 DEG C, open drain tap, pressure in still is down to 1.4MPa, keeps 0.6 hour, the most uniform blood pressure lowering, make reacting kettle inner pressure be down to normal pressure in 2.4 hours, keep 0.8 hour at ambient pressure, stop stirring, being taken out from reactor by product puts into cold rinse bank, dries and obtains product；
Step 3, above-mentioned product and antioxidant, silane coupler, plasticizer, light absorber, nucleator are put in reactor together, close kettle cover, reactor is carried out evacuation process, and is passed through nitrogen, reactor is to slowly warm up to 190 DEG C, and is incubated 5 hours；
Step 4, temperature of reaction kettle is down to room temperature, takes out material, in material, add flow promortor after being dried in atmosphere 12 hours, carry out ball milling 5 hours, then the powder body obtained by ball milling is put in vacuum drying oven and dried 48 hours, obtains polytetrafluorethylepowder powder material.
Each composition weight number is:
Politef: 100 parts；High density polyethylene (HDPE): 30 parts；Carbon: 2 parts；Bronze: 2 parts；White carbon black: 0.5 part；Flow promortor: 2 parts；Solvent: 120 parts；Antioxidant: 1 part；Silane coupler: 2 parts；Plasticizer: 10 parts；Light absorber: 2 parts；Nucleator: 0.5 part.
Performance test:
By embodiment 1, finished-product material obtained by 2 is shaped to product by SLS technology, and carries out performance test, obtains tests below data:
| Hot strength (Mpa) | Elastic modelling quantity (Mpa) | Bending strength (Mpa) | Bending modulus (Mpa) | Impact strength (Mpa) | Precision (um) | |
| Experimental example 1 | 74.5 | 1870.3 | 115.6 | 2350 | 47.5 | 20 |
| Experimental example 2 | 135.6 | 2561 | 145.2 | 3255 | 55.6 | 30 |
Visible, the goods obtained by polytetrafluorethylepowder powder material that the preparation method of employing the application and component proportion are produced have higher physical and mechanical properties and dimensional accuracy.
Finally illustrate is, above example is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to preferred embodiment, it will be understood by those within the art that, technical scheme can be modified or equivalent, without deviating from objective and the scope of technical solution of the present invention, it is encompassed by the middle of scope of the presently claimed invention.
Claims (10)
1. a polytetrafluorethylepowder powder material based on selective laser sintering, it is characterised in that: each composition weight number is as follows: politef: 100 parts；High density polyethylene (HDPE): 30 parts；Carbon: 0.5-2 part；Bronze: 0.2-2 part；White carbon black: 0.05-0.5 part；Flow promortor: 0.1-2 part；Solvent: 101-120 part；Antioxidant: 0.5-1 part；Silane coupler: 0.2-2 part；Plasticizer: 5-10 part；Light absorber: 0.5-2 part；Nucleator: 0.2-0.5 part.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1, it is characterised in that: the mean diameter of described politef is 0.1nm ~ 20nm.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1 and 2, it is characterised in that: the melt index of described high density polyethylene (HDPE) is the high density polyethylene (HDPE) of 0.5 ~ 2.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1, it is characterised in that: described flow promortor is nano silicon, nano aluminium oxide or nano-calcium carbonate.
5. according to a kind of based on selective laser sintering the polytetrafluorethylepowder powder material described in claim 3 or 4, it is characterised in that: in described solvent, each volume components number is: ethanol 80-120 part；Butanone 10-15 part；Diethylene glycol 1-5 part；Water 10-15 part.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1, it is characterised in that: described antioxidant is made up of with sulfur vinegar class with phosphorous acid lipid or phenols phenols.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1, it is characterised in that: described plasticizer be hexylene glycol, glycerol, to the mixture of one or more in light yl benzoic acid vinegar, sulfonephthalein amine.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1, it is characterised in that: described light absorber is benzophenone class, benzotriazole, triazines and one or more in hindered amines light absorber；Wherein benzophenone class light absorber is: 2,4-DihydroxyBenzophenone or 2-hydroxyl, 4-methoxy benzophenone, benzotriazole light absorber is 2-(2 ＇ hydroxyl-3 ＇, the 5 tertiary phenyl of ＇-two)-5-chlorination benzotriazole, triazines light absorber is 2,4,6-tri-(2 ＇-n-butoxyphenyl)-1,3,5 one triazines, hindered amines light absorber is two (2,2,6,6-tetramethyl-4-piperidyls) sebacate or double (1,2,2,6,6-pentamethyl-4-piperidyls) sebacate.
