CN109569543A - A kind of compressible adsorbent material of 3D printing and preparation method thereof - Google Patents
A kind of compressible adsorbent material of 3D printing and preparation method thereof Download PDFInfo
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- CN109569543A CN109569543A CN201910017446.8A CN201910017446A CN109569543A CN 109569543 A CN109569543 A CN 109569543A CN 201910017446 A CN201910017446 A CN 201910017446A CN 109569543 A CN109569543 A CN 109569543A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/118—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using filamentary material being melted, e.g. fused deposition modelling [FDM]
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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
- B33Y10/00—Processes of additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The present invention discloses a kind of compressible adsorbent material of 3D printing and preparation method thereof, and the compressible adsorbent material of 3D printing is 50 ~ 70 parts of polyurethane (TPU), water-soluble pore creating material 10 ~ 25, biological material 20 ~ 40 according to weight percent composition.It is made by following methods: (1) each component being mixed and 3D printing wire rod is made by melting extrusion;(2) specific structure is printed as by FDM technology;(3) solvent is handled.It is good with desorption effect that the present invention prepares the absorption of compressible adsorbent material, can be applied to the absorption of sewage, air and organic contaminants in soil and heavy metal.
Description
Technical field
The invention belongs to environmental treatment technical fields, and in particular to a kind of compressible adsorbent material of 3D printing and its preparation side
Method.
Background technique
As process of industrialization accelerates, energy shortage and problem of environmental pollution become increasingly conspicuous.Water pollution is always one
Serious environmental problem, even micro heavy, dyestuff, drug are all great to human body damage in water body.In existing crowd
In more water treatment technologies, absorption is one of most simple, cost-effective method.Currently, researcher develops many novel suctions
Enclosure material, such as biological adsorption agent, polymer, metal oxide, nano material, chemical modification adsorbent.It is most of in these
High-efficiency adsorbent is mostly powder or particle, increases difficulty for recycling.The synthesis technology of expensive cost of material, complexity, difficult time
It receives the factors such as recycling and limits the practical application of these high-efficiency adsorbents.Therefore, it is necessary to study can low cost manufacturing and
The adsorbent of recycling and reusing can efficiently be desorbed.
3D printing is a kind of novel intelligent Manufacturing Technology, is compared compared to traditional molding mode, has and quickly prepares, is fine
The advantages that change manufactures, stock utilization is high.Wherein fused glass pellet (FDM) 3D printing technique the most universal, it can will be high
Molecular material is printed as the device of labyrinth.
It is basis material that the present invention, which selects elastomer, and TPU contains Soft hard segment structure, in compression process, is responsible for energy
The expendable variation to dissipate relates generally to the destruction of hard section, and hard segment structure generates Malin under the effect of big deformation repeated compression
This effect, derived from block structure sliding, broken and reconstruct;It is responsible for the deformation for restoring variation and relating generally to soft segment of elasticity, it is soft
It is good that section mutually raises flexibility, is conducive to reply;Hydrogen bond for hard section keep crystal phase be important, it is expected that fragmentation and it is unordered again
It accumulates and the fracture of hydrogen bond and re-forms related, and the release of hydrogen bond energy is the physical resources of energy dissipation.
Using the Nature biomass abundant as adsorbent material, raw material sources are abundant, realize its higher value application.By simple
Lignin from biomass and hemicellulose are extracted in solvent processing, retain cellulose skeleton and porous structure, while removing pore creating material,
Porous structure is formed in the life of TPU matrix, hole is conducive to inside solvent penetration, handles Internal biological matter.It is freeze-dried final
Obtain the high resiliency 3D printing absorption sponge of high porosity, low-density.Spongy tridimensional network has many attracting
Characteristic, such as reversible compression, high porosity, low-density and flexibility.The compressibility of micropore overall network is for pollutant
Quick adsorption and discharge it is particularly advantageous.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of 3D printing wire rod of achievable porous surface and
Preparation method.
In order to realize that the present invention, specific technical solution are as follows:
A kind of compressible adsorbent material of 3D printing, is made of the component of following weight percent:
Polyurethane (TPU) 50 ~ 70
Water-soluble pore creating material 10 ~ 25
Biological material 20 ~ 40.
The water-soluble pore creating material is one or more of in PVP, PVA, sucrose, NaCl, sodium carbonate.
