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GB/T 30044-2013: Coal direct liquefaction -- Determination of constituents of heavy products -- Solvent extract
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Coal direct liquefaction -- Determination of constituents of heavy products -- Solvent extract
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GB/T 30044-2013
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Basic data | Standard ID | GB/T 30044-2013 (GB/T30044-2013) | | Description (Translated English) | Coal direct liquefaction -- Determination of constituents of heavy products -- Solvent extract | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | D21 | | Classification of International Standard | 73.040 | | Word Count Estimation | 9,970 | | Quoted Standard | GB/T 23251 | | Regulation (derived from) | National Standards Bulletin No. 25 of 2013 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This standard specifies the terms and definitions of direct coal liquefaction heavy product component analysis method feeds, reagents and materials, equipment, measurement procedure, the results of the calculation precision of the method and test reports. | GB/T 30044-2013: Coal direct liquefaction -- Determination of constituents of heavy products -- Solvent extract
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Coal direct liquefaction. Determination of constituents of heavy products. Solvent extract
ICS 73.040
D21
National Standards of People's Republic of China
Direct coal liquefaction liquefaction heavy product component analysis
Solvent Extraction
Solventextract
Issued on. 2013-12-17
2014-05-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
This standard was drafted in accordance with GB/T 1.1-2009 given rules.
The standard proposed by China Coal Industry Association.
This standard coal by the National Standardization Technical Committee (SAC/TC42) centralized.
This standard was drafted. Coal Research Institute Beijing Coal Chemical Research Branch.
The main drafters of this standard. Valley little while, Li Peilin, Zhong Jinlong, Mao Xuefeng, Zhang Xiaojing, Dushu Feng, Wu Yan, Inspiration from Hu Fating.
Direct coal liquefaction liquefaction heavy product component analysis
Solvent Extraction
1 Scope
This standard specifies the terms and definitions of direct coal liquefaction heavy product component analysis method feeds, reagents and materials, equipment, measuring
Set step, the results of the calculation, method precision and test reports.
This standard applies to direct coal liquefaction heavy product components analysis.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 23251 coal chemical coal Technical Guidelines
3 Terms and Definitions
GB/T 23251 define the terms and definitions section and the following terms and definitions apply to this document.
3.1
Direct coal liquefaction coaldirectliquefaction
Coal under the action of high pressure, high temperature and the hydrogenation reaction catalyst with hydrogen, whereby liquid fuel directly into the process.
[GB/T 23251-2009, the definition 3.8]
3.2
Heavy product heavyproduct
For other liquefied under the direct coal liquefaction of solid residues generated or at room temperature.
3.3
Liquefied oil liquefiedoil
Direct coal liquefaction product n-hexane-soluble components.
3.4
Asphaltene asphaltene
Direct coal liquefaction products of n-hexane-insoluble and soluble components of toluene.
3.5
Before asphaltene preasphaltene
Direct coal liquefaction product in a toluene-insoluble and soluble components of tetrahydrofuran.
4 Method summary
The sample size of less than 0.2mm is placed in the filter cartridge using hexane extraction, n-hexane insoluble matter was dried to a constant mass-based dry
Quality insolubles after drying to calculate the mass fraction of n-hexane insolubles. In the same way, the n-hexane insoluble matter was extracted with toluene
Take, measuring the mass fraction of a toluene-insoluble matter. Similarly, the particle size of less than 0.2mm specimen was placed a filter paper tube and extracted with tetrahydrofuran, the
6.7.1 Soxhlet extractor. diameter 45mm ~ 55mm.
6.7.2 flat-bottomed flask. 500mL, bottle diameter 28mm ~ 30mm.
6.7.3 Condenser. spherical end mill with port and extractor, and with two symmetrical holes, water jacket length of at least 300mm.
7 analytical sample preparation
The heavy coal liquefaction product samples crushed to less than 3mm, reduced separation of about 50g, ground to less than 0.2mm as a sample for analysis,
spare.
