CN102476041B - Activated carbon adsorption wire and preparation method and application method thereof - Google Patents
Activated carbon adsorption wire and preparation method and application method thereof Download PDFInfo
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Abstract
The invention discloses an activated carbon adsorption wire and a preparation method and an application method thereof. The preparation method of the activated carbon adsorption wire includes steps of (1) mixing water with sodium silicate according to the weight ratio of (1-5) : (0.1-3) to prepare an inorganic binder; (2) grinding activated carbon until the particle size thereof is lower than 80 meshes, mixing the ground activated carbon with the inorganic binder which is prepared in the step (1) according to the weight ratio of (3-7) : (6-10) while stirring the mixture uniformly to prepare a mixed colloidal solution; (3) impregnating polished metal wires into the mixed colloidal solution prepared from the step (2), taking the impregnated metal wires out and then drying the same naturally; and (4), purifying the metal wires in vacuum and then storing the same hermetically. The activated carbon adsorption wire prepared by the preparation method is not easy to slip off, is uniform in adsorption capacity, and accordingly accuracy of data analysis is improved and accurately quantitative analysis of the technology of the adsorption wire is realized.
Description
Technical field
The present invention relates to oil and gas geochemistry exploration technique field, say further, relate to a kind of charcoal absorption silk, preparation method and using method.
Background technology
C
5-C
21Hydrocarbons is that oil and gas geochemistry is reconnoitred (hydrocarbon geochemical exploration, the important content of studying in the career field down together), because it is very little that such material is reconnoitred in the sample content at oil and gas geochemistry, therefore the general Instrumental Analysis detectability that all is lower than routine must carry out the enrichment preliminary treatment to the component to be measured in the sample.The adsorption filament method namely is to take the principle of adsorption and enrichment, earlier target hydrocarbon component to be measured is accumulated adsorption and enrichment, and then the method for resolving by heating again discharges adsorbed component, and then carries out instrument again and detect.
The preparation method of charcoal absorption silk is the key link of this analytical technology, and different throwing methods are directly connected to the accuracy of testing result to all multifactor generation considerable influences such as enrichment adsorption effects.Existing adsorption filament technology of preparing: coat inorganic silicic acid sodium adhesive at wire one end, insert in the activated carbon powder again, taking-up is dried, and sealing is preserved stand-by after high temperature, the vacuum purification.There are the following problems for prior art: 1, Tu Fu activated carbon powder is inhomogeneous; 2, dry, activated carbon powder is easy to come off in purification, absorption and the resolving; 3, charcoal absorption dosage differs greatly on the silk, causes the error of analysis result bigger, is difficult for carrying out quantitative analysis.
Summary of the invention
For solving the problem that active carbon easily comes off, quantity of sorbent differs greatly that exists in the prior art, the invention provides a kind of charcoal absorption silk, preparation method and application, make charcoal absorption silk technology realize accurate quantitative analysis, thereby promote the effect that the adsorption filament technology is reconnoitred at oil and gas geochemistry.
One of purpose of the present invention provides a kind of charcoal absorption silk, prepares according to the following steps:
(1) water and sodium metasilicate are mixed with inorganic bond, and the weight ratio of water and sodium metasilicate is (1～5): (0.1～3); Be preferably: (2～4): (1～3)
(2) active carbon is ground to below 80 orders, and the inorganic bond that makes with step (1) is by weight (3～7): (6～10) are preferably (4～6): (7～9) stir and make mixed colloidal solution;
(3) wire immerses after polishing in the mixed colloidal solution that step (2) makes, and takes out natural air drying after leaving standstill 5-20s;
(4) vacuum purification, sealing is preserved.
The preferred iron wire of wire or nickel wire described in the step (3), the wire length that enters in the mixed colloidal solution is 0.5-3cm.
Two of purpose of the present invention provides a kind of preparation method of charcoal absorption silk.