The biological material is one or more of in wood powder, bamboo powder, stalk, rice hulls.
A kind of preparation method of the compressible adsorbent material of 3D printing, comprising the following steps:
(1) after polyurethane (TPU), water-soluble pore creating material, biological material being mixed according to the ratio, through double screw extruder [here
Step to refine again, be related to single, double screw extruder] melt blending, extrusion, granulation, then gained pellet is passed through into line
Material machine squeezes out, traction obtains 3D printing wire rod;
(2) 3D printing wire rod obtained in step (1) is printed as 3D device by FDM technology;
(3) 3D device obtained in step (2) is immersed in 2wt%NaClO2, it is anti-at 100 DEG C with second acid for adjusting pH=4.5
2 ~ 6 h are answered, then, react 6 ~ 8 h at 80 DEG C with 8wt%NaOH solution, use ethyl alcohol: water volume ratio is the ethyl alcohol of 40:60
It is cleaned in aqueous solution, finally, freeze-drying 24 hours.
The double screw extruder parameter are as follows: 60 ~ 160 DEG C of temperature, revolving speed is 50 ~ 250 rpm.
The wire rod machine parameter are as follows: 60 ~ 160 DEG C of temperature, revolving speed is 10 ~ 100 rpm.
The water-soluble pore creating material is one or more of in PVP, PVA, sucrose, NaCl, sodium carbonate.
The biological material is one or more of in wood powder, bamboo powder, stalk, rice hulls.
The above-mentioned compressible adsorbent material of a kind of 3D printing of the invention or the compressible adsorbent material of a kind of 3D printing
Preparation method application, which is characterized in that the application as rhodamine B adsorbent.
Beneficial effects of the present invention: (1) raw material sources enrich, are easy to get;(2) the compressible adsorbent material prepared is adsorbed and is taken off
Attached effect is good, can improve adsorption desorption efficiency by compress mode;(3) prepare compressible adsorbent material micro-nano hole is more, group
It is abundant, adsorption effect is good, can be applied to the absorption of sewage, air and organic contaminants in soil and heavy metal.
Detailed description of the invention
Fig. 1 is using 3D printing wire rod printing shaping product compression process figure prepared by the embodiment of the present invention 1.
Fig. 2 is to compress to adsorb to rhodamine B using 3D printing wire rod printing shaping product prepared by the embodiment of the present invention 1
Curve.
Specific embodiment
Embodiment 1
A kind of compressible adsorbent material of 3D printing is made of 60 parts of polyurethane (TPU), 10 parts of PVP, 30 parts of pine powder.
Preparation method is to sequentially include the following steps:
(1) it is added in double screw extruder and melts after mixing 6.0 kg TPU, 1.0 kg PVP, 3.0kg pine powder
It is blended, double screw extruder parameter are as follows: 80 DEG C of an area, two 90 DEG C of areas, three 100 DEG C of areas, four 120 DEG C of areas, five 135 DEG C of areas, 6th area
150 DEG C, seven 160 DEG C of areas, eight 160 DEG C of areas, nine 155 DEG C of areas, 150 DEG C of die head, revolving speed is 200 rpm, and extruding pelletization obtains wire rod
Master batch;10.0 kg wire rod master batches are added in wire rod machine machine and are processed, wire rod machine parameter are as follows: 150 DEG C of an area, two areas 160
DEG C, three 160 DEG C of areas, four 150 DEG C of areas, revolving speed is 50 rpm, and the silk cooling by water of extrusion by traction machine travel and controls wire vent
Line footpath obtains the 3D printing wire rod that porous surface can be achieved.
(2) by the above-mentioned 3D printing wire rod for obtaining can be achieved porous surface, hollow out is printed as by 3D printer (FDM)
Small cube, print temperature are 160 DEG C.
(3) hollow out small cube obtained in (2) is immersed in 2wt%NaClO2, with second acid for adjusting pH=4.5, at 100 DEG C
Lower reaction 2h.Then, 6 h are reacted at 80 DEG C with 8%NaOH solution.Finally in ethyl alcohol: water volume ratio is the ethanol water of 40:60
It is cleaned in solution, finally, freeze-drying 24 hours.
It is 100 mg/L's that obtained compressible adsorbent material hollow out small cube (see figure 1), which is added to 50 mL concentration,
In rhodamine B solution, compression absorption is specific as shown in Fig. 2, display has preferable absorption property.