8 measuring step
8.1 Determination of n-hexane insolubles
8.1.1 weighed sample
0.5g of cotton, divided into two approximately equal parts, put in filter cartridge made funnel-shaped, the other part is placed a filter paper
The upper portion of the cylinder, and then the filter cartridge into the weighing bottle, in a blast in the oven at 100 ℃ ~ 105 ℃ drying to constant mass (for two consecutive
Poor quality of the drying times of no more than 0.0020g), record the mass (m1). Weigh a sample for analysis (1 ± 0.1) g (m), accurate to 0.0002g, from
Remove the upper part of the filter cartridge cotton, the sample was placed in the filter cartridge, and then placed on top cotton filter cartridge.
8.1.2 pre-dispersed sample
The sample is weighed into a paper cylinder containing n-hexane lidded jar, bottle hexane height above the filter drum samples
Height, capped the jar into an ultrasonic oscillator, shaking at 55 ℃ at least 30min.
8.1.3 Sample extraction
The filter cartridge moved Soxhlet extractor, a jar of n-hexane solvent into the flat-bottomed flask, added in the flask solvent amount of solvent
2/3 of the volume of the flask, and the extract is placed in a preheated oil bath at a constant temperature, according to Figure 1 shown installed Soxhlet extraction apparatus. Open cooling water control
Oil bath temperature to about reflux hexane solvent 6min average time until the filter cartridge leaking nearly colorless solvent, extraction time is not usually
Less than 48h.
8.1.4 Drying constant weight
After extraction stop oil bath was heated until the oil bath was removed after cooling extractor, remove the filter paper tube, placed in a beaker, in a fume hood to be positive
After the hexane solvent play to make, weighing bottle into the weighing bottle placed in a vacuum oven at 100 ℃ ~ 105 ℃ dried for at least 3h, remove the weighing
Bottles and cover caps, placed in a desiccator to cool to room temperature and weighed. Then check Sjogren, every 1h, until the last two weighing result
If the difference does not exceed 0.0020g, quality as the basis for the final weighing (m2) result of the calculation.
8.2 Determination of toluene insolubles
8.2.1 pre-dispersed sample
The hexane insolubles were placed in cylindrical filter paper containing toluene lidded jar, to be higher than the height of the bottle toluene high sample cartridge filter
Degrees, capped the jar into an ultrasonic oscillator, shaking at 55 ℃ at least 30min.
8.2.2 toluene extraction
The filters were transferred to soxhlet tube, the toluene solvent was poured into the jar Florence flask, the flask was added the amount of solvent is the solvent
2/3 of the volume of the flask, and the extract is placed in a preheated oil bath at a constant temperature, as shown in Figure 1 installed good Soxhlet extraction apparatus. Open cooling water control
Oil bath temperature solvent such as toluene reflux average 6min around again until the filter cartridge leaking solvent nearly colorless, usually extracted a lot of time
In 24h.
8.2.3 Drying constant weight
After extraction stop oil bath was heated until the oil bath was removed after cooling extractor, remove the filter paper tube, placed in a beaker, in a fume hood to be A
Benzene play to make, weighing bottle into the weighing bottle placed in a vacuum oven at 100 ℃ ~ 105 ℃ dried for at least 3h, dried or placed blast
Box, at 110 ℃ ~ 115 ℃ dried for at least 2h, remove the weighing bottle and cover caps, placed in a desiccator to cool to room temperature and weighed. then
Sjogren check every 30min, until the difference between the results of the last two weighing not more than 0.0020g, in order to quality for the last weighing
Basis (m3) as a result of the calculation.
8.3 Determination of THF insolubles
8.3.1 Sample Weighing
0.5g of cotton, divided into two approximately equal parts, put in filter cartridge made funnel-shaped, the other part is placed a filter paper
The upper portion of the cylinder, and then the filter cartridge into the weighing bottle, in a blast in the oven at 100 ℃ ~ 105 ℃ drying to constant mass (for two consecutive
Poor quality of the drying times of no more than 0.0020g), the recording quality (m4). Weigh a sample for analysis (1 ± 0.1) g (m5), accurate to 0.0002g, from
Remove the upper part of the filter cartridge cotton, the sample was placed in the filter cartridge, and then placed on top cotton filter cartridge.
