左旋海松酸的分离及其理化数据测试

doi:10.3969/j.issn.1673-5854.2019.06.008

Biomass Chemical Engineering ›› 2019, Vol. 53 ›› Issue (6): 45-50.doi: 10.3969/j.issn.1673-5854.2019.06.008

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Isolation and Physical-chemical Data Testing of Levopimaric Acid

Zhiwen QI^1,²(),Chengzhang WANG^1,*(),Jianxin JIANG²

1. Institute of Chemical Industry of Forest Products, CAF; National Engineering Lab. for Biomass Chemical Utilization; Key Lab. of Chemical Engineering of Forest Products, National Forestry and Grassland Administration; Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China
2. College of Materials Science and Technology, Beijing Forestry University, Beijing 100083, China

Received:2018-05-15 Online:2019-11-30 Published:2019-12-10
Contact: Chengzhang WANG E-mail:angelkissgod@163.com;wangczlhs@sina.com
Supported by:
国家自然科学基金资助项目(31570564);江苏省生物质能源与材料重点实验室基本科研业务费项目(JSBEM-S-201509)

Abstract

Abstract:

Levopimaric acid was isolated from turpentine by amination method and ultrasonic assisted recrystallization, and its physical and chemical data were experimental measured. By single factor and orthogonal test, the optimum isolation conditions of levopimaric acid were as follows:ethanol concentration 100%, crystallization temperature 0 ℃, volume ratio of ethanol used for crystallization 20 : 1(mL : g), ultrasonic frequency was 53 kHz, 2 recrystallization times; purity of levopimaric acid was 97%. Ultrasonic assisted crystallization was used to shorten the nucleation time of the levopimaric acid crystal, and a fine-uniform rectangular transparent crystal was obtained after 5-6 h. The molecular structure of levopimaric acid was characterized by FT-IR, NMR(¹H NMR, ¹³C NMR) and GC-MS. According to the oxygen elastic calorimeter, TG-DSC and group contribution, the standard molar enthalpy(Δ_fH_m^?) and melting enthalpy of levopimaric acid were -700.23 and 94.99 kJ/mol, respectively.

Key words: levopimaric acid, isolation, ultrasonic, enthalpy change

CLC Number:

TQ35

Zhiwen QI,Chengzhang WANG,Jianxin JIANG. Isolation and Physical-chemical Data Testing of Levopimaric Acid[J]. Biomass Chemical Engineering, 2019, 53(6): 45-50.

Figures/Tables 6

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Table 1

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Table 2

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References 12

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编号 No.	A 结晶温度/℃ crystallization temperature	B 乙醇质量分数/% EtOH	C 乙醇用量/mL dosage of ethanol	D 超声波频率/kHz ultrasonic frequency	纯度/% purity
1	2	85	40	45	75.27
2	2	95	20	28	87.94
3	2	100	30	53	91.05
4	0	85	20	53	87.41
5	0	95	30	45	85.34
6	0	100	40	28	90.02
7	8	85	30	28	79.36
8	8	95	40	53	86.52
9	8	100	20	45	87.34
k₁	84.75	80.68	83.94	82.65
k₂	87.59	86.60	87.56	85.77
k₃	84.41	89.47	85.25	88.33
R	3.18	8.79	3.62	5.68

序号 No.	质量/mg mass	外部能量/J out energy	点火能量/J ignite energy	燃烧热量/J burn energy	C_V/ (J·K^-1)
1	910	50	70	42562	10500
2	927	50	70	43209	10500
3	930	50	70	43356	10500

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Isolation and Physical-chemical Data Testing of Levopimaric Acid

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