Embodiment 2
A kind of compressible adsorbent material of 3D printing is made of 60 parts of polyurethane (TPU), 20 parts of PVA, 20 parts of pine powder.
Preparation method is to sequentially include the following steps:
(1) it is added in double screw extruder and melts after mixing 6.0 kg TPU, 2.0 kg PVA, 2.0kg pine powder
It is blended, double screw extruder parameter are as follows: 80 DEG C of an area, two 90 DEG C of areas, three 100 DEG C of areas, four 120 DEG C of areas, five 140 DEG C of areas, 6th area
150 DEG C, seven 160 DEG C of areas, eight 160 DEG C of areas, nine 150 DEG C of areas, 145 DEG C of die head, revolving speed is 200 rpm, and extruding pelletization obtains wire rod
Master batch;10.0 kg wire rod master batches are added in wire rod machine and are processed, wire rod machine parameter are as follows: 150 DEG C of an area, two areas 160
DEG C, three 160 DEG C of areas, four 150 DEG C of areas, revolving speed is 50 rpm, and the silk cooling by water of extrusion by traction machine travel and controls wire vent
Line footpath obtains the 3D printing wire rod that porous surface can be achieved.
(2) by the above-mentioned 3D printing wire rod for obtaining can be achieved porous surface, hollow out is printed as by 3D printer (FDM)
Small cube, print temperature are 160 DEG C.
(3) 3D device obtained in (2) is immersed in 2wt%NaClO2, anti-at 100 DEG C with second acid for adjusting pH=4.5
Answer 4 h.Then, 6 h are reacted at 80 DEG C with 8%NaOH solution.Finally in ethyl alcohol: water volume ratio is that the ethyl alcohol of 40:60 is water-soluble
It is cleaned in liquid, finally, freeze-drying 24 hours.
Embodiment 3
A kind of compressible adsorbent material of 3D printing is made of 70 parts of polyurethane (TPU), 10 parts of NaCl, 20 parts of bamboo powder.
Preparation method is to sequentially include the following steps:
(1) it is added in double screw extruder and melts after mixing 7.0 kg TPU, 1.0 kg NaCl, 2.0 kg bamboo powders
It is blended, double screw extruder parameter are as follows: 80 DEG C of an area, two 90 DEG C of areas, three 100 DEG C of areas, four 120 DEG C of areas, five 140 DEG C of areas, 6th area
150 DEG C, seven 160 DEG C of areas, eight 160 DEG C of areas, nine 150 DEG C of areas, 145 DEG C of die head, revolving speed is 200 rpm, and extruding pelletization obtains wire rod
Master batch;10.0 kg wire rod master batches are added in wire rod machine and are processed, wire rod machine parameter are as follows: 150 DEG C of an area, two areas 160
DEG C, three 160 DEG C of areas, four 150 DEG C of areas, revolving speed is 50 rpm, and the silk cooling by water of extrusion by traction machine travel and controls wire vent
Line footpath obtains the 3D printing wire rod that porous surface can be achieved.
(2) by the above-mentioned 3D printing wire rod for obtaining can be achieved porous surface, hollow out is printed as by 3D printer (FDM)
Small cube, print temperature are 160 DEG C.
(3) 3D device obtained in (2) is immersed in 2wt%NaClO2, anti-at 100 DEG C with second acid for adjusting pH=4.5
Answer 6 h.Then, 8 h are reacted at 80 DEG C with 8%NaOH solution.Finally in ethyl alcohol: water volume ratio is that the ethyl alcohol of 40:60 is water-soluble
It is cleaned in liquid, finally, freeze-drying 24 hours.
Embodiment 4
A kind of compressible adsorbent material of 3D printing is by 50 parts of polyurethane (TPU), NaCO320 parts, 30 parts of wheat bran compositions.
Preparation method is to sequentially include the following steps:
(1) by 5.0 kg TPU, 2.0 kg NaCO3, 3.0 kg wheat bran are added in double screw extruder and are melted after mixing
It is blended, double screw extruder parameter are as follows: 80 DEG C of an area, two 90 DEG C of areas, three 100 DEG C of areas, four 120 DEG C of areas, five 140 DEG C of areas, 6th area
150 DEG C, seven 160 DEG C of areas, eight 160 DEG C of areas, nine 150 DEG C of areas, 145 DEG C of die head, revolving speed is 200 rpm, and extruding pelletization obtains wire rod
Master batch;10.0 kg wire rod master batches are added in wire rod machine and are processed, wire rod machine parameter are as follows: 150 DEG C of an area, two areas 160
DEG C, three 160 DEG C of areas, four 150 DEG C of areas, revolving speed is 50 rpm, and the silk cooling by water of extrusion by traction machine travel and controls wire vent
Line footpath obtains the 3D printing wire rod that porous surface can be achieved.