8.3.2 pre-dispersed sample
The paper said that a good sample tube containing tetrahydrofuran into the jar lid, to be more than the height of the bottle tetrahydrofuran filter cartridge like
Height goods, capped the jar into an ultrasonic oscillator, shaking at 55 ℃ at least 30min.
8.3.3 Extraction
The filter cartridge soxhlet moved, the tetrahydrofuran solvent was poured into the jar Florence flask, the flask was added the solvent and the solvent
An amount of 2/3 volume flask, the extractor is placed in a constant temperature oil bath preheated, according to Figure 1 shown installed Soxhlet extraction apparatus. Open cooling water,
Controlled oil bath temperature to about reflux tetrahydrofuran solvent 6min average time until the filter cartridge leaking solvent nearly colorless, usually extracted when
Room is 4h ~ 8h.
8.3.4 Drying constant weight
After stopping the extraction of oil bath was heated until the oil bath was removed after cooling extractor, remove the filter paper tube, beaker, in a fume hood, to be
After the tetrahydrofuran solvent play to make, into a weighing bottle. The weighing bottle is placed in a vacuum oven at 100 ℃ ~ 105 ℃ dried for at least 3h, remove
Weighing bottle and cover caps, placed in a desiccator to cool to room temperature and weighed. Then check Sjogren, every 1h, until the last two, said
The amount does not exceed the difference between the results of 0.0020g, quality as the basis for the final weighing (m6) result of the calculation.
9 result of the calculation
9.1 Calculation of heavy oil in the liquefied product
9.1.1 n-hexane insolubles content HI according to formula (1).
HI =
m2-m1
m × 100%
(1)
Where.
HI --- sample of n-hexane insolubles content (%);
m2 --- weighing bottle, the quality of the filter cartridge, cotton and n-hexane insolubles and units of grams (g);
m1 --- weighing bottle, the quality of the filter cartridge and cotton and, in grams (g);
M --- the quality of the sample, in grams (g).
(2) 9.1.2 calculate the mass fraction of heavy products X0 liquefied oil by the formula.
X0 = 100-HI (2)
Where.
X0 --- heavy products in mass fraction (%) of liquefied oil.
9.2 asphaltenes heavy products Calculation
9.2.1 toluene insolubles content of TI according to equation (3) Calculated.
TI =
m3-m1
m × 100%
(3)
Where.
TI --- sample mass fraction of toluene insolubles (%);
Quality of m3 --- weighing bottle, filter cartridges, cotton and toluene insolubles and units of grams (g).
9.2.2 heavy products in asphaltene content Xasp according to formula (4) Calculated.
Xasp = HI-TI (4)
Where.
Xasp --- heavy products in asphaltene content (%).
9.3 product before heavy asphaltenes computing
9.3.1 THF insolubles content of THFI according to formula (5) Calculated.
THFI =
m6-m4
m5
× 100% (5)
Where.
--- THFI sample tetrahydrofuran-insoluble fraction of the mass (%);
Quality of m6 --- weighing bottle, paper tubes, cotton wool and tetrahydrofuran-insoluble and, in grams (g);
m4 --- weighing bottle, the quality of the filter cartridge and cotton and, in grams (g);
m5 --- sample mass, in grams (g).
9.3.2 heavy product before asphaltene content Xpreasp according to equation (6) Calculated.
Xpreasp = TI-THFI (6)
Where.
Xpreasp --- heavy products in mass fraction (%) before asphaltenes.
10 precision of the method
10.1 Repeatability limit
The absolute difference between two independent test results obtained under repeatability conditions at the 95% confidence level should not exceed specified in Table 1.
10.2 reproducibility limit
The absolute difference between two independent test results obtained under reproducibility conditions at 95% confidence level should not exceed specified in Table 1.
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