CN107189378A - A kind of resistant to elevated temperatures 3D printing material of high tenacity for building - Google Patents
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building Download PDFInfo
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- CN107189378A CN107189378A CN201710463167.5A CN201710463167A CN107189378A CN 107189378 A CN107189378 A CN 107189378A CN 201710463167 A CN201710463167 A CN 201710463167A CN 107189378 A CN107189378 A CN 107189378A
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- 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
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
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Abstract
The invention discloses a kind of resistant to elevated temperatures 3D printing material of high tenacity for building, its raw material, which is pressed, includes polydactyl acid, phenolic resin, epoxy acrylic resin, silicon rubber, polyamide, haloflex, LLDPE, microcrystalline cellulose, ramee, dimethicone, glacial acetic acid, polycaprolactone, 4, 4 di-2-ethylhexylphosphine oxides (phenyl isocyanate), nano-aluminum hydroxide, nanometer silicon carbide, antimony oxide, micaceous iron oxide, trbasic zinc phosphate, silane coupler KH 570, stearic acid, chlorinated paraffin, accelerator, fire retardant, vulcanizing agent, plasticizer and modified toughened auxiliary agent.The 3D printing toughness of material of the present invention is good, with excellent resistance to elevated temperatures.
Description
Technical field
The present invention relates to the technical field of 3D printing material, more particularly to a kind of resistant to elevated temperatures 3D printing of high tenacity for building
Material.
Background technology
3D printing technique is also known as increases material manufacturing technology or rapid shaping technique, originates from earliest in the 1980s, being one
Kind by computer-aided design data by way of former is successively superimposed with material come realize entity manufacture technology.3D
Printing technique is a kind of emerging, rising manufacturing technology, realizes material from material is subtracted and is fabricated onto increasing material manufacturing
Great to change, the utilization rate of its material is more than 90%.With traditional industry subtract material manufacture compared with, 3D printing technique by produce make
Make and separated from large-scale, complicated traditional industry manufacturing process, change manufacturing philosophy, the production and processing side of traditional industry
Formula and management mode, will shake the whole world manufacturing industry, be known as " the third time industrial revolution " technology represent.3D printing technique
It has been widely used in the fields such as space flight and aviation, automobile making, teaching research and biomedicine.
At present, on the market the maximum and most widely used 3D printer of sales volume be can print the fusion sediments of engineering plastics into
Type 3D printer, the technology used is thermoplastic extrusion technology.But the degradability of its 3D printing material used is poor, toughness and resistance
Combustion performance can not meet demand during actual use, so needing a kind of resistant to elevated temperatures 3D printing material of high tenacity for building of design badly
To solve the problems of the prior art.
The content of the invention
To solve technical problem present in background technology, the present invention proposes that a kind of resistant to elevated temperatures 3D of high tenacity for building is beaten
Print material, good toughness, with excellent resistance to elevated temperatures.
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building proposed by the present invention, its raw material includes by weight:Change
80-120 parts of PLA of property, 4-8 parts of phenolic resin, 3-9 parts of epoxy acrylic resin, 2-6 parts of silicon rubber, polyamide 3-5
Part, 2-5 parts of haloflex, 2-6 parts of LLDPE, 15-25 parts of microcrystalline cellulose, 4-8 parts of ramee, diformazan
3-9 parts of base silicone oil, 2-6 parts of glacial acetic acid, 1-5 parts of polycaprolactone, 4-8 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), nanometer hydrogen-oxygen
Change 1-6 parts of aluminium, 2-8 parts of nanometer silicon carbide, 2-4 parts of antimony oxide, 1-5 parts of micaceous iron oxide, 3-8 parts of trbasic zinc phosphate, silane even
Join 2-5 parts of agent KH-570,2-5 parts of stearic acid, 1-4 parts of chlorinated paraffin, 1-5 parts of accelerator, 2-8 parts of fire retardant, vulcanizing agent 2-6
Part, 3-5 parts of plasticizer, modified toughened auxiliary agent 3-9 parts.
Preferably, polydactyl acid is prepared by following technique:In under nitrogen protection, by lactide, initiator, trichlorine
Methane and miscellaneous two ring of 1,8- dichloro-bicyclic (5,4,0) -7- 11 are dilute well mixed, heat up, insulation, then add benzoic acid and mix
Close uniform, stirring is subsequently added into isopropanol precipitating, and washing and filtering is dried to constant weight, is cooled to room temperature and obtains polydactyl acid.
