CN109161976A - A kind of 3D printing resin material for the field 4D of illumination reversible deformation - Google Patents
A kind of 3D printing resin material for the field 4D of illumination reversible deformation Download PDFInfo
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- CN109161976A CN109161976A CN201811029688.0A CN201811029688A CN109161976A CN 109161976 A CN109161976 A CN 109161976A CN 201811029688 A CN201811029688 A CN 201811029688A CN 109161976 A CN109161976 A CN 109161976A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/32—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising halogenated hydrocarbons as the major constituent
-
- 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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
- C08F259/02—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing chlorine
- C08F259/04—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing chlorine on to polymers of vinyl chloride
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
Abstract
The invention belongs to 3D printing Material Fields, particularly belong to the photosensitive 3D printing material of fusion sediment, the material is under no light condition (in camera bellows) after fusion sediment 3D printing molding, different forms can be presented by the illumination of varying strength, and metamorphosis is reversible, this invertibity is related to intensity of illumination.The material includes that following components in percentage by weight is prepared: polyvinyl chloride accounting weighs 6 ~ 33%, acrylonitrile accounting weight 5-7%, photosensitizer accounting weighs 10 ~ 20%, and light stabilizer accounting weighs 1 ~ 2%, and inversion agent accounting weighs 8 ~ 10, free radical accounting weight: 0.3 ~ 2%, light sensation cation and anion exchange compound accounting weighs 16 ~ 35%, and cationic initiator accounting weighs 0.5 ~ 2%, and anionic initiator accounting weighs 0.4 ~ 1.8%, Cationic Quench agent accounting weighs 0.2 ~ 0.8%, and anion quencher accounting weighs 0.4 ~ 1.2%.The applicable intensity of illumination range of photosensitive reversible 3D printing resin material of the invention is the lux 0.5LX ~ 140,000 (LX).The sensitive volume belongs to the universal illumination field of daily life field, therefore the photosensitive resin has more universal photosensitive property.
Description
Technical field
The invention belongs to 3D printing intellectual material technical field more particularly to a kind of 4D printing consumables of photosensitive reversible deformation
Preparation method and application.
Background technique
The it is proposed of 4D printing (Four-dimensional Printing) concept is the amusement design conference in 2013
On, it is put forward for the first time by the Tibbits et al. of the Massachusetts Institute of Technology.So-called 4D printing refers to its dimension more than 3D printing
Degree, i.e. time dimension, but its forming method remains and continues to use 3D printing molding.The three-dimensional article prepared by using 3D printing
Body, under specific environmental stimuli (such as light, sound, electricity, magnetic field, irradiation etc.), the physical characteristic (herein referring to shape) of material occurs
Change with the change of outside stimulus degree.4D prints many deficiencies for overcoming traditional 3D printing material, the material used in it
Material is a kind of intellectual material of sensitivity, and the research and development of this material is important for pushing the change in prospective material field to have
Meaning.
Currently, being still in infancy both at home and abroad for the research of 4D material, Temperature Excitation is all rested on mostly, and magnetic field is swashed
It encourages and light-sensitive material.Such as patent CN201810249105 proposes a kind of corresponding 4D printed material of magnetic.And patent
CN201410610090 proposes a kind of photosensitive 3D printing material, etc..These materials all have certain novelty.But these
Material is belonged to after extraneous incentive action, and shape is irreversible or expendable 3D printing material, therefore these materials
Material cannot be known as 4D printing consumables truly.And this 4D printed material proposed by the invention is a kind of photosensitive reversible
Deformable material, its deformation extent are related to the intensity of illumination of environment.The material not only prints field in 4D, or even in novel intelligence
Energy Material Field is all with a wide range of applications.
Summary of the invention
The object of the present invention is to provide a kind of systems of the 4D printed material of shape reversible deformation based on intensity of illumination response
Preparation Method, applicable intensity of illumination range are 0.5-140000LX, and excitation optical source wavelength range is 450-780nm.
The 4D printing consumables print temperature of photosensitive reversible deformation of the present invention is between 220-250 DEG C, and color is light
Sepia, corresponding deformation can be generated by meeting different illumination intensity due to this material, and this deformation is unfavorable for 3D printing molding, because
This present invention has strict demand to the intensity of illumination of Photocopy Room, that is, 10LX should be lower than by printing indoor intensity of illumination.
