CN106543687A - A kind of modified 3D printing resin of graphene oxide and its production method - Google Patents
A kind of modified 3D printing resin of graphene oxide and its production method Download PDFInfo
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- CN106543687A CN106543687A CN201610935406.8A CN201610935406A CN106543687A CN 106543687 A CN106543687 A CN 106543687A CN 201610935406 A CN201610935406 A CN 201610935406A CN 106543687 A CN106543687 A CN 106543687A
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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
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08L71/14—Furfuryl alcohol polymers
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/36—Furfuryl alcohol
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08L61/14—Modified phenol-aldehyde condensates
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to auxiliary material field is cast, the production method of the modified 3D printing resin of more particularly to a kind of graphene oxide.The invention provides a kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 7 13%, formic acid 1.5 2.5%, furfuryl alcohol 45 65%, formaldehyde 13 19%, resorcinol 7 13%, graphene oxide 3 7%, coupling agent 0.5 1.5% and ethylene urea 0.5 1.5%.For traditional deficiency of the steel-casting resin in terms of 3D molding sand printings in prior art, creative introduces graphene oxide, steel-casting scab is solved the problems, such as fundamentally, in addition, moulding can be implemented to the sand mo(u)ld of high heat-resisting, high rigidity, more complicated thinner high-end foundry goods can be used for, stable chemical performance, it is adaptable to use 3D printing technique, sand bond is high, it is easy to operate, anti-burnon excellent performance.
Description
Technical field
The present invention relates to cast auxiliary material field, the modified 3D printing resin of more particularly to a kind of graphene oxide and its
Production method.
Background technology
Traditional product manufacturing, is that raw material is shaped to blank using mould mostly, then using the side such as machining
Method removes excess stock, is shaped to the part of desired size, can be described as " subtracting material autofrettage ".And 3D forming techniques phase therewith
Instead, it is that three-dimensional objects entity is produced by the successively addition of material, is defined as " increasing material manufacturing " method.3D printing techniques have
The advantage such as section material, efficient, design liberalization, has had the developing history of more than 20 years in America and Europe, and Jing gets involved deeply work
Industry manufactures field.
Traditional cast steel self-hardening resin binding agent is mainly alkalescent phenol resin, because 3D molding sand print systems are glued to resin
Degree has very high requirement（＜ 15mpa.s, 25 DEG C）, viscosity height can block printhead, cause printhead distortion.Alkalescent phenol resin
Because its viscosity it is too high, it is impossible to meet the demand of 3D molding sand printing, and this kind of binding agent shelf-life is short, storage condition required very
It is high.Therefore, how to prepare it is a kind of efficiently, the stable chemical performance graphene oxide modified 3D printing resin low with viscosity into
For the problem of this area urgent need to resolve.
The content of the invention
For traditional deficiency of the steel-casting resin in terms of 3D molding sand printings in prior art, creative draws the present invention
Graphene oxide is entered, Graphene is both most thin material, and most tough material, because which is in molding sand normal temperature strength and high temperature
Advantage in terms of intensity, so the cast steel 3D printing resin being modified by Graphene can fundamentally solve steel-casting scab
Problem, in addition, moulding can be implemented to the sand mo(u)ld of high heat-resisting, high rigidity, more complicated thinner high-end foundry goods can be used for, chemically
Can be stable, it is adaptable to use 3D printing technique, sand bond is high, easy to operate, anti-burnon excellent performance.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
The present invention proposes a kind of modified 3D printing resin of graphene oxide, it is characterised in that including following chemical constituent：Benzene
Phenol, formic acid, furfuryl alcohol, formaldehyde, resorcinol, graphene oxide, coupling agent and ethylene urea.
Further, the modified 3D printing resin of the graphene oxide, it is characterised in that the quality of each chemical constituent
Percentage is：Phenol 7-13%, formic acid 1.5-2.5%, furfuryl alcohol 45-65%, formaldehyde 13-19%, resorcinol 7-13%, graphite oxide
Alkene 3-7%, coupling agent 0.5-1.5% and ethylene urea 0.5-1.5%.
Meanwhile, the present invention proposes a kind of production method of the modified 3D printing resin of graphene oxide, it is characterised in that
Comprise the following steps：
（1）To melt in phenol, formaldehyde, furfuryl alcohol input reactor, and add formic acid solution, open stirring, be passed through steam pressure
0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）To step（1）Graphene oxide is added in the polymer of production, steam is passed through, 1-3h is incubated；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol, ethylene urea and coupling agent to stir, both obtained steel-casting 3D printing resin.
Beneficial effects of the present invention are as follows：
1st, the modified 3D printing resin of graphene oxide that the present invention is provided is creative in process of production to introduce oxidation stone
Black alkene, by the introducing of graphene oxide, can improve the normal temperature strength and elevated temperature strength of molding sand, fundamentally prevent foundry goods and glue
The generation of sand defect；Meanwhile, Graphene is very thin material, has good elasticity again, can be used for more complicated thinner high-end casting
Part.
