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浙江大学学报（农业与生命科学版）
Journal of Zhejiang University (Agriculture and Life Sciences)  2023, Vol. 49 Issue (3): 398-412    DOI: 10.3785/j.issn.1008-9209.2022.04.181
Resource utilization & environmental protection     
Preparation of single-material carrier formulation fertilizer made by material extrusion three-dimensional printing and its controlled release effect
Xin ZHANG1(),Qian WU2,Qingxu MA1,Jun YIN2,Yinfeng HE3(),Lianghuan WU1()
1.Key Laboratory of Environment Remediation and Ecological Health, Ministry of Education, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058, Zhejiang, China
2.School of Mechanical Engineering, Zhejiang University, Hangzhou 310027, Zhejiang, China
3.Nottingham Ningbo China Beacons of Excellence Research and Innovation Institute, Ningbo 315000, Zhejiang, China
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Abstract  

As a processing technology that can rapidly fabricate customized products in small batches, three-dimensional (3D) printing has great application potential in horticultural gardens. On the basis of existing studies on controlled releasing materials for 3D printing, the carrier materials for solo nutrition were developed after a range of formulation screening. The new formulations were suitable for material extrusion 3D printing and the single-material carrier formulation fertilizer contained sodium alginate or xanthan gum as a binder, mannitol as a filler, ethanol/water with fixed ratio as a solvent, sepiolite as a thickening agent, and urea as the core fertilizer. It was confirmed that the maximum adding ratio of urea could reach 1∶4 [m (urea)∶V (solvent)] when using sodium alginate as a binder, while the maximum adding ratio could reach 3∶4 [m (urea)∶V (solvent)] when using xanthan gum as a binder. It was confirmed that the developed formulation could also be used as the carrier of other types of nutrients including KCl, K2HPO4, and ZnSO4. This work also demonstrated that it was possible to combine different nutrients and achieve element couplings by using multi-material extrusion 3D printing technology. Through the printing parameter adjustment experiment, the optimal printing was achieved when the printing speed was 200 mm/min, and the extrusion speed was 0.02 mm/s, and the extrusion height was 1 mm, and the nozzle diameter was 1 mm. The controlled release period of different formulations were further studied by the sand column leaching method. There were significant differences between the controlled release period of single-material carrier formulation fertilizers under different formulations and their post-treatments. The modified formulation with sepiolite can obviously change the release rate of single-material carrier formula fertilizer and the longest controlled release period reached 30 d.

Key words： material extrusion three-dimensional (3D) printing      new fertilizer      horticultural garden      controlled release effect     
Received: 18 April 2022      Published: 25 June 2023
CLC:  S143  
Corresponding Authors: Yinfeng HE,Lianghuan WU     E-mail: zhangxin1996@zju.edu.cn;Yinfeng.he@nottingham.ac.uk;finm@zju.edu.cn
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Xin ZHANG
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Qingxu MA
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Lianghuan WU
Cite this article:

Xin ZHANG,Qian WU,Qingxu MA,Jun YIN,Yinfeng HE,Lianghuan WU. Preparation of single-material carrier formulation fertilizer made by material extrusion three-dimensional printing and its controlled release effect. Journal of Zhejiang University (Agriculture and Life Sciences), 2023, 49(3): 398-412.

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https://www.zjujournals.com/agr/10.3785/j.issn.1008-9209.2022.04.181     OR     https://www.zjujournals.com/agr/Y2023/V49/I3/398


材料挤出三维打印单材料载体配方肥的制备与控释效果

三维打印（three-dimensional printing, 3D打印）作为一项可以快速小批量生产定制产品的加工技术，在园艺园林方向的应用潜力巨大。本研究借鉴3D打印缓释配方相关研究，完成单材料载体配方肥各组分的初步筛选，利用材料挤出3D打印技术成功打印出以海藻酸钠或黄原胶为黏结剂、甘露醇为填充剂、固定配比的乙醇溶液为溶剂、海泡石为增稠剂、尿素为核心肥料的单材料载体配方肥，确定尿素在海藻酸钠作为黏结剂时的最高添加比例为1∶4（尿素与溶剂质量体积比），而在黄原胶作为黏结剂时的最高添加比例为3∶4（尿素与溶剂质量体积比）；明确了用氯化钾、磷酸二氢钾、硫酸锌在最佳配方下替换尿素也可以实现打印；还通过多材料挤出3D打印技术进一步探讨了不同养分组合和元素耦合的打印可能性。通过打印参数调节试验明确了配方肥的最佳打印条件：打印速度200 mm/min、挤出速度0.02 mm/s、挤出高度1 mm、喷嘴直径1 mm。通过砂柱淋洗法进一步研究了不同配方肥的控释周期，发现不同配方及打印后处理下的单材料载体配方肥控释周期存在明显差异，经海泡石改良后的配方可以明显改变单材料载体配方肥的养分释放速率，其控释周期最长可达30 d。