Preferably, polydactyl acid is prepared by following technique:In under nitrogen protection, by lactide, initiator, trichlorine
Methane and miscellaneous two ring of 1,8- dichloro-bicyclic (5,4,0) -7- 11 are dilute well mixed, are warming up to 30-50 DEG C, are incubated 30-50min,
Then add benzoic acid to be well mixed, stir 20-30min in 350-450r/min rotating speeds, be subsequently added into isopropanol precipitating, wash
Filtering, dries to constant weight in 50-70 DEG C, is cooled to room temperature and obtains polydactyl acid.
Preferably, in the preparation technology of polydactyl acid, miscellaneous two ring of lactide, initiator, chloroform, 1,8- dichloros-
The weight ratio of the dilute, benzoic acid of bicyclic (5,4,0) -7- 11 and isopropanol is 5-15:1-3:2-5:3-6:1-4:2-6.
Preferably, in the preparation technology of polydactyl acid, initiator is by phenol and 1- hydroxyls pyrene by weight 1-3:2-6 is mixed
Conjunction is formed.
Preferably, modified toughened auxiliary agent is prepared by following technique:Hexamethylene diamine and phenylurea are well mixed, are warming up to
80-120 DEG C, 10-30min is incubated, then under nitrogen protection, flow back 16-20h in 100-110 DEG C, is subsequently cooled to room temperature,
Add ethyl acetate to be well mixed, then use and dried after salt acid elution, rotary evaporation to constant weight, be cooled to room temperature, then add
PLLA is well mixed, and in 60-100 DEG C of dry 2-4h, 5-15min then is blended in 160-200 DEG C, is cooled to room temperature and obtains
To modified toughened auxiliary agent.
Preferably, in the preparation technology of modified toughened auxiliary agent, hexamethylene diamine, phenylurea, ethyl acetate and PLLA
Weight ratio is 1-3:2-5:3-6:4-8.
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building of the present invention, its raw material, which is pressed, includes polydactyl acid, phenol
Urea formaldehyde, epoxy acrylic resin, silicon rubber, polyamide, haloflex, LLDPE, microcrystalline cellulose
Element, ramee, dimethicone, glacial acetic acid, polycaprolactone, 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), nano-aluminum hydroxide,
Nanometer silicon carbide, antimony oxide, micaceous iron oxide, trbasic zinc phosphate, Silane coupling reagent KH-570, stearic acid, chlorinated paraffin, promotion
Agent, fire retardant, vulcanizing agent, plasticizer and modified toughened auxiliary agent.Wherein, polydactyl acid is handed over by being protected down in nitrogen by third
Ester, initiator, chloroform and miscellaneous two ring of 1,8- dichloro-bicyclic (5,4,0) -7- 11 are dilute well mixed, heat up, insulation, so
Benzoic acid being added afterwards to be well mixed, stirring, being subsequently added into isopropanol precipitating, washing and filtering is dried to constant weight, is cooled to room temperature and obtains
To polydactyl acid, in the 3D printing material for applying to the present invention so that 3D printing material of the invention has excellent toughness
And resistance to elevated temperatures.Modified toughened auxiliary agent is heated up by the way that hexamethylene diamine and phenylurea are well mixed, and insulation is then protected in nitrogen
Under shield, backflow is subsequently cooled to room temperature, adds ethyl acetate and is well mixed, and then uses and is dried extremely after salt acid elution, rotary evaporation
Constant weight, is cooled to room temperature, then adds PLLA and is well mixed, dries, be then blended, be cooled to room temperature and obtain being modified increasing
In tough auxiliary agent, the 3D printing material for applying to the present invention, the toughness and heat-resisting quantity of 3D printing material of the present invention are effectively increased
Energy.The 3D printing toughness of material of the present invention is good, with excellent resistance to elevated temperatures.
Embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this hair
It is bright, rather than for limiting the invention, any modification made on the basis of the present invention, equivalent substitution etc. are in this hair
In bright protection domain.