2nd, the graphene oxide that the present invention is provided is modified 3D printing resin because introducing Graphene, and Graphene has very
Good elasticity, stretch range can reach the 20% of own dimensions, and feeding excellent performance can be solved to a certain extent because of fluid shape
The casting defect that change brings.
3rd, the graphene oxide that the present invention is provided is modified 3D printing resin compared with traditional cast steel resin, with performance
It is stable, it is unlikely to deteriorate, viscosity is low, and mulling is convenient, advantage simple to operate.
Specific embodiment
In order that those skilled in the art more fully understand technical scheme, with reference to specific embodiment to this
Invention is described in further detail.The embodiments described below is exemplary, is only used for explaining the present invention, and is not understood that
For limitation of the present invention.
For traditional deficiency of the steel-casting resin in terms of 3D molding sand printings in prior art, creative draws the present invention
Graphene oxide is entered, Graphene is both most thin material, and most tough material, because which is in molding sand normal temperature strength and high temperature
Advantage in terms of intensity, so the cast steel 3D printing resin being modified by Graphene can fundamentally solve steel-casting scab
Problem, in addition, moulding can be implemented to the sand mo(u)ld of high heat-resisting, high rigidity, more complicated thinner high-end foundry goods can be used for, chemically
Can be stable, it is adaptable to use 3D printing technique, sand bond is high, easy to operate, anti-burnon excellent performance.
The invention provides a kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 7-13%, first
Sour 1.5-2.5%, furfuryl alcohol 45-65%, formaldehyde 13-19%, resorcinol 7-13%, graphene oxide 3-7%, coupling agent 0.5-1.5%
With ethylene urea 0.5-1.5%.Meanwhile, the present invention proposes a kind of production method of the modified 3D printing resin of graphene oxide, its
Preparation process is：（1）To melt in phenol, formaldehyde, furfuryl alcohol input reactor, and add formic acid solution, open stirring, be passed through steam
Pressure 0.1-0.2MPa, reaction temperature is at 80-110 DEG C；（2）To step（1）Graphene oxide is added in the polymer of production, is led to
Enter steam, be incubated 1-3h；（3）After insulation 1-3h, vacuum distillation kettle is transferred to, in temperature 60-80 DEG C, vacuum 0.05-
Vacuum distillation dehydration 1-2h under the conditions of 0.095MPa；（4）Resorcinol is added thereto to after distillation dehydration, 100-130 is warming up to
DEG C, it is incubated 1-3h；（5）Room temperature is down to, adds furfuryl alcohol, ethylene urea and coupling agent to stir, steel-casting has both been obtained with 3D printing tree
Fat.
Embodiment one
A kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 10%, formic acid 2%, furfuryl alcohol 55%, formaldehyde
16%th, resorcinol 10%, graphene oxide 5%, coupling agent 1% and ethylene urea 1%.
A kind of production method of the modified 3D printing resin of graphene oxide, its preparation process is：
（1）Melting phenol 10%, formaldehyde 16%, furfuryl alcohol 50% are put in reactor, formic acid solution 2% is added, stirring is opened, is passed through
Steam pressure 0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）Graphene oxide 5% is added in the polymer of first step production, steam is passed through, is incubated 1-3h；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol 10% is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol 5%, ethylene urea 1%, coupling agent 1% to stir, both obtained steel-casting 3D printing resin.
Embodiment two
A kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 7%, formic acid 2.5%, furfuryl alcohol 52%, formaldehyde
19%th, resorcinol 12%, graphene oxide 6%, coupling agent 0.5% and ethylene urea 1%.
A kind of production method of the modified 3D printing resin of graphene oxide, its preparation process is：
（1）Melting phenol 7%, formaldehyde 19%, furfuryl alcohol 50% are put in reactor, formic acid solution 2.5% is added, stirring is opened, is led to
Enter steam pressure 0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）Graphene oxide 6% is added in the polymer of first step production, steam is passed through, is incubated 1-3h；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol 12% is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol 2%, ethylene urea 1%, coupling agent 0.5% to stir, steel-casting has both been obtained with 3D printing tree
Fat.
Embodiment three
A kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 9%, formic acid 1.5%, furfuryl alcohol 64%, formaldehyde
13%th, resorcinol 8%, graphene oxide 3%, coupling agent 0.7% and ethylene urea 0.8%.
A kind of production method of the modified 3D printing resin of graphene oxide, its preparation process is：
（1）Melting phenol 9%, formaldehyde 13%, furfuryl alcohol 60% are put in reactor, formic acid solution 1.5% is added, stirring is opened, is led to
Enter steam pressure 0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）Graphene oxide 3% is added in the polymer of first step production, steam is passed through, is incubated 1-3h；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol 8% is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol 4%, ethylene urea 0.8%, coupling agent 0.7% to stir, steel-casting has both been obtained with 3D printing tree
Fat.
Example IV
A kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 8%, formic acid 1.8%, furfuryl alcohol 53%, formaldehyde
15%th, resorcinol 13%, graphene oxide 7%, coupling agent 1.2% and ethylene urea 1%.