关键词： 材料挤出三维打印,  新型肥料,  园艺园林,  控释效果 

配方

Formulation

甘露醇

Mannitol/g

海藻酸钠

Sodium alginate/g

黄原胶

Xanthan gum/g

尿素

Urea/g

溶剂体积比（乙醇∶水）

Solvent volume ratio (ethanol∶water)

溶剂

Solvent/mL

F1180.2003∶720
F2180.2053∶720
F3180.20103∶720
F4180.20153∶720
F5181.0003∶720
F6181.0053∶720
F7181.00103∶720
F8181.00153∶720
F91800.203∶720
F101800.253∶720
F111800.2103∶720
F121800.2153∶720
F131801.003∶720
F141801.053∶720
F151801.0103∶720
F161801.0153∶720
Table 1 Formulation table
Fig. 1 Experimental equipment and printing one-dimensional (1D) and 3D structural design diagramsA. Experimental 3D printer; B. “Ji” character structure; C. Printing design diagrams of the first layer with different porosities.
Fig. 2 Comparison pictures of formulations F1-F16 before and after inversionA. Front views of formulations F1-F8 (the red box marked represents solid-liquid separation); B. Front views of formulations F9-F16 (the red box marked represents solid-liquid separation); C. Upside-down views of formulations F1-F8 (the red box marked represents solid-liquid separation); D. Upside-down views of formulations F9-F16 (the red box marked represents the collapse part).
Fig. 3 Steady-state mechanical changes of viscosity and shear stress with shear rate for different formulations
Fig. 4 Dynamic loss factors for different formulations with angular frequency (A) and the average dynamic loss factors of different formulations (B)

打印参数

Printing

parameter

打印速度

Printing

speed/

(mm/min)

挤出速度

Extrusion

speed/

(mm/s)

喷嘴直径

Nozzle

diameter/

mm

温度

Temperature/

℃

a2500.05125
b2000.05125
c1500.05125
d1000.05125
e2500.02125
f2000.02125
g1500.02125
h1000.02125
Table 2 Adjustment of printing parameters
Fig. 5 Band performance of formulations F6 and F14 at different printing and extrusion speeds
Fig. 6 Band widths and fill rates under different printing parametersA-B. Band widths under different printing parameters of formulations F6 and F14; C-D. Fill rates under different printing parameters. Please see the Table 2 for the printing parameters of a-c and e-h.
Fig. 7 Modeling structures of the printable formulations in different printing parameters
Fig. 8 Relationships between printing speed and printing time of nozzle
Fig. 9 Display diagrams of “Zhejiang University school emblem” printed by different formulations
Fig. 10 Printing display diagram of formulation F14 (A), and the N cumulative release rates of formulations F6 and F14 before and after modification (B)
Fig. 11 N cumulative release rates of formulation F14 with different porositiesP0 represents 0 porosity, and P50 represents 50% porosity, and P67 represents 67% porosity.
Fig. 12 Multi-material 3D printing designA. Display diagram of composite structure; B-C. Display diagrams of composite structure printed by different combination formulations; D. Display diagram of core-shell structure; E. Display diagram of core-shell structure printed by different formulations. F17∶F6+sepiolite; F18: Replacing urea with KCl in formulation F14.
Fig. 13 SEM images of formulations F6 and F14 before and after modification

配方

Formulation

抗压强度

Compressive strength/N

含水率

Moisture content/%

F633.50±6.251.54

F6+海泡石

F6+sepiolite

＞501.48
F6+CaCl2＞502.68
F1438.33±7.681.58

F14+海泡石

F14+sepiolite

＞501.55
F15＞501.10
Table 3 Compressive strengths and moisture contents of different formulations
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