Comprise following steps:
(1) water and sodium metasilicate are mixed with inorganic bond by described weight ratio;
(2) after active carbon ground, the inorganic bond that makes with step (1) stirred by described weight ratio and makes mixed colloidal solution;
(3) wire immerses after polishing in the mixed colloidal solution that step (2) makes, and takes out natural air drying;
(4) vacuum purification, sealing is preserved
The vacuum purification temperature is 180-300 ℃ in the described step (4), is preferably 250 ℃, vacuum is-and 0.05MPa～-0.1MPa, the clarification time is 1～5h.
Concrete operations can be undertaken by following scheme:
The adsorbent prescription: the used inorganic bond employing water of the present invention and sodium metasilicate are formulated by 3: 1 weight ratios.After active carbon is ground to-120 orders, stir and evenly mix into mixed colloidal solution according to 5: 8 part by weight with inorganic bond.
Throwing method (see figure 1): it is that 8-10cm common metal silk 102 (iron wire or nickel wire) is carrier that the present invention adopts length, after one end is rough through sand papering, immerse in the active carbon and inorganic bond mixed colloidal solution of (1cm length) prior mixing, make its surface evenly be coated with the above-mentioned colloidal solution of last layer, natural air drying after the taking-up.
The purifier (see figure 2): the charcoal absorption silk behind the natural wind is positioned in the closed container purified treatment under 250 ℃ of following vacuum conditions, and sealing is preserved stand-by then.
Can adopt following operation: open plug 201, the charcoal absorption silk 205 that makes is put into purification bottle 202, build plug 201, put into the hole of pot arch 206 purifying bottle, open two-port valve 203, open vavuum pump 204, purified treatment 4h to 250 ℃ of following vacuum conditions heats, close two-port valve 203, pot arch 206, vavuum pump 204, sealing is preserved stand-by.
Three of purpose of the present invention provides the application of charcoal absorption silk, adopts one of following two kinds of methods:
A) absorption of solid sample
The solid sample (breaking into pieces to particle diameter 0.5cm) of packing in port grinding bottle is inserted in the sample purifying the back adsorption filament, covers the ground bottle stopper, puts into baking oven, dries by the fire 16～48 hours the C in the sample bottle under 40-60 ℃ of condition
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment;
Concrete steps are as follows:
The solid sample 301 (breaking into pieces to particle diameter 0.5cm) of packing in dress sample bottle 302 is inserted in the sample purifying back charcoal absorption silk, covers sealing bottle cork 304, puts into baking oven, dries by the fire 24 hours the C in the sample under 60 ℃ of conditions
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment.
B) absorption of fluid sample
The fluid sample of packing in the fluid sample air-tight bottle, certain space is left on top, adsorption filament is not coated with the adsorbent end is fixed on the bottle stopper, makes to be coated with the adsorbent end and to be placed on the fluid sample upper space, 40-60 ℃ of following adsorption and enrichment 16～48h of water-bath heating.
Concrete steps are as follows:
The certain quantity of fluid sample 404 of in fluid sample air-tight bottle 402, packing into, certain space is left on top, the charcoal absorption silk is not coated with the adsorbent end to be fixed on the sealing plug 401, make the charcoal absorption silk be coated with the adsorbent end and be placed on the fluid sample upper space, 40-60 ℃ of following adsorption and enrichment 24h of water-bath heating, the C in the fluid sample
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment.
Analyze: open bottle stopper, take out adsorption filament, cut the silk (0.5cm) that is coated with the adsorbent end, cut thread put into heat cracker or Curie point pyrolyzer carries out desorb, and feeding gas chromatograph or gas chromatograph-mass spectrometer (GC-MS) carry out C
5-C
21Hydrocarbons is analyzed.
The no stripping of charcoal absorption silk of the present invention itself and volatilization organic component can not impact test result.
Active carbon grinds the back and is mixed into mixed colloidal solution with inorganic bond, uniformity and the uniformity of adsorption filament activated carbon coating have been guaranteed, also eliminated adsorption filament active carbon obscission in use, the present invention has simultaneously adopted the purification method under the high-temperature vacuum condition in the closed container, make to purify and preserve integrated, reduce the pollution that intermediate link may cause adsorption filament, improved the accuracy of analyzing data, realized the accurate quantitative analysis of adsorption filament technology.