Embodiment 1
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building proposed by the present invention, its raw material includes by weight:Change
100 parts of PLA of property, 6 parts of phenolic resin, 6 parts of epoxy acrylic resin, 4 parts of silicon rubber, 4 parts of polyamide, chlorinated polyethylene
3.5 parts of alkene, 4 parts of LLDPE, 20 parts of microcrystalline cellulose, 6 parts of ramee, 6 parts of dimethicone, glacial acetic acid 4
Part, 3 parts of polycaprolactone, 6 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), 3.5 parts of nano-aluminum hydroxide, 5 parts of nanometer silicon carbide, three
Aoxidize 3 parts of two antimony, 3 parts of micaceous iron oxide, 5.5 parts of trbasic zinc phosphate, 3.5 parts of Silane coupling reagent KH-570,3.5 parts of stearic acid, chlorination
2.5 parts of paraffin, 3 parts of accelerator, 5 parts of fire retardant, 4 parts of vulcanizing agent, 4 parts of plasticizer, 6 parts of modified toughened auxiliary agent.
Polydactyl acid is prepared by following technique:In under nitrogen protection, 10 parts of lactides, 2 parts are drawn by weight
Send out agent, 3.5 parts of chloroforms and miscellaneous two ring of 4.5 parts of 1,8- dichloros-bicyclic (5,4,0) -7- 11 dilute well mixed, be warming up to 40
DEG C, 40min is incubated, 2.5 parts of benzoic acid is then added and is well mixed, stir 25min in 400r/min rotating speeds, be subsequently added into 4 parts
Isopropanol precipitating, washing and filtering is dried to constant weight in 60 DEG C, is cooled to room temperature and obtains polydactyl acid.
In the preparation technology of polydactyl acid, initiator is by phenol and 1- hydroxyls pyrene by weight 2:4 mix.
Modified toughened auxiliary agent is prepared by following technique:2 parts of hexamethylene diamines and 3.5 parts of phenylureas are mixed equal by weight
It is even, 100 DEG C are warming up to, 20min is incubated, then under nitrogen protection, flow back 18h in 105 DEG C, is subsequently cooled to room temperature, adds
4.5 parts of ethyl acetate are well mixed, and are then used and are dried after salt acid elution, rotary evaporation to constant weight, are cooled to room temperature, then add
6 parts of PLLAs are well mixed, and in 80 DEG C of dry 3h, 10min then is blended in 180 DEG C, is cooled to room temperature and obtains being modified increasing
Tough auxiliary agent.
Embodiment 2
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building proposed by the present invention, its raw material includes by weight:Change
80 parts of PLA of property, 8 parts of phenolic resin, 3 parts of epoxy acrylic resin, 6 parts of silicon rubber, 3 parts of polyamide, haloflex
5 parts, it is 2 parts of LLDPE, 25 parts of microcrystalline cellulose, 4 parts of ramee, 9 parts of dimethicone, 2 parts of glacial acetic acid, poly-
5 parts of caprolactone, 4 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), 6 parts of nano-aluminum hydroxide, 2 parts of nanometer silicon carbide, three oxidations two
4 parts of antimony, 1 part of micaceous iron oxide, 8 parts of trbasic zinc phosphate, 2 parts of Silane coupling reagent KH-570,5 parts of stearic acid, 1 part of chlorinated paraffin, promotion
5 parts of agent, 2 parts of fire retardant, 6 parts of vulcanizing agent, 3 parts of plasticizer, 9 parts of modified toughened auxiliary agent.
Polydactyl acid is prepared by following technique:In under nitrogen protection, by weight by 5 parts of lactides, 3 parts of initiations
Agent, 2 parts of chloroforms and miscellaneous two ring of 6 parts of 1,8- dichloros-bicyclic (5,4,0) -7- 11 are dilute well mixed, are warming up to 30 DEG C, guarantor
Warm 50min, then adds 1 part of benzoic acid and is well mixed, stir 20min in 450r/min rotating speeds, be subsequently added into 6 parts of isopropyl alcohol precipitations
Form sediment, washing and filtering is dried to constant weight in 50 DEG C, is cooled to room temperature and obtains polydactyl acid.
In the preparation technology of polydactyl acid, initiator is by phenol and 1- hydroxyls pyrene by weight 1:6 mix.
