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中文
Table of Content
30 October 2008, Volume 28 Issue 5
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研究报告
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Synthesis and Properties of Polyol from Hydrogenated Terpinene-maleic Ester Type Epoxy Resin Modified by Gallic Acid
WU Guo-min;KONG Zhen-wu;CHEN Jian;HUANG Huan
2008, 28 (
5
): 1-6.
Abstract
(
649
)
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(1232KB) (
442
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A new kind of polyol (HTME-GA polyol) was synthesized from hydrogenated terpinene-maleic ester type epoxy resin (HTME) modified by gallic acid (GA), and the suitable synthesis conditions were confirmed by studying the factors of synthesis reaction. HTME-GA polyol could be obtained by reacting GA with HTME at reflux temperature for about 3 hours in the solvent of
n
-propyl alcohol with the amount about 12.5 times of GA by molar weight and catalyst of quaternary ammonium salt with the amount about 2% of the reactants by weight. The chemical structure of HTME-GA polyol was characterized by chemical analysis, FT-IR and
13
C NMR spectral methods. HTME-GA polyol was crosslinked with two different curing agents, namely HN90T (HDI trimer) and EC385 (HDI trimer modified with polyether). It was shown that the crosslinked product of HTME-GA polyol with EC385 had better mechanical properties, and the crosslinked product of HTME-GA polyol with HN90T had better properties of resistance against liquids and higher hardness, while with poor flexibility. The increase of molar ratio of NCO/OH resulted in higher hardness and better liquid resistance of crosslinked product.
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Study on Chemical Compositions of
Eucommia ulmoides
Oliv. Inner Bark and Its Extractives
SI Chuan-ling;DENG Xiao-juan;WANG Dan;LIU Peng-tao;LIU Zhong
2008, 28 (
5
): 7-10.
Abstract
(
614
)
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(366KB) (
465
)
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Chemical compositions, including proximate composition, mineral, fatty acid and monosaccharide compositions of inner barks and extractives of the
Eucommia ulmoides
Oliv. were studied. Carbohydrate(92.97%)was the major constituent in proximate composition of
E. ulmoides
inner barks. The most quantitatively abundant constituents of fatty acid, mineral and [JP3]monosaccharide compositions were
α
-linolenic acid(27.4%), Ca(5.1769mg/g)and glucose(130.51mg/g), respectively. From the water soluble fraction of
E. ulmoide
inner barks, 5 compounds were isolated and their structures were elucidated as astragalin (1), isoquercetrin (2), quercetin-3-O-xyloglucoside (3), isochlorogenic acid A (4) and isochlorogenic acid C (5) by spectroscopic analyses and chemical evidence. Compounds 3-5 were isolated for the first time from this species.
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Study on Synthesis and Structure of Cellulose Acetate Propionate
DUAN Li-yan;JIN Li-wei;CAO Zhen-yan;XU Yu-zhi;WANG Chun-peng;CHU Fu-xiang
2008, 28 (
5
): 11-15.
Abstract
(
551
)
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Cellulose acetate propionate (CAP) was synthesized through heterogeneous esterification of cellulose. The substituting degree of CAP was determined by
13
C NMR and chemical titration. The structure and properties of CAP were investigated by IR, gel permeation chromatography (GPC), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The results showed that the crystallinity of CAP was decreased from 68% to 30%-40%, and the glass transition temperature was about 150℃. The plasticizing properties after esterification have been improved.
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Kinetics of Pectin Extraction from
Premna microphylla
Turcz. Leaves
WANG Cun-wen;XU Wen;WANG Wei-guo;ZHANG Jun-feng;WU Yuan-xin;CHI Ru-an
2008, 28 (
5
): 16-20.
Abstract
(
748
)
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522
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The kinetics of extracting pectin from
Premna microphylla
Turcz. leaves with acid-solution was studied. A kinetic model of pectin extraction is proposed taking account of impact of dissolved pectin molecule degradation. The maximum yield and optimal extraction time were determined using mathematical methods. It can be applied to describe extraction of pectin from
P. microphylla
leaves using hydrochloric acid at temperatures of 60,70,80 and 90℃ in laboratory. The rate constant of extraction was established to be varied from 3.01×10
-4
s
-1
at 60℃ to 8.64×10
-4
s
-1
at 90℃,while the maximum yield of 8.007% was obtained at 90℃ over a period of 50.19min. The theoretical results predicted with kinetic model were in good agreement with experimental data from
P.microphylla
leaves. The proposed theoretical model describes adequately the pectin extraction process in an acid medium, and provides an opportunity to predict the yield of pectin, the quantity of gradated pectin substances and the optimum duration of extraction.