Description of drawings
Fig. 1 charcoal absorption silk structural representation
Fig. 2 charcoal absorption silk vacuum purifier structural representation of heating
The solid sample adsorbent equipment structural representation of Fig. 3 charcoal absorption silk
The fluid sample adsorbent equipment structural representation of Fig. 4 charcoal absorption silk
Fig. 5 the present invention does the gas chromatograph-mass spectrometer (GC-MS) of the Daqing oil field water sample yiy-20 of active carbon adsorption filament analysis and analyzes chromatogram
Description of reference numerals
The even mixed colloidal solution of 101 inorganic bonds and active carbon, 102 wires
201 plugs, 202 purify bottle, 203 two-port valves, 204 vavuum pumps, 205 charcoal absorption silks, 206 pot arches
301 solid samples, 302 dress sample bottles, 304 sealing bottle corks;
401 are sealing plug, 402 fluid sample air-tight bottles, 404 fluid samples
The specific embodiment
Below in conjunction with embodiment, further specify the present invention.
Used raw material among the embodiment:
Sodium metasilicate, Shanghai reagent company
Active carbon, Guangzhou Chemical Reagent Factory
Embodiment 1
Adsorbent prescription: formulated by 3: 1 weight ratios with inorganic bond employing water and sodium metasilicate.After active carbon is ground to-120 orders, stir and evenly mix into mixed colloidal solution according to 5: 8 part by weight with inorganic bond.
Throwing method (see figure 1): be that 8cm nickel wire 102 is carrier with length, after one end is rough through sand papering, immerse in the active carbon and inorganic bond mixed colloidal solution of (1cm length) prior mixing, make its surface evenly be coated with the above-mentioned colloidal solution of last layer, natural air drying after the taking-up.
The purifier (see figure 2): the charcoal absorption silk behind the natural air drying is positioned in the closed container purified treatment under 250 ℃ of following vacuum conditions, and sealing is preserved stand-by then.
Sample absorption (see figure 3): the 200g South Yellow Sea sea-bottom deposit matter sample (breaking into pieces to particle diameter 0.5cm) of in port grinding bottle, packing into, be inserted in the sample purifying the back adsorption filament, cover the ground bottle stopper, put into baking oven, baking is 24 hours under 60 ℃ of conditions, the C in the sample bottle
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment;
Analyze: open bottle stopper, take out adsorption filament, cut the silk (0.5cm) that is coated with the adsorbent end, the silk of cutting is put into heat cracker carry out desorb, and the feeding gas chromatograph-mass spectrometer (GC-MS) carries out C
5-C
21Hydrocarbons is analyzed.Analysis result sees Table 2
Embodiment 2
The adsorbent prescription: the used inorganic bond employing water of the present invention and sodium metasilicate are formulated by 3: 1 weight ratios.After active carbon is ground to-120 orders, stir and evenly mix into mixed colloidal solution according to 5: 8 part by weight with inorganic bond.
Throwing method (see figure 1): be that 8cm nickel wire 102 is carrier with length, after one end is rough through sand papering, immerse in the active carbon and inorganic bond mixed colloidal solution of (1cm length) prior mixing, make its surface evenly be coated with the above-mentioned colloidal solution of last layer, natural air drying after the taking-up.
The purifier (see figure 2): the charcoal absorption silk behind the natural air drying is positioned in the closed container purified treatment under 250 ℃ of following vacuum conditions, and sealing is preserved stand-by then.
Adsorbent equipment: fluid sample absorption (see figure 4): the 500mL fluid sample of in the fluid sample air-tight bottle, packing into, the 8cm height space is left on top, adsorption filament is not coated with the adsorbent end to be fixed on the bottle stopper, make to be coated with the adsorbent end and to be placed on the fluid sample upper space 60 ℃ of following adsorption and enrichment 24h of water-bath heating.