(2) by the above-mentioned 3D printing wire rod for obtaining can be achieved porous surface, hollow out is printed as by 3D printer (FDM)
Small cube, print temperature are 160 DEG C.
(3) 3D device obtained in (2) is immersed in 2wt%NaClO2, anti-at 100 DEG C with second acid for adjusting pH=4.5
Answer 6 h.Then, 8 h are reacted at 80 DEG C with 8%NaOH solution.Finally in ethyl alcohol: water volume ratio is that the ethyl alcohol of 40:60 is water-soluble
It is cleaned in liquid, finally, freeze-drying 24 hours.
Claims (9)
1. a kind of compressible adsorbent material of 3D printing, which is characterized in that be made of the component of following weight percent:
Polyurethane (TPU) 50 ~ 70
Water-soluble pore creating material 10 ~ 25
Biological material 20 ~ 40.
2. the compressible adsorbent material of a kind of 3D printing according to claim 1, which is characterized in that the water-soluble pore-creating
Agent is one or more of in PVP, PVA, sucrose, NaCl, sodium carbonate.
3. the compressible adsorbent material of a kind of 3D printing according to claim 1, which is characterized in that the biological material
It is one or more of in wood powder, bamboo powder, stalk, rice hulls.
4. a kind of preparation method of any compressible adsorbent material of 3D printing of claim 1 ~ 3, which is characterized in that including
Following steps:
(1) it is melted altogether after according to the ratio mixing polyurethane (TPU), water-soluble pore creating material, biological material, through double screw extruder
Mixed, extrusion is granulated, then gained pellet is obtained 3D printing wire rod by wire rod machine extrusion, traction;
(2) 3D printing wire rod obtained in step (1) is printed as 3D device by FDM technology;
(3) 3D device obtained in step (2) is immersed in 2wt%NaClO2, with second acid for adjusting pH=4.5, reacted at 100 DEG C
2 ~ 6 h, then, react 6 ~ 8 h at 80 DEG C with 8wt%NaOH solution, use ethyl alcohol: water volume ratio is the ethanol water of 40:60
It is cleaned in solution, finally, freeze-drying 24 hours.
5. a kind of preparation method of the compressible adsorbent material of 3D printing according to claim 4, which is characterized in that described double
Screw extruder parameter are as follows: 60 ~ 160 DEG C of temperature, revolving speed is 50 ~ 250 rpm.
6. a kind of preparation method of the compressible adsorbent material of 3D printing according to claim 4, which is characterized in that the line
Material machine parameter are as follows: 60 ~ 160 DEG C of temperature, revolving speed is 10 ~ 100 rpm.
7. a kind of preparation method of the compressible adsorbent material of 3D printing according to claim 4, which is characterized in that described
Water-soluble pore creating material is one or more of in PVP, PVA, sucrose, NaCl, sodium carbonate.
8. a kind of preparation method of the compressible adsorbent material of 3D printing according to claim 4, which is characterized in that described
Biological material is one or more of in wood powder, bamboo powder, stalk, rice hulls.
One described in 9. claim 1 ~ the 3 any a kind of compressible adsorbent material of 3D printing or claim 4 ~ 8 is any
The application of the preparation method of the kind compressible adsorbent material of 3D printing, which is characterized in that the application as rhodamine B adsorbent.
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Cited By (2)
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CN110240218A (en) * | 2019-07-20 | 2019-09-17 | 福建师范大学 | Preparation method for synthesizing 3D framework @ MOFs water treatment device without adding metal salt |
CN110240219A (en) * | 2019-07-20 | 2019-09-17 | 福建师范大学 | A method of 3D skeleton@MOFs water disposal device is synthesized as metal source with 3D skeleton |
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CN110240218A (en) * | 2019-07-20 | 2019-09-17 | 福建师范大学 | Preparation method for synthesizing 3D framework @ MOFs water treatment device without adding metal salt |
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