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New Process for Isolation and Preparation of Isopimaric Acid
LI Xing-di;CHEN Yu-xiang;ZHAO Zhen-dong;BI Liang-wu;GU Yan;LI dong-mei;WANG Jing
2008, 28 (
5
): 21-25.
Abstract
(
694
)
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Taking advantage of the selectively crystalline specialty of 2-amino-2-methyl-1-propanol toward isopimaric acid, butanolidine isopimarate (2-amino-2-methyl-1-propanol isopimaric acid salt) was prepared by reacting 2-amino-2-methyl-1-propanol with thermally isomerized slash pine rosin that was freshly prepared from oleoresin or rosin, then purified by multi-recrystallization. Thereafter, isopimaric acid was isolated from the butanolidine isopimarate by acidic decomposition in a yield of 10.1% based on the rosin, with purity of 95.4% isopimaric acid. The isolation yield of isopimaric acid is 42.2% based on its content in rosin.
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Determination of Shikimic Acid Content in
Illicium verum
Hook.f. Using Near-infrared Spectroscopic Analysis Model Based on Partial Least-square Method
LU Jia-hui;GUO Wei-liang;YUE Bai-ling;WANG Di;MENG Qing-fan;TENG Li-rong
2008, 28 (
5
): 26-30.
Abstract
(
678
)
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571
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Partial least-square (PLS) method was applied to establish quantitative analysis model using near-infrared (NIR) spectra for determination of shikimic acid content in aniseed
(Illicium verum
Hook.f.). Various spectrometric pretreatment methods were used respectively for conversion of NIR spectra of aniseed powdered samples in order to remove the noise in spectra. The pretreated spectra were applied to develop PLS quantitative analysis model respectively. Each model was optimized by selecting the most efficacious spectrometric pretreatment method and the most suitable number of factors. The optimum model was selected depending on the root mean squares of calibration set calculated by cross-validation(RMSECV), the correlation coefficient of the values prediction by cross-validation method and actual values and the root mean squares of prediction set(RMSEP). The results demonstrated that the optimum model possessed good stability and high precision. This method has great prospect for quantitative analysis of Chinese traditional medicine.
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Studies on Anti-microbial Functions of Bamboo Charcoal and Nanometer-TiO
2
-modified Bamboo Charcoal
ZHOU Jian-bin;YE Han-ling;WEI Juan;FU Jin-he;ZHANG Qi-sheng
2008, 28 (
5
): 31-34.
Abstract
(
663
)
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513
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Nanometer-TiO
2
was used to modify granular and powdered bamboo charcoals respectively. These charcoals, together with bamboo charcoals of different carbonization temperatures (500, 600, 700, 800℃), were used in the anti-microbial experiments in the absence of light, and
Aspergillus niger
and
Trichoderma viride
were used as representative strains. The results showed that both nanometer-TiO
2
-modified bamboo charcoals (particles, powders) had the strongest anti-microbial functions, and the prevention efficacies (
E
) were 90% and 100% respectively. Bamboo charcoal of different carbonization tempertures had poor anti-microbial functions with
E
of 25%, 25%, 25% and 0 respectively. Nano-TiO
2
material did not have anti-microbial functions, and its
E
was 0. Nanometer-TiO
2
-modified bamboo charcoal was proved to be a new-style bamboo charcoal material which had strong anti-microbial functions than normal activated carbon.
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Study on Extraction of Rubusoside from
Rubus suavissimus
S. Lee by Macroporous Resins Adsorption
ZHOU Ru-jin;HUANG Min;ZHANG Ling;MA Yu-gang;LI Chun-hai
2008, 28 (
5
): 35-39.