Analyze: open bottle stopper, take out adsorption filament, cut the silk (0.5cm) that is coated with the adsorbent end, the silk of cutting is put into heat cracker carry out desorb, and the feeding gas chromatograph-mass spectrometer (GC-MS) carries out C
5-C
21Hydrocarbons is analyzed.
Fig. 5 is that the gas chromatograph-mass spectrometer (GC-MS) that utilizes the present invention to be the Daqing oil field water sample yiy-20 of active carbon adsorption filament analysis is analyzed chromatogram, table 2 is the hydrocarbons content that charcoal absorption silk method detects Daqing oil field water sample yiy-20, has obtained good effect.
Embodiment 3～7
Adsorbent prescription: it is formulated that inorganic bond adopts water and sodium metasilicate weight ratio to be respectively 1: 0.1,1: 3,3: 1,5: 0.1,5: 3.After active carbon is ground to-120 orders, stir and evenly mix into mixed colloidal solution according to 5: 8 part by weight with inorganic bond.
Throwing method (see figure 1): be that 8cm nickel wire 102 is carrier with length, after one end is rough through sand papering, immerse in the active carbon and inorganic bond mixed colloidal solution of (1cm length) prior mixing, make its surface evenly be coated with the above-mentioned colloidal solution of last layer, natural air drying after the taking-up.
The purifier (see figure 2): the charcoal absorption silk behind the natural air drying is positioned in the closed container purified treatment under 250 ℃ of following vacuum conditions, and sealing is preserved stand-by then.
Sample absorption (see figure 3): the 200g South Yellow Sea seabed A1 sediment sample (breaking into pieces to particle diameter 0.5cm) of in port grinding bottle, packing into, be inserted in the sample purifying the back adsorption filament, cover the ground bottle stopper, put into baking oven, baking is 24 hours under 60 ℃ of conditions, the C in the sample bottle
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment;
Analyze: open bottle stopper, take out adsorption filament, cut the silk (0.5cm) that is coated with the adsorbent end, the silk of cutting is put into heat cracker carry out desorb, and the feeding gas chromatograph-mass spectrometer (GC-MS) carries out C
5-C
21Hydrocarbons is analyzed.Analysis result sees Table 3.
Embodiment 8～12
The adsorbent prescription: inorganic bond employing water and sodium metasilicate are formulated by 3: 1 weight ratios.Active carbon stirs and evenly mixs into mixed colloidal solution according to 5: 8 part by weight with inorganic bond after being ground to-80 ,-100 ,-120 ,-140 ,-160 orders respectively.
Throwing method (see figure 1): be that 8cm nickel wire 102 is carrier with length, after one end is rough through sand papering, immerse in the active carbon and inorganic bond mixed colloidal solution of (1cm length) prior mixing, make its surface evenly be coated with the above-mentioned colloidal solution of last layer, natural air drying after the taking-up.
The purifier (see figure 2): the charcoal absorption silk behind the natural air drying is positioned in the closed container purified treatment under 250 ℃ of following vacuum conditions, and sealing is preserved stand-by then.
Sample absorption (see figure 3): the 200g South Yellow Sea seabed A2 sediment sample (breaking into pieces to particle diameter 0.5cm) of in port grinding bottle, packing into, be inserted in the sample purifying the back adsorption filament, cover the ground bottle stopper, put into baking oven, baking is 24 hours under 60 ℃ of conditions, the C in the sample bottle
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment;
Analyze: open bottle stopper, take out adsorption filament, cut the silk (0.5cm) that is coated with the adsorbent end, the silk of cutting is put into heat cracker carry out desorb, and the feeding gas chromatograph-mass spectrometer (GC-MS) carries out C
5-C
21Hydrocarbons is analyzed.Analysis result sees Table 4.
Embodiment 13～17
The adsorbent prescription: inorganic bond employing water and sodium metasilicate are formulated by 3: 1 weight ratios.After active carbon is ground to-120 orders, stir and evenly mix into mixed colloidal solution according to 3: 6,3: 10,5: 8,7: 6,7: 10 part by weight with inorganic bond respectively.