Modified toughened auxiliary agent is prepared by following technique:1 part of hexamethylene diamine and 5 parts of phenylureas are mixed equal by weight
It is even, 80 DEG C are warming up to, 30min is incubated, then under nitrogen protection, flow back 20h in 100 DEG C, is subsequently cooled to room temperature, adds 3
Part ethyl acetate is well mixed, and is then used and is dried after salt acid elution, rotary evaporation to constant weight, be cooled to room temperature, then adds 8 parts
PLLA is well mixed, and in 60 DEG C of dry 4h, 15min then is blended in 160 DEG C, is cooled to room temperature and obtains modified toughened help
Agent.
Embodiment 3
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building proposed by the present invention, its raw material includes by weight:Change
120 parts of PLA of property, 4 parts of phenolic resin, 9 parts of epoxy acrylic resin, 2 parts of silicon rubber, 5 parts of polyamide, chlorinated polyethylene
2 parts of alkene, 6 parts of LLDPE, 15 parts of microcrystalline cellulose, 8 parts of ramee, 3 parts of dimethicone, 6 parts of glacial acetic acid,
1 part of polycaprolactone, 8 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), 1 part of nano-aluminum hydroxide, 8 parts of nanometer silicon carbide, three oxidations
Two 2 parts of antimony, 5 parts of micaceous iron oxide, 3 parts of trbasic zinc phosphate, 5 parts of Silane coupling reagent KH-570,2 parts of stearic acid, 4 parts of chlorinated paraffin, rush
Enter 1 part of agent, 8 parts of fire retardant, 2 parts of vulcanizing agent, 5 parts of plasticizer, 3 parts of modified toughened auxiliary agent.
Polydactyl acid is prepared by following technique:In under nitrogen protection, 15 parts of lactides, 1 part are drawn by weight
Send out agent, 5 parts of chloroforms and miscellaneous two ring of 3 parts of 1,8- dichloros-bicyclic (5,4,0) -7- 11 dilute well mixed, be warming up to 50 DEG C,
30min is incubated, 4 parts of benzoic acid is then added and is well mixed, stir 30min in 350r/min rotating speeds, be subsequently added into 2 parts of isopropanols
Precipitation, washing and filtering is dried to constant weight in 70 DEG C, is cooled to room temperature and obtains polydactyl acid.
In the preparation technology of polydactyl acid, initiator is by phenol and 1- hydroxyls pyrene by weight 3:2 mix.
Modified toughened auxiliary agent is prepared by following technique:3 parts of hexamethylene diamines and 2 parts of phenylureas are mixed equal by weight
It is even, 120 DEG C are warming up to, 10min is incubated, then under nitrogen protection, flow back 16h in 110 DEG C, is subsequently cooled to room temperature, adds 6
Part ethyl acetate is well mixed, and is then used and is dried after salt acid elution, rotary evaporation to constant weight, be cooled to room temperature, then adds 4 parts
PLLA is well mixed, and in 100 DEG C of dry 2h, 5min then is blended in 200 DEG C, is cooled to room temperature and obtains modified toughened help
Agent.
Embodiment 4
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building proposed by the present invention, its raw material includes by weight:Change
85 parts of PLA of property, 7 parts of phenolic resin, 4 parts of epoxy acrylic resin, 5 parts of silicon rubber, 3.5 parts of polyamide, chlorinated polyethylene
4 parts of alkene, 3 parts of LLDPE, 22 parts of microcrystalline cellulose, 5 parts of ramee, 8 parts of dimethicone, 3 parts of glacial acetic acid,
4 parts of polycaprolactone, 5 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), 5 parts of nano-aluminum hydroxide, 3 parts of nanometer silicon carbide, three oxidations
Two 3.5 parts of antimony, 2 parts of micaceous iron oxide, 7 parts of trbasic zinc phosphate, 3 parts of Silane coupling reagent KH-570,4 parts of stearic acid, 2 parts of chlorinated paraffin,
4 parts of accelerator, 3 parts of fire retardant, 5 parts of vulcanizing agent, 3.5 parts of plasticizer, 8 parts of modified toughened auxiliary agent.
