新型淀粉基高吸水树脂抑尘剂的制备及其应用

doi:10.16085/j.issn.1000-6613.2022-1498

摘要/Abstract

摘要：

为了获得一种可工业化生产的淀粉基高吸水树脂抑尘材料，以木薯淀粉、丙烯酸为原料，过硫酸铵和亚硫酸钠为引发剂，N,N'-亚甲基双丙烯酰胺为交联剂，在机械活化作用下一步固相法合成木薯淀粉接枝丙烯酸高吸水性树脂抑尘剂。采用黏度、吸水率为评价指标，通过单因素和正交试验获得最优制备参数。采用FTIR、XRD、SEM、¹³C NMR等对产品进行了结构表征和应用性能测试。结果表明，木薯淀粉成功接枝丙烯酸形成高吸水性树脂，该方法能有效地破坏淀粉颗粒结构，提高反应效率。在球磨时间3h、中和度80%、反应温度60℃、丙烯酸与淀粉摩尔比为1∶1、引发剂用量0.9g、交联剂用量0.05g、球磨介质500mL、球磨转速380r/min条件下，所合成的淀粉基抑尘剂黏度为670mPa·s，吸水率为116.21g/g，单体转化率为96.81%，接枝率为42.35%，接枝效率为81.36%。喷洒浓度2%淀粉基抑尘剂的尘样可有效延长水分蒸发时间，固化尘样颗粒，增强尘样抗破坏性能，提高抑尘效果。尘样蒸发7h后含湿率仍高达6.85%，40目以上的尘样粒径达到38.93%，风速9m/s下的抑尘率达到96.40%，抑尘效果大大优于喷洒水的尘样，证明淀粉基抑尘剂为一种绿色环保型抑尘剂。

关键词: 机械活化固相法, 接枝淀粉, 聚合物, 制备, 抗蒸发性

Abstract:

To establish a starch-based super absorbent polymer dust suppressant for industrial manufacture, a super absorbent resin dust suppressant was synthesized by mechanical activation one-step solid phase (MAMS) method, which took cassava starch, acrylic acid (AA) as raw materials, ammonium persulfate (AP) and sodium sulfite (SS) as initiator, and N, N'-methylene bisacrylamide as cross-linking agent. Process conditions for preparation of the materials were optimized by orthogonal test and single factor method according to viscosity and water absorption rate. FTIR, XRD, SEM and ¹³C NMR were used to test and characterize the materials. The results showed that the cassava starch was successfully grafted with acrylic acid to form a super-absorbent resin. This method could effectively destroy the starch granule structure and improve the reaction efficiency. The optimal conditions were as follows. The ball milling reaction time was 3h, the AA neutralization degree was 80%, the reaction temperature was 60℃, the AA/starch mole ratio was 1∶1, the initiator dosage was 0.9g, the cross-linking agent dosage was 0.05g and the rotation speed of the ball mill was 380r/min with 500mL ball mill medium. Under these conditions, the viscosity of the dust suppressant was 670mPa·s, the water absorption ratio was 116.21g/g, and the monomer conversion, grafting rate and grafting efficiency were 96.81%, 42.35% and 81.36% respectively. The dust samples sprayed with a concentration of 2% starch-based dust inhibitor could effectively prolong the water evaporation time, solidify the dust particles, enhance the damage resistance of the dust samples and improve the dust suppression effect. After evaporating for 7h, the moisture content of the dust samples was still as high as 6.85%, the particle size of the samples with more than 40 meshes was 38.93%, and the dust suppression rate under the wind speed of 9m/s reached 96.40%. The dust suppression effect was much better than those dust samples sprayed with water, proving the starch-based dust inhibitor to be a green and environmentally friendly one.

Key words: mechanical activation solid phase method, grafted starch, polymers, preparation, evaporation resistance

中图分类号:

TQ314.2

杨家添, 唐金铭, 梁恣荣, 黎胤宏, 胡华宇, 陈渊. 新型淀粉基高吸水树脂抑尘剂的制备及其应用[J]. 化工进展, 2023, 42(6): 3187-3196.

