响应面法优化羟丙基壳聚糖的合成工艺

doi:10.3969/j.issn.1673-5854.2019.01.004

Abstract

Abstract:

Hydroxypropyl chitosan(HPCS) was synthesized from chitosan(CTS) and propylene oxide. The structure and morphology of HPCS were characterized by infrared spectroscopy(FT-IR), ¹H nuclear magnetic resonance(¹H NMR), X-ray diffraction(XRD) and environmental scanning electron microscopy(ESEM). And the effects of the synthesis process on the intrinsic viscosity were investigated. The results showed that the hydroxypropyl group was successfully grafted onto chitosan and HPCS was obtained. On the basis of single factor experiment, the response surface methodology was used to optimize the process. The optimum conditions for HPCS synthesis were reaction temperature 60 ℃, reaction time 6 h, NaOH mass fraction 30%, alkalization time 20 min and the amount of propylene oxide 12.6 g. Under these conditions, the intrinsic viscosity of HPCS was 206.32 mL/g, the relative molecular mass was 2.738×10⁵, and the degree of substitution(D_S)was 0.426.

Key words: hydroxypropyl chitosan, response surface optimization, intrinsic viscosity

CLC Number:

TQ35
O636

Rui GUO,Yao ZHANG,Shuang HAN,Ning WANG. Response Surface Optimization of Hydroxypropyl Chitosan Synthesis[J]. Biomass Chemical Engineering, 2019, 53(1): 25-32.

Figures/Tables 8

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References 21

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方差来源 variance source	平方和 sum of squares	自由度 free degree	均方 mean square	F值 F value	P值 P value	显著性 significance
模型model	1688.14	9	187.57	86.81	< 0.0001	*
X₁	44.13	1	44.13	20.42	0.0027	*
X₂	23.22	1	23.22	10.75	0.0135	*
X₃	108.19	1	108.19	50.07	0.0002	*
X₁X₂	11.32	1	11.32	5.24	0.0559
X₁X₃	20.25	1	20.25	9.37	0.0183	*
X₂X₃	6.92	1	6.92	3.20	0.1167
X₁²	829.72	1	829.72	383.99	< 0.0001	*
X₂²	476.92	1	476.92	220.71	< 0.0001	*
X₃²	49.40	1	49.40	22.86	0.0020	*
残差residual	15.13	7	2.16
失拟项lack of fit	12.17	3	4.06	5.49	0.0667
误差error	2.96	4	0.74
总变异total variation	1703.27	16

Response Surface Optimization of Hydroxypropyl Chitosan Synthesis

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编号 No.	X₁ NaOH质量分数/% mass fraction of NaOH	X₂ 碱化时间/min alkalization time	X₃ 环氧丙烷用量/g amount of propylene oxide	Y 特性黏数/(mL·g^-1) intrinsic viscosity
1	30	20	12	205.89
2	32	20	11	184.71
3	32	20	13	185.23
4	30	25	11	188.55
5	32	25	12	178.28
6	30	20	12	203.92
7	30	20	12	204.12
8	30	25	13	195.61
9	28	20	11	185.02
10	32	15	12	177.45
11	30	15	13	195.62
12	30	20	12	205.53
13	28	25	12	186.23
14	28	15	12	178.67
15	28	20	13	194.54
16	30	15	11	183.30
17	30	20	12	204.73