A kind of specific preparation method of 3D printing resin material for the field 4D of illumination reversible deformation of the present invention
It is as follows:
(1) in the Argyll Robertson pupil/sign Argyll-Robertson kettle for having vacuum stirring device and vacuum add-on system, quality described in accordance with the claim 1
Than sequentially adding polyvinyl chloride, acrylonitrile, photosensitizer, light stabilizer stirs in an atmospheric pressure environment then at 85 DEG C
It 120 minutes, softens it as light blue.
(2) then light blue softening object being vacuumized, is rushing nitrogen protection, vacuum degree is lower than in the no light conditions of 100Pa,
Inversion agent, free radical, light sensation cation and anion exchange compound, cationic initiator and anionic initiator are continuously added, is heated up
To 220 DEG C, stirring rate is that the reaction was continued 1 hour by 50 ~ 80r/min.
(3) intermediate product for preparing step 2 keeps vacuum degree and no light conditions constant, closes vacuum equipment and nitrogen
Equipment is protected, reduces temperature to 120 DEG C, anion quencher is added and Cationic Quench agent continues to stir 30min.
(4) intermediate product for preparing step 3 is placed in mixer after 160-180 DEG C of mixing 90min, at 50 DEG C
Raw material are made in unglazed freeze-day with constant temperature 6 hours.
(5) raw material described in step 4 are carried out squeezing out wire drawing, prepares the silk material that diameter is 0.8 ~ 3.5mm, extrusion process
Wire vent rate control is in 10M/min hereinafter, hot candied temperature is between 220-250 DEG C.
(6) silk material for preparing step 5 carries out normal-temperature vacuum drying 1 hour, and isolation air is kept in dark place.
Detailed description of the invention
Fig. 1 is Morphology of the molding fresh flower sample of material 3D printing of the present invention under different illumination intensity.
Fig. 2 is that photosensitive structure of the molding bird sample of material 3D printing of the present invention in the ten thousand LX illumination section 0.5-14 becomes
Change.
Fig. 3 is photosensitive change of the molding Eiffel Tower sample of material 3D printing of the present invention in the ten thousand LX illumination section 0.5-14
Change.
Specific embodiment
It illustrates and is described in detail below with reference to proportion described in claim 1 and its Rights attached thereto:
Embodiment 1
10 parts of polyvinyl chloride are taken, 6 parts of acrylonitrile, 12 parts of photosensitizer, 1.3 parts of light stabilizer are placed in vacuum mixer, with 60r/
The stirring rate of min is stirred 120 minutes in an atmospheric pressure environment, is softened it as light blue at 85 DEG C.Then will
Light blue softening object is vacuumizing, and rushes nitrogen protection, and vacuum degree is to continuously add 9 parts of inversion agent in the no light conditions of 50Pa, from
By 0.7 part of base, 20 parts of light sensation cation and anion exchange compound, 1.2 parts of cationic initiator and 0.8 part of anionic initiator are risen
For temperature to 220 DEG C, stirring rate is that the reaction was continued 1 hour by 70r/min.It then keeps vacuum degree and no light conditions constant, closes true
Null device and nitrogen protection equipment reduce temperature to 120 DEG C, are added 0.5 part and 0.3 part of Cationic Quench agent of anion quencher
Continue to stir 30min acquisition intermediate product.Then, intermediate product is placed in mixer after 170 DEG C of mixing 90min,
Raw material are made in unglazed freeze-day with constant temperature 6 hours at 50 DEG C.Raw material are carried out to squeeze out wire drawing, prepare the silk that diameter is 0.8mm
Material, extrusion process wire vent rate control is in 10M/min, and hot candied temperature is at 225 DEG C.The silk material of preparation is finally subjected to normal-temperature vacuum
1 hour dry, isolation air is kept in dark place.