Abstract
(
778
)
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557
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Adsorption of rubusoside from
Rubus suavissimus
S. Lee by 6 kinds of macroporous resins were tested to obtain the best adsorbent. Some of factors, not only on adsorption of rubusoside including the concentration of rubusoside, pH value and flow rate of solution, but also on desorption such as selection of desorbents and temperature, were investigated. The results showed that AB-8 resin was the best adsorbent for adsorption of rubusoside from
R.suavissimus
among 6 kinds of macroporous resins. The optimum conditions for adsorption by AB-8 resin were as follows: rubusoside solution concentration 7.7mg/L, pH value 8 and flow rate 3 BV/h. For desorption, ethanol solution showed good performance and temperature had obvious influence so both processes concerned were gained to complete desorption of rubusoside from adsorbent. One process can be operated under the conditions of 70% ethanol solution as desorbent, flow rate 3 BV/h(BV means the resin bed volume on chromatography column), total desorbent 5 BV at room temperature, or under the conditions of 60% ethanol solution as desorbent, flow rate 3 BV/h, total desorbent 4 BV at 40℃. Rubusoside was obtained successfully from
R. suavissimus
by this process in our laboratory.
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Synthesis and Characterization of Polymerized Rosin Epoxy Resin
HUANG Huo-yang;HA Cheng-yong;LI Yin-wen;SHEN Min-min
2008, 28 (
5
): 40-44.
Abstract
(
585
)
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768
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Polymerized rosin epoxy resin was synthesized by esterification and ring-closing reaction of polymerized rosin and epichlorohydrin. The product was identified by FT-IR and
1
H NMR spectrometries. The influencing factors of product properties were discussed emphatically. The suitable reaction conditions were as follows:mole ratio of polymerized rosin to epichlorohydrin 1:8,reaction temperature 75℃,reaction time 8h. The product had following properties:epoxy value 0.19mol/100g, viscosity (at 30℃) 30.8Pa·s, and acid value 0.2mg/g. This novel epoxy rosin had a rigid polycyclic structure, which would enrich the varieties of epoxy resin,widen the application range of rosin and increase the additional value of rosin.
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Kinetics of Pyrolysis and Metal-salt Catalized Pyrolysis of Wood
LIAO Yan-fen;MA Xiao-qian;SUN Yong-ming
2008, 28 (
5
): 45-50.
Abstract
(
607
)
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803
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According to thermogravimetric analysis under different heating rates, the kinetic characteristics of pyrolysis of Chinese fir wood catalyzed by potassium salt was studied. In response to the separation of DTG peaks and the activation energy under different conversion rate calculated by distribution activation energy model, it was found that potassium salt had catalytic effect on decomposition of hemi-cellulose at low temperature, and on the whole pyrolysis process of cellulose. Besides, it weakened or even eliminated the shoulder peak of DTG curves(200-270℃) and promoted dehydration and cross-linking reaction, which improved the char yield, and the ordering of residue carbon, which was represented by the increase of char yield from 16.3% to 25.3% and the abrupt increase of activation energy at the residue carbon decomposition stage after 80% conversion rate. Based on the three-component parallel-reaction mechanism, a non-lineal regression method was adopted to fit and calculate the kinetic parameters for pyrolysis of Chinese fir wood. Results showed that decomposition of cellulose could be regarded as first-order reaction. Potassium salt enhanced the pyrolysis of cellulose and hemi-cellulose, decreased their activation energy from 148.12 and 235.43 kJ/mol to 108.84 and 171.41 kJ/mol respectively, while the catalytic effect on lignin was insignificant.
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Research on Extraction of Anti-microbial Active Components from
Phyllostachys pubescens
Mazel ex H. de Lehaie Leaves
YAO Zhi-rui;CAO Guang-qun;YANG Cheng
2008, 28 (
5
): 51-54.
Abstract
(
583
)
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(709KB) (
611
)
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Extraction of active components from moso bamboo
(Phyllostachys pubescens
Mazel ex H. de Lehaie) leaves and their anti-microbial actives were studied. The minimum inhibitory concentration (MIC) of the active components from
P. pubescens
leaves against
Staphylococcus aureus
and
Escherichia coli
was determined by serial liquid dilution method. The results showed that anti-microbial effect of extracts from
P. pubescens
leaves against
S. aureus
and
E. coli
was optimum with the extraction condition: 60℃, 60% (volume fraction)ethanol, ratio of liquid to solid 20:1, 2h. The MIC of the extracts from
P. pubescens
leaves was 3.125g/L against
S. aureus
, and 6.25g/L against
E. coli
.