A kind of polytetrafluorethylepowder powder material based on selective laser sintering the most according to claim 1, it is characterised in that: described nucleator is any one in silicon dioxide, aquadag, lithium fluoride, boron nitride, Alborex M 12.
10. according to the preparation method of a kind of based on selective laser sintering the polytetrafluorethylepowder powder material described in any one of claim 1-9, it is characterised in that: comprise the following steps:
Step one, politef and high density polyethylene (HDPE), carbon, white carbon black, bronze mixs, uniformly load in reactor, solvent is added in reactor, sealing, evacuation, it is passed through carbon dioxide, and to make reactor initial pressure be 0.1-0.3MPa；
Step 2, heating, make reactor be gradually heating to 150 ~ 180 DEG C, opens stirring, it is continuously heating to 180 ~ 220 DEG C, open drain tap, pressure in still is down to 1.3 ~ 1.4MPa, keeps 0.5 ~ 0.6 hour, the most uniform blood pressure lowering, make reacting kettle inner pressure be down to normal pressure in 1.9 ~ 2.4 hours, keep at ambient pressure 0.5 ~ 0.8 hour, stop stirring, being taken out from reactor by product puts into cold rinse bank, dries and obtains product；
Step 3, above-mentioned product and antioxidant, silane coupler, plasticizer, light absorber, nucleator are put in reactor together, close kettle cover, reactor is carried out evacuation process, and is passed through nitrogen, reactor is to slowly warm up to 160 ~ 190 DEG C, and is incubated 4 ~ 5 hours；
Step 4, temperature of reaction kettle is down to room temperature, take out material, in material, add flow promortor after being dried in atmosphere 11 ~ 12 hours, carry out ball milling 4 ~ 5 hours, again the powder body that ball milling obtains is put in vacuum drying oven and dry 45-48 hour, obtain polytetrafluorethylepowder powder material.
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Cited By (6)
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| CN110467769A (en) * | 2019-08-26 | 2019-11-19 | 华南理工大学 | A kind of anti-oxidant high-density polyethylene composite material and preparation method thereof |
| CN110982201A (en) * | 2019-11-04 | 2020-04-10 | 常州容和高分子材料科技有限公司 | Preparation process of modified PTFE (Polytetrafluoroethylene) oil seal material |
| WO2021214664A1 (en) | 2020-04-21 | 2021-10-28 | 3M Innovative Properties Company | Particles including polytetrafluoroethylene and process for making a three-dimensional article |
| WO2022113926A1 (en) * | 2020-11-25 | 2022-06-02 | Ａｇｃ株式会社 | Composition, laminate , and film of tetrafluoroethylene-based polymer |
| WO2023063297A1 (en) * | 2021-10-13 | 2023-04-20 | ダイキン工業株式会社 | Composition, circuit board, and method for producing composition |
| US11731346B2 (en) | 2020-03-02 | 2023-08-22 | Honeywell Federal Manufacturing & Technologies, Llc | Additively manufacturing fluorine-containing polymers |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110467769A (en) * | 2019-08-26 | 2019-11-19 | 华南理工大学 | A kind of anti-oxidant high-density polyethylene composite material and preparation method thereof |
| CN110982201A (en) * | 2019-11-04 | 2020-04-10 | 常州容和高分子材料科技有限公司 | Preparation process of modified PTFE (Polytetrafluoroethylene) oil seal material |
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| WO2021214664A1 (en) | 2020-04-21 | 2021-10-28 | 3M Innovative Properties Company | Particles including polytetrafluoroethylene and process for making a three-dimensional article |
| WO2022113926A1 (en) * | 2020-11-25 | 2022-06-02 | Ａｇｃ株式会社 | Composition, laminate , and film of tetrafluoroethylene-based polymer |
| WO2023063297A1 (en) * | 2021-10-13 | 2023-04-20 | ダイキン工業株式会社 | Composition, circuit board, and method for producing composition |
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