Polydactyl acid is prepared by following technique:In under nitrogen protection, 8 parts of lactides, 2.5 parts are drawn by weight
Send out agent, 3 parts of chloroforms and miscellaneous two ring of 5 parts of 1,8- dichloros-bicyclic (5,4,0) -7- 11 dilute well mixed, be warming up to 35 DEG C,
45min is incubated, 2 parts of benzoic acid is then added and is well mixed, stir 22min in 420r/min rotating speeds, be subsequently added into 5 parts of isopropanols
Precipitation, washing and filtering is dried to constant weight in 55 DEG C, is cooled to room temperature and obtains polydactyl acid.
In the preparation technology of polydactyl acid, initiator is by phenol and 1- hydroxyls pyrene by weight 1.5:5 mix.
Modified toughened auxiliary agent is prepared by following technique:1.5 parts of hexamethylene diamines and 4 parts of phenylureas are mixed equal by weight
It is even, 85 DEG C are warming up to, 25min is incubated, then under nitrogen protection, flow back 19h in 102 DEG C, is subsequently cooled to room temperature, adds 4
Part ethyl acetate is well mixed, and is then used and is dried after salt acid elution, rotary evaporation to constant weight, be cooled to room temperature, then adds 7 parts
PLLA is well mixed, and in 65 DEG C of dry 3.5h, 12min then is blended in 165 DEG C, is cooled to room temperature and obtains modified toughened
Auxiliary agent.
Embodiment 5
A kind of resistant to elevated temperatures 3D printing material of high tenacity for building proposed by the present invention, its raw material includes by weight:Change
Property 115 parts of PLA, 5 parts of phenolic resin, 8 parts of epoxy acrylic resin, 3 parts of silicon rubber, 4.5 parts of polyamide, chlorination gather
3 parts of ethene, 5 parts of LLDPE, 18 parts of microcrystalline cellulose, 7 parts of ramee, 3 parts of dimethicone, glacial acetic acid 5
Part, 2 parts of polycaprolactone, 7 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), 2 parts of nano-aluminum hydroxide, 7 parts of nanometer silicon carbide, three oxygen
Change 2.5 parts of two antimony, 4 parts of micaceous iron oxide, 4 parts of trbasic zinc phosphate, 4 parts of Silane coupling reagent KH-570,3 parts of stearic acid, chlorinated paraffin 3
Part, 2 parts of accelerator, 7 parts of fire retardant, 3 parts of vulcanizing agent, 4.5 parts of plasticizer, 4 parts of modified toughened auxiliary agent.
Polydactyl acid is prepared by following technique:In nitrogen protection under, by weight by 12 parts of lactides, 1.5 parts
Initiator, 4 parts of chloroforms and miscellaneous two ring of 4 parts of 1,8- dichloros-bicyclic (5,4,0) -7- 11 are dilute well mixed, are warming up to 45
DEG C, be incubated 35min, then add 3 parts of benzoic acid and be well mixed, 28min is stirred in 380r/min rotating speeds, be subsequently added into 3 parts it is different
Propyl alcohol is precipitated, washing and filtering, is dried in 65 DEG C to constant weight, is cooled to room temperature and obtains polydactyl acid.
In the preparation technology of polydactyl acid, initiator is by phenol and 1- hydroxyls pyrene by weight 2.5:3 mix.
Modified toughened auxiliary agent is prepared by following technique:2.5 parts of hexamethylene diamines and 3 parts of phenylureas are mixed equal by weight
It is even, 115 DEG C are warming up to, 15min is incubated, then under nitrogen protection, flow back 17h in 108 DEG C, is subsequently cooled to room temperature, adds 5
Part ethyl acetate is well mixed, and is then used and is dried after salt acid elution, rotary evaporation to constant weight, be cooled to room temperature, then adds 5 parts
PLLA is well mixed, and in 95 DEG C of dry 2.5h, 8min then is blended in 195 DEG C, is cooled to room temperature and obtains modified toughened
Auxiliary agent.
By the resistant to elevated temperatures 3D printing material application of high tenacity for building in embodiment 1-5 into actual 3D printing production,
The performance of resulting product is detected that obtained data are as shown in table 1.