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Isolation and Identification of An Effective Actinomycete Strain for Degradating Rice Straw
XU Jie;YANG Qian
2008, 28 (
5
): 55-59.
Abstract
(
561
)
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587
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An actinomycete strain C-5, capable of degradating rice straw effectively, was isolated from soil which had been under the stock pile for several years, using methods of cellulose culture-medium selection and Congo red dyeing. The isolated strain was identified as
Streptomyces
sp. according to its phenotypic features and 16S rRNA phylogenetic analysis. This strain has enzymatic activities of cellulase, laccase, peroxidase, xylanase and pectinase simultaneously. After 30d of inoculating with C-5, the dry weigh of rice straw was decreased by 72%. C-5 could decompose rice straw effectively and had good application prospects in improving utilization of the rice straw resource.
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Study on Application of Coconut Shell-based Activated Carbon as Electrode Material and Adsorbent
WANG Yu-xin;SU Wei;LIU Cong-min;SHI Zhi-qiang;ZHOU Ya-ping
2008, 28 (
5
): 60-64.
Abstract
(
546
)
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(812KB) (
495
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Activated carbon with high specific surface area was prepared from coconut shell charcoal(CsAC), the structural properties of which were measured. The electrochemical performances of electric double-layer capacitor (EDLC) with CsAC as electrode material were investigated, including cyclic voltammetric and constant current charge/discharge properties. Results showed that EDLC had good charge/discharge performance and the specific capacitance of CsAC reached 164 F/g. Adsorption isotherms of NH
3
, CO
2
, CH
4
, N
2
, O
2
and H
2
on CsAC were measured at 298K. Considerable difference among the adsorption capacities toward different gases was observed and NH
3
was adsorbed much more than CO
2
, CH
4
, N
2
, O
2
and H
2
. According to adsorption amount ratio of two gases, it was concluded that CsAC was a very good adsorbent for the separation of NH
3
from its mixtures such as NH
3
/N
2
,NH
3
/O
2
and NH
3
/air. CsAC was also suitable for the separation of NH
3
from its mixture of CH
4
,as well as for the separation of CO
2
from its mixtures of O
2
or N
2
or both.
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Study on Microcapsulation Technology of Ginger Essential Oil
ZHANG Wei-ming;SHI Xue-ping;SUN Xiao-ming
2008, 28 (
5
): 65-69.
Abstract
(
567
)
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592
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Microcapsulation technology of ginger essential oil was studied. Arabic gum, maltodextrin and saybean protein were chosen as wall material. The optimum technology was obtained through three-factor single-shape gravity-center method. The technology of microcapsulation of ginger essential oil was as follows: the mass ratio of heart material,arabic gum,maltodextrin and soybean protein was 4:3:9:4, which account for 25% of the total emulsion, the condition of homogenization was:three times, 20MPa, 6min; 30MPa, 6min and 40MPa, 6min respectively, and air inlet temperature was 160℃.
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Study on Catalytic Thermochemical Liquefaction of Cornstalk
YAN Yong-bin;PANG Hao;YANG Xiao-xu;LIAO Bing
2008, 28 (
5
): 70-76.
Abstract
(
574
)
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(1304KB) (
607
)
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The liquefaction of cornstalk was conducted in polyhydric alcohols under different reaction conditions. The liquefied product was analyzed to investigate the change of its properties during liquefaction process and its components. The results indicated that the liquefaction efficiency was high in the mixed solvents of polyethylene glycol and glycerin (mass ratio 80:20), using sulfuric acid (mass fraction 3%) as catalyst. When liquid/solid mass ratio was 10:2, the residue content was only 8.1% after 180min. In the incipient reaction stage, lignin in cornstalk was liquefied wholly. With the prolongation of liquefaction, residue content decreased gradually, and hydroxyl value of liquefied product also decreased gradually from 375 to 330mg/g, and acid value increased gradually from 13 to 27mg/g;The molecular weight (
M
W
) was 1200-1450. By GC-MS analysis, the liquefied products contained oligomers of polyhydric alcohols,carboxylic acids and their esters because of oxidation and esterification of polyhydric alcohols and the decomposed cornstalk components.
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Study on Preparation of Starch-based Polyisocyanate Adhesives Using Composite-modified Starch
SHI Jun-you;;GU Ji-you;TU Huai-gang;WANG Shu-min
2008, 28 (
5
): 77-83.