Embodiment 2
30 parts of polyvinyl chloride are taken, 5.5 parts of acrylonitrile, 16 parts of photosensitizer, 1.5 parts of light stabilizer are placed in vacuum mixer, with
The stirring rate of 80r/min is stirred 120 minutes in an atmospheric pressure environment, is softened it as light blue at 85 DEG C.With
Light blue softening object is being vacuumized afterwards, is rushing nitrogen protection, vacuum degree is to continuously add inversion agent 8 in the no light conditions of 20Pa
Part, 0.5 part of free radical, 17 parts of light sensation cation and anion exchange compound, 1.6 parts of cationic initiator and anionic initiator 1.2
Part, 220 DEG C are warming up to, stirring rate is that the reaction was continued 1 hour by 75r/min.It then keeps vacuum degree and no light conditions constant, closes
Vacuum equipment and nitrogen protection equipment are closed, temperature is reduced to 120 DEG C, 0.8 part of anion quencher and Cationic Quench agent is added
0.5 part is continued to stir 30min acquisition intermediate product.Then, intermediate product is placed in mixer in 180 DEG C of mixing 90min
Afterwards, raw material are made in unglazed freeze-day with constant temperature 6 hours at 50 DEG C.Raw material are carried out to squeeze out wire drawing, preparing diameter is 3.5mm
Silk material, extrusion process wire vent rate control is in 5M/min, and hot candied temperature is at 240 DEG C.The silk material of preparation is finally subjected to room temperature
Vacuum drying 1 hour, isolation air are kept in dark place.
Embodiment 3
20 parts of polyvinyl chloride are taken, 7 parts of acrylonitrile, 15 parts of photosensitizer, 1 part of light stabilizer is placed in vacuum mixer, with 65r/min
Stirring rate stir 120 minutes, softened it as light blue in an atmospheric pressure environment at 85 DEG C.It then will be light blue
Color softening object is vacuumizing, and rushes nitrogen protection, and vacuum degree is to continuously add 10 parts of inversion agent, freely in the no light conditions of 40Pa
0.8 part of base, 32 parts of light sensation cation and anion exchange compound, 1.8 parts of cationic initiator and 1.3 parts of anionic initiator, heating
To 220 DEG C, stirring rate is that the reaction was continued 1 hour by 80r/min.It then keeps vacuum degree and no light conditions constant, closes vacuum
Equipment and nitrogen protection equipment reduce temperature to 120 DEG C, be added 0.8 part of 1.2 parts of anion quencher and Cationic Quench agent after
Continuous stirring 30min obtains intermediate product.Then, intermediate product is placed in mixer after 170 DEG C of mixing 90min, 50
Raw material are made in unglazed freeze-day with constant temperature 6 hours at DEG C.Raw material are carried out to squeeze out wire drawing, the silk material that diameter is 2mm is prepared, squeezes
Process wire vent rate control is in 8M/min out, and hot candied temperature is at 230 DEG C.The silk material of preparation is finally subjected to normal-temperature vacuum dry 1
Hour, isolation air is kept in dark place.
Claims (13)
1. a kind of 3D printing resin material of illumination reversible deformation, it is characterised in that: affiliated resin includes below by quality point
The raw material that number is constituted: polyvinyl chloride accounting weighs 6 ~ 33%, and acrylonitrile accounting weight 5-7%, photosensitizer accounting weighs 10 ~ 20%, light stabilizer
Accounting weighs 1 ~ 2%, and inversion agent accounting weighs 8 ~ 10, free radical accounting weight: 0.3 ~ 0.8%, light sensation cation and anion exchange compound accounting
16 ~ 35% are weighed, cationic initiator accounting weighs 0.5 ~ 2%, and anionic initiator accounting weighs 0.4 ~ 1.8%, Cationic Quench agent accounting
0.2 ~ 0.8% is weighed, anion quencher accounting weighs 0.4 ~ 1.2%.
2. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein photosensitizer is Hai Mubo
One of which in fragrant (hematoporphyrin monomethyl ether) and N- lucid asparagus acyl group chlorin.
3. light stabilizer according to claim 1 is hindered amine light stabilizer 3159, it belongs to high molecular weight piperazine ketone
Hindered amine light stabilizer.
4. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein inversion agent is 2- hydroxyl-
2- methyl-1-phenyl butyl ether.
5. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein free radical be super oxygen from
By base.
6. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein light sensation zwitterion is handed over
Changing compound is the positive hexadecyl ester of 3,5- di-tert-butyl-4-hydroxybenzoic acid, 4- benzyloxy -2- dihydroxy benaophenonel, N- (2- second
Phenyl)-N'- (2- ethylbenzene)-oxalyl and 2, the chemical reaction compound of 2,6,6- tetramethyl -4- piperidine esters.
7. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein cation light initiator
For alkyl sulfosalt.
8. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein anionic photoinitiators
Benzoin ether derivative.
9. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein Cationic Quench agent are
Nickel salt class excited state quenchers, nickel dibutyl dithiocarbamate.
10. a kind of 3D printing resin material of illumination reversible deformation according to claim 1, wherein anion quencher is
2,2- thiobis (4- tert-octyl phenol) n-butylamine nickel salt.
11. superoxide radical according to claim 5 the preparation method is as follows: BiOBr is close in light transmission with oxygen-enriched aqueous solution
It closes in container, at a temperature of -30 DEG C, in the environment of 10-50Pa vacuum degree, is placed in ultraviolet light 20 hours or so, wherein often
0.3 gram of BiOBr reaction is added in the oxygen-enriched aqueous solution of 100ml, and after completion of the reaction, vacuum degree is restored to normal pressure, slowly promotes temperature
Degree is rear closed to save backup to room temperature (1 DEG C/Min of heating rate).
12. light sensation cation and anion exchange compound according to claim 6 is the preparation method comprises the following steps: 3,5- di-t-butyl -4- hydroxyls
The positive hexadecyl ester of yl benzoic acid；4- benzyloxy -2- dihydroxy benaophenonel；N- (2- ethoxyl phenenyl)-N'- (2- ethylbenzene)-second
Two acyls and 2, the ratio that the mass ratioes of 2,6,6- tetramethyl -4- piperidine esters is 1:0.8:1.5:1 are uniformly mixed, with tablet press machine in
It is spare that 30MPa pressure pushes slabbing.
13. the 3D printing resin material of a kind of illumination reversible deformation according to claim 1, due to this material shape
Uncertain (material shape is related to environment illumination intensity), in order to ensure in 3D printing forming process, the stabilization of material shape
Property, printing environment is intensity of illumination between 0-10LX, and material hot briquetting temperature is 220 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811029688.0A CN109161976A (en) | 2018-09-05 | 2018-09-05 | A kind of 3D printing resin material for the field 4D of illumination reversible deformation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811029688.0A CN109161976A (en) | 2018-09-05 | 2018-09-05 | A kind of 3D printing resin material for the field 4D of illumination reversible deformation |
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| CN109161976A true CN109161976A (en) | 2019-01-08 |
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| CN201811029688.0A Pending CN109161976A (en) | 2018-09-05 | 2018-09-05 | A kind of 3D printing resin material for the field 4D of illumination reversible deformation |
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Citations (8)
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|---|---|---|---|---|
| CN101462891A (en) * | 2008-10-16 | 2009-06-24 | 中国科学院长春应用化学研究所 | Method for dynamically and invertibly regulating solid material surface wettability |
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| CN105399966A (en) * | 2015-12-29 | 2016-03-16 | 哈尔滨工业大学 | Preparation of shape-memory polymer and application of shape-memory polymer to 4D printing |
| CN106633721A (en) * | 2016-11-18 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Self-repair material and article with shape memory effect and preparation method thereof |
| CN106773532A (en) * | 2015-11-19 | 2017-05-31 | 芜湖启泽信息技术有限公司 | It is a kind of to be applied to photosensitive resin of 3D printing and preparation method thereof |
| CN107698718A (en) * | 2016-08-08 | 2018-02-16 | 惠展电子材料（上海）有限公司 | Photosensitive resin for laser 3D printing and preparation method thereof |
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| CN108484937A (en) * | 2018-04-02 | 2018-09-04 | 吉林大学 | A kind of preparation method of near infrared light driving 4D intelligent deformation materials |
-
2018
- 2018-09-05 CN CN201811029688.0A patent/CN109161976A/en active Pending
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Effective date of registration: 20190417 Address after: 330001 No. 7777 Changdong Avenue, Aixi Lake Management Office, Qingshan Lake District, Nanchang City, Jiangxi Province Applicant after: Inst. of Applied Physics, Jiangxi Prov. Academy of Sciences Address before: 330001 No. 7777 Changdong Avenue, Nanchang City, Jiangxi Province, Institute of Applied Physics, Jiangxi Academy of Sciences Applicant before: Fu Yuan |
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