YANG Jiatian, TANG Jinming, LIANG Zirong, LI Yinhong, HU Huayu, CHEN Yuan. Preparation and application of novel starch-based super absorbent polymer dust suppressant[J]. Chemical Industry and Engineering Progress, 2023, 42(6): 3187-3196.

图/表 17

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水平	因素
水平	反应温度 /℃	中和度 /%	淀粉与丙烯酸摩尔比	引发剂用量 /g	交联剂用量 /g
1	40	60	0.5∶1	0.6	0.03
2	50	70	0.75∶1	0.9	0.05
3	60	80	1∶1	1.2	0.07
4	70	90	1∶0.75	1.5	0.09

水平	因素
水平	反应温度 /℃	中和度 /%	淀粉与丙烯酸摩尔比	引发剂用量 /g	交联剂用量 /g
1	40	60	0.5∶1	0.6	0.03
2	50	70	0.75∶1	0.9	0.05
3	60	80	1∶1	1.2	0.07
4	70	90	1∶0.75	1.5	0.09

球磨时间（t_g） /h	单体转化率（α） /%	接枝率（G） /%	接枝效率（G_E） /%
1	36.46	21.26	68.47
2	56.64	29.56	70.69
3	96.81	42.35	81.36
4	85.42	38.76	78.26
5	69.51	33.99	74.21

球磨时间（t_g） /h	单体转化率（α） /%	接枝率（G） /%	接枝效率（G_E） /%
1	36.46	21.26	68.47
2	56.64	29.56	70.69
3	96.81	42.35	81.36
4	85.42	38.76	78.26
5	69.51	33.99	74.21

实验序号	反应温度/℃	中和度/%	淀粉与丙烯酸摩尔比	引发剂用量/g	交联剂用量/g	黏度/mPa·s	吸水率/g·g^-1
1	1(40)	1(60)	1(0.5∶1)	1(0.6)	1(0.03)	90	19.53
2	1(40)	2(70)	2(0.75∶1)	2(0.9)	2(0.05)	300	80.43
3	1(40)	3(80)	3(1∶1)	3(1.2)	3(0.07)	330	77.49
4	1(40)	4(90)	4(1∶0.75)	4(1.5)	4(0.09)	150	12.38
5	2(50)	1(60)	2(0.75∶1)	3(1.2)	4(0.09)	170	20.88
6	2(50)	2(70)	1(0.5∶1)	4(1.5)	3(0.07)	160	25.12
7	2(50)	3(80)	4(1∶0.75)	1(0.6)	2(0.05)	290	72.73
8	2(50)	4(90)	3(1∶1)	2(0.9)	1(0.03)	510	78.26
9	3(60)	1(60)	3(1∶1)	4(1.5)	2(0.05)	430	90.59
10	3(60)	2(70)	4(1∶0.75)	3(1.2)	1(0.03)	240	55.62
11	3(60)	3(80)	1(1∶1)	2(0.9)	4(0.09)	320	59.82
12	3(60)	4(90)	2(0.75∶1)	1(0.6)	3(0.07)	200	42.12
13	4(70)	1(60)	4(1∶0.75)	2(0.9)	3(0.07)	240	35.15
14	4(70)	2(70)	3(1∶1)	1(0.6)	4(0.09)	240	71.36
15	4(70)	3(80)	2(0.75∶1)	4(1.5)	1(0.03)	220	38.59
16	4(70)	4(90)	1(0.5∶1)	3(1.2)	2(0.05)	260	60.17
K₁	217.5	232.5	208	205	265	黏度极差分析
K₂	282.5	235	223	342.5	320
K₃	297.5	290	378	250	232.5
K₄	240	280	230	240	220
R₁	80	57.5	170	137.5	100
K₅	52.6775	41.5375	41.16	51.435	48	吸水率极差分析
K₆	49.2475	58.1325	45.505	63.415	75.98
K₇	62.0375	62.1575	79.425	53.54	44.97
K₈	51.3175	48.2325	43.97	41.67	41.11
R₂	12.79	20.62	38.265	21.745	34.87