Table 1:
As shown in Table 1, the resistant to elevated temperatures 3D printing material of high tenacity for building in embodiment 1- embodiments 5 has excellent
Toughness and resistance to elevated temperatures.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of resistant to elevated temperatures 3D printing material of high tenacity for building, it is characterised in that its raw material includes by weight:It is modified poly-
80-120 parts of lactic acid, 4-8 parts of phenolic resin, 3-9 parts of epoxy acrylic resin, 2-6 parts of silicon rubber, 3-5 parts of polyamide, chlorine
Change 2-5 parts of polyethylene, 2-6 parts of LLDPE, 15-25 parts of microcrystalline cellulose, 4-8 parts of ramee, dimethyl-silicon
Oily 3-9 parts, 2-6 parts of glacial acetic acid, 1-5 parts of polycaprolactone, 4-8 parts of 4,4- di-2-ethylhexylphosphine oxides (phenyl isocyanate), nano-aluminum hydroxide
1-6 parts, 2-8 parts of nanometer silicon carbide, 2-4 parts of antimony oxide, 1-5 parts of micaceous iron oxide, 3-8 parts of trbasic zinc phosphate, silane coupler
2-5 parts of KH-570,2-5 parts of stearic acid, 1-4 parts of chlorinated paraffin, 1-5 parts of accelerator, 2-8 parts of fire retardant, 2-6 parts of vulcanizing agent, increasing
Mould 3-5 parts of agent, modified toughened auxiliary agent 3-9 parts.
2. the fire-retardant degradable 3D printing material of high tenacity according to claim 1, it is characterised in that polydactyl acid is by such as
It is prepared by lower technique:In under nitrogen protection, by lactide, initiator, chloroform and miscellaneous two ring of 1,8- dichloro-bicyclic (5,
4,0) -7- 11 is dilute well mixed, heats up, insulation, then adds benzoic acid and is well mixed, and stirring is subsequently added into isopropyl alcohol precipitation
Form sediment, washing and filtering is dried to constant weight, is cooled to room temperature and obtains polydactyl acid.
3. the fire-retardant degradable 3D printing material of high tenacity according to claim 1 or 2, it is characterised in that polydactyl acid
Prepared by following technique:In under nitrogen protection, by lactide, initiator, chloroform and miscellaneous two ring of 1,8- dichloro-bicyclic
(5,4,0) -7- 11 is dilute well mixed, is warming up to 30-50 DEG C, is incubated 30-50min, then adds benzoic acid and is well mixed, in
350-450r/min rotating speeds stir 20-30min, are subsequently added into isopropanol precipitating, and washing and filtering is dried to constant weight in 50-70 DEG C,
It is cooled to room temperature and obtains polydactyl acid.
4. the fire-retardant degradable 3D printing material of high tenacity according to claim any one of 1-3, it is characterised in that modified poly-
In the preparation technology of lactic acid, miscellaneous two ring of lactide, initiator, chloroform, 1,8- dichloros-bicyclic (5,4,0) -7- 11 is dilute,
The weight ratio of benzoic acid and isopropanol is 5-15:1-3:2-5:3-6:1-4:2-6.
5. the fire-retardant degradable 3D printing material of high tenacity according to claim any one of 1-4, it is characterised in that modified poly-
In the preparation technology of lactic acid, initiator is by phenol and 1- hydroxyls pyrene by weight 1-3:2-6 is mixed.
6. the fire-retardant degradable 3D printing material of high tenacity according to claim any one of 1-5, it is characterised in that modified to increase
Tough auxiliary agent is prepared by following technique:Hexamethylene diamine and phenylurea are well mixed, 80-120 DEG C is warming up to, 10- is incubated
30min, then under nitrogen protection, flow back 16-20h in 100-110 DEG C, is subsequently cooled to room temperature, adds ethyl acetate mixing
Uniformly, then use and dried after salt acid elution, rotary evaporation to constant weight, be cooled to room temperature, then add PLLA mixing equal
It is even, in 60-100 DEG C of dry 2-4h, 5-15min then is blended in 160-200 DEG C, is cooled to room temperature and obtains modified toughened auxiliary agent.
7. the fire-retardant degradable 3D printing material of high tenacity according to claim any one of 1-6, it is characterised in that modified to increase
In the preparation technology of tough auxiliary agent, hexamethylene diamine, phenylurea, the weight ratio of ethyl acetate and PLLA are 1-3:2-5:3-6:4-
8。
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