A kind of production method of the modified 3D printing resin of graphene oxide, its preparation process is：
（1）Melting phenol 8%, formaldehyde 15%, furfuryl alcohol 48% are put in reactor, formic acid solution 1.8% is added, stirring is opened, is led to
Enter steam pressure 0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）Graphene oxide 7% is added in the polymer of first step production, steam is passed through, is incubated 1-3h；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol 13% is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol 5%, ethylene urea 1%, coupling agent 1.2% to stir, steel-casting has both been obtained with 3D printing tree
Fat.
Embodiment five
A kind of modified 3D printing resin of graphene oxide, its raw materials for production is：Phenol 13%, formic acid 2%, furfuryl alcohol 50%, formaldehyde
18%th, resorcinol 11%, graphene oxide 4%, coupling agent 1.5%, ethylene urea 0.5%.
A kind of production method of the modified 3D printing resin of graphene oxide, its preparation process is：
（1）Melting phenol 13%, formaldehyde 18%, furfuryl alcohol 42% are put in reactor, formic acid solution 2% is added, stirring is opened, is passed through
Steam pressure 0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）Graphene oxide 4% is added in the polymer of first step production, steam is passed through, is incubated 1-3h；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol 11% is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol 8%, ethylene urea 0.5%, coupling agent 1.5% to stir, steel-casting has both been obtained with 3D printing tree
Fat.
The modified 3D printing resin of graphene oxide that the above-mentioned embodiments of Jing are obtained has compared with traditional cast steel resin
There is stable performance, be unlikely to deteriorate, viscosity is low, mulling is convenient, advantage simple to operate；It is creative in process of production to introduce
Graphene oxide, by the introducing of graphene oxide, can improve the normal temperature strength and elevated temperature strength of molding sand, fundamentally prevent
The generation of foundry goods scab defect, meanwhile, Graphene is very thin material, has good elasticity again, and stretch range can reach itself
The 20% of size, feeding excellent performance can solve the casting defect brought because of fluid deformation to a certain extent, can be used for more multiple
Miscellaneous thinner high-end foundry goods.
Above the modified 3D printing of graphene oxide provided by the present invention is described in detail with resin, herein should
The principle and embodiment of the application are set forth with embodiment, the explanation of above example is only intended to help and understands
The present processes and its core concept；Simultaneously for one of ordinary skill in the art, according to the thought of the application, in tool
Will change in body embodiment and range of application, in sum, this specification content is should not be construed as to the application
Restriction.
Claims (3)
1. the modified 3D printing resin of a kind of graphene oxide, it is characterised in that including following chemical constituent：Phenol, formic acid, chaff
Alcohol, formaldehyde, resorcinol, graphene oxide, coupling agent and ethylene urea.
2. the modified 3D printing resin of graphene oxide as claimed in claim 1, it is characterised in that the matter of each chemical constituent
Measuring percentage is：Phenol 7-13%, formic acid 1.5-2.5%, furfuryl alcohol 45-65%, formaldehyde 13-19%, resorcinol 7-13%, oxidation stone
Black alkene 3-7%, coupling agent 0.5-1.5% and ethylene urea 0.5-1.5%.
3. the production method of the modified 3D printing resin of a kind of graphene oxide, it is characterised in that comprise the following steps：
（1）To melt in phenol, formaldehyde, furfuryl alcohol input reactor, and add formic acid solution, open stirring, be passed through steam pressure
0.1-0.2MPa, reaction temperature is at 80-110 DEG C；
（2）To step（1）Graphene oxide is added in the polymer of production, steam is passed through, 1-3h is incubated；
（3）After insulation 1-3h, vacuum distillation kettle is transferred to, is subtracted under the conditions of temperature 60-80 DEG C, vacuum 0.05-0.095MPa
Pressure distillation dehydration 1-2h；
（4）Resorcinol is added thereto to after distillation dehydration, 100-130 DEG C is warming up to, 1-3h is incubated；
（5）Room temperature is down to, adds furfuryl alcohol, ethylene urea and coupling agent to stir, both obtained steel-casting 3D printing resin.
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| WO2019029641A1 (en) | 2017-08-11 | 2019-02-14 | 宁夏共享化工有限公司 | Self-hardening organic synthetic resin mixture used for additive manufacturing, and application therefor |
| CN110605774A (en) * | 2018-06-15 | 2019-12-24 | 科华控股股份有限公司 | Solution capable of cleaning nozzle of printing head of 3D printer |
| WO2020077882A1 (en) * | 2018-10-17 | 2020-04-23 | 沈阳铸造研究所有限公司 | Binder used for sand casting 3d printing and preparation method therefor |
| EP3615197A4 (en) * | 2017-06-05 | 2020-06-10 | Lawrence Livermore National Security, LLC | System and method for forming activated carbon aerogels and performing 3d printing |
| CN112142936A (en) * | 2020-08-31 | 2020-12-29 | 四川东树新材料有限公司 | Additive manufacturing rapid prototyping furan resin and preparation method thereof |
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| CN112142936A (en) * | 2020-08-31 | 2020-12-29 | 四川东树新材料有限公司 | Additive manufacturing rapid prototyping furan resin and preparation method thereof |
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