Abstract
(
844
)
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(1188KB) (
617
)
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Preparations of Ⅰ,Ⅱ types starch-based aqueous polyisocyanate (API) adhesives using composite-modified corn starch are systemically studied. Using dosages of composite-modified starch emulsion, oxalic acid,polyvinyl alcohol(PVA), and polymeric MDI(PMDI) as main influencing factors, compressive, tensile and shearing strengths as evaluation target, formulation ofⅠtype starch-based API which meets index requirement of JISK 6806-1995 is optimized by orthogonal test and factors affecting physical and chemical properties of adhesive are analyzed systemically. Testified by validating test, the best optimized formulation has obvious operability of production. Cross-linking agent PMDI can be directly used without sealing, which meets completely the requirement for manufacture process of glued wood products.
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Studies on Correlations between Components of Essential Oil and Mass of Fresh Rhizome of
Atractylodes lancea
(Thunb.) DC. from Mt. Maoshan
WU Bao-cheng;WEI Yang-lian;GAO Xing;ZHAO Ya-mei;GU Zi-xia;HANG Yue-yu
2008, 28 (
5
): 84-88.
Abstract
(
584
)
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(804KB) (
460
)
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One hundred individuals of rhizomes of
Atractylodes lancea
(Thunb.)DC were collected from Mt. Maoshan and 4 essential oil components (atractylodin, atractylon, hinesol and
β
-eudesmol) were determined by GC. The correlations among the 4 essential oil components and between the rhizome mass were analyzed. Results showed that, under wild conditions, variation among masses of rhizomes, was large, but their masses were small generally, with only 7% individuals of rhizomes having mass more than 30 g. All rhizomes of
A. lancea
from Mt. Maoshan contained atractylodin which had the least variation, whereas,
β
-eudesmol was absent in 3% individuals of rhizomes, atractylon was absent in 7% of individuals and hinesol was absent in 50% of individuals. Atractylodin was the typical essential oil component in the rhizomes of wild
A. lancea
with high content. The rhizomes collected from Mt. Maoshan and other areas could be distinguished by the absence or presence of hinesol. The mass of rhizomes was positively correlated with atractylon. The correlation between atractylodin and atractylon was the highest,and the correlation between hinesol and
β
-eudesmol was also high, which explained the coordinated changes between atractylodin and atractylon, as well as between hinesol and
β
-eudesmol.
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Study on Antioxidant Effects of Polyphenols from Old Leaves of
Toona sinensis
(A. Juss) Roem
WANG Chang-lu;REN Lu;CHEN Zhi-qiang;JIANG Shen-hua;LIU Chang-jin;XIA Lian-fa
2008, 28 (
5
): 89-92.
Abstract
(
645
)
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(858KB) (
527
)
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Preliminary identification of polyphenols from old leaves of Chinese mahogany
(Toona sinensis
(A. Juss) Roem (TP)) had been made and four antioxidant testing methods, namely: reductive power measurement, ferric reducing ability of plasma (FRAP) method, DPPH radical scavenging activity measurement and
β
-carotene bleaching method, were tested respectively to study antioxidant ability of TP. Results of reductive power measurement and FRAP method showed that absorbances under wave length
λ
700 and 593 nm respectively of TP were higher than that of butylated hydroxy toluene(BHT) which proved that TP owned a stronger antioxidant ability. Results of DPPH radical scavenging ability measurement were all above 90%, as high as those of Vc. Result of
β
-carotene bleaching method indicated that TP showed an apparently dosage-dependent relationship and strong antioxidant ability.
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Interpretation on Degraded Products of Lignin during GIF Biomimetic Bleaching of Bamboo Pulp by GC-MS
JIA Yan-di;ZHOU Xue-fei;ZHU Zheng-liang
2008, 28 (
5
): 93-99.
Abstract
(
570
)
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(1117KB) (
477
)
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The degraded products of lignin were identified by gas chromatography-mass spectrometry (GC-MS) during GIF biomimetic bleaching of bamboo pulp to explore lignin degradation mechanism. The results showed that residual lignin was further degraded by GIF biomimetic system. The main ways of lignin degradation were involved with demethylation, formation and opening of quinone-type structures, cleavages of alkyl-aryl ether bond and carbon-carbon linkage in side-chain. The degraded products contained much carbonyl compounds, which was the result of catalytic oxidation in GIF biomimetic system. The pulp brightness was improved because of the removals of some quinone-type structures, conjugated carbonyl and phenolic compounds. Some carbohydrate-degraded products were also detected out by GC-MS.
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Preparation of Bleached Low-chlorine Shellac by Catalytic Hydrogenation and Its Structural Characterization
LIAO Ya-long;CHAI Xi-juan
2008, 28 (
5
): 100-104.
Abstract
(
574
)
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(872KB) (
640
)
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Bleached natural shellac with low chlorine content, which had been widely used in food industry and pharmacy, was prepared and characterized. The bleached natural shellac product with low chlorine content was prepared by means of catalytic hydrogenation of the bleached shellac in the presence of Ni-Fe binary-metal catalyst and hydrogen. Most of chlorine bonded to the double bond of terpenic acids of shellac and compacted in the molecule of shellac were eliminated by sodium hypochlorite bleaching under the conditions of Ni content 2.91%, catalyst quantity 8 g/L, H
2
flow rate 50 mL/min, and reaction temperature 90℃ for 240 min. Moreover, the mechanism of catalytic hydrogenation in preparation of the products was elucidated by the aid of structure characterization of the products through elementary analysis, infrared spectrometry, and ultraviolet spectrophotometry. It was demonstrated that chlorine content in the final product could reach 0.44% under optimum conditions, chlorine content in the final product was 1/5 of that before dechlorination by catalytic hydrogenation, and chlorine compacted in the molecule of shellac was substituted by hydrogen.
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Study on Determining the Antioxidant Activity of Betulin from Betula Bark
SUN Hong;ZHANG Ze;LIU Lin-yu
2008, 28 (
5
): 105-108.
Abstract
(
749
)
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(848KB) (
503
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A new method of determining the antioxidant activity of betulin from betula bark is established.In HCl-NaOAc(pH value 4.20) buffer solution, the hydroxyl free radical from Fenton reaction is captured by excess KI and the released I
3
-
combines with Rhodamine B(RhB
λ
max
=556nm) to form associated compound, so the absorbance at maximum wavelength decreases. The concentration of hydroxyl free radical(calculated by the concentration of hydrogen peroxide) is proportional to the decreased absorbance of the RhB system in the range of 0.14-0.68mg/L. Based on this fact, the antioxidatant activities of betulin and ascorbic acid are measured with satisfactory results.
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Research on Epoxidation of
α
-Pinene Catalyzed by Mn(Ⅱ) Sulfate Using H
2
O
2
as Oxidant
OUYANG Xiao-yue;JIANG Huan-feng
2008, 28 (
5
): 109-112.
Abstract
(
547
)
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(779KB) (
573
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A simple and practical procedure of epoxidation of
α
-pinene catalyzed by Mn
2+
sulfate together with NH
4
HCO
3
and CH
3
CN as co-catalysts, using 30% H
2
O
2
as oxidant is presented. The influences of the factors in the reaction were investigated. The optimum conditions are as follows: CH
3
CN 15mL, NH
4
HCO
3
2g,
tert
-BuOH 60mL, 30% H
2
O
2
40mL when 8mL
α
-pinene. Under such conditions after 48h reaction time, the conversion of
α
-pinene was completed, the yield of 2,3-epoxypinane was 81% (by GC analysis).
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Progress of Research on Antitumor and Antimicrobial Activities of Resin Acids and Their Derivatives
CHEN Yong;LIN Zhong-xiang
2008, 28 (
5
): 113-119.
Abstract
(
673
)
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(925KB) (
487
)
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Resin acids are the major components of rosin. This article gave a review on the structures and biological activities including antitumor, antivirus and antibacterial activities of resin acids and their derivatives including 52 compounds. The prospects of their future applications in the biomedicine and other areas were discussed.
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Applications of Plant Triglyceride Oil and Its Derivatives in the Field of Polymers
XU Li;SITU Yue;HU Jian-feng;ZENG Han-wei;CHEN Huan-qin
2008, 28 (
5
): 120-126.
Abstract
(
633
)
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481
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The investigation development and key points, synthesis methods and application prospects of natural triglyceride oil and its derivatives in the field of polymers are reviewed. The problems and development trend are pointed out when natural triglyceride oil and its derivatives are used in the field of polymers.
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