Throwing method (see figure 1): be that 8cm nickel wire 102 is carrier with length, after one end is rough through sand papering, immerse in the active carbon and inorganic bond mixed colloidal solution of (1cm length) prior mixing, make its surface evenly be coated with the above-mentioned colloidal solution of last layer, natural air drying after the taking-up.
The purifier (see figure 2): the charcoal absorption silk behind the natural air drying is positioned in the closed container purified treatment under 250 ℃ of following vacuum conditions, and sealing is preserved stand-by then.
Sample absorption (see figure 3): the 200g South Yellow Sea seabed A3 sediment sample (breaking into pieces to particle diameter 0.5cm) of in port grinding bottle, packing into, be inserted in the sample purifying the back adsorption filament, cover the ground bottle stopper, put into baking oven, baking is 24 hours under 60 ℃ of conditions, the C in the sample bottle
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment;
Analyze: open bottle stopper, take out adsorption filament, cut the silk (0.5cm) that is coated with the adsorbent end, the silk of cutting is put into heat cracker carry out desorb, and the feeding gas chromatograph-mass spectrometer (GC-MS) carries out C
5-C
21Hydrocarbons is analyzed.Analysis result sees Table 5.
Comparative Examples:
(1) water and sodium metasilicate are mixed with inorganic bond, and the weight ratio of water and sodium metasilicate is 3: 1
(2) active carbon is ground to-120 orders, gets part and is tiled on the clean paper stand-by;
(3) nickel wire immerses after polishing in the binder solution that step (1) makes, and twists with finger immediately after the taking-up and rolls across active carbon layer, makes its surface stick activated carbon granule, and placement is dried;
(4) vacuum purification, sealing is preserved.
Test 1
The charcoal absorption silk 1 and the Comparative Examples charcoal absorption silk that adopt embodiment 1 to make carry out the GC-MS detection, the results are shown in Table 1, examination criteria is petroleum geology Office of Marine Geology of Ministry of Geology and Mineral Resources company standard: hydrocarbon geochemical exploration soil (rock, water) sample C6-C18 hydrocarbons is measured chromatogram/mass spectrography DS/T 02.12-2000, and sample is South Yellow Sea sea-bottom deposit matter sample
The conventional throwing method of table 1 charcoal absorption silk and throwing method GC-MS of the present invention analyze the content contrast
From the data of table 1 as can be seen, for most target compounds, the adsorption efficiency of the adsorption filament that the present invention is prepared is improved than the adsorption filament that conventional method makes, the adsorbance of total hydrocarbon also improves, therefore, adopt the adsorption efficiency of the charcoal absorption silk made from the present invention good than conventional method.
Table 2 charcoal absorption silk method detects the hydrocarbons content of Daqing oil field water sample yiy-20
| Component | Retention time (min) | Throwing content that method is surveyed of the present invention (μ L/L) |
| Pentane | 1.17 | 0.64 |
| The 2-methylpentane | 1.27 | 0.66 |
| N-hexane | 1.34 | 1.75 |
| Benzene | 1.39 | 4.84 |
| Cyclohexane | 1.47 | 11.26 |
| The 2-methyl hexane | 1.48 | 15.34 |
| The 3-methyl hexane | 1.49 | 14.92 |
| Normal heptane | 1.90 | 464.11 |
| Hexahydrotoluene | 1.98 | 9.13 |
| 2.4-dimethylhexane | 2.05 | 33.46 |
| Toluene | 2.06 | 5.22 |
| The 3-methyl heptane | 2.14 | 7.49 |
| Normal octane | 2.20 | 238.00 |
| 2.4-dimethyl heptane | 2.65 | 108.15 |
| 1.3-dimethyl benzene | 2.85 | 27.11 |
| 1.2-dimethyl benzene | 2.99 | 13.11 |
| Positive nonane | 3.33 | 178.23 |
| 1.3.5-trimethylbenzene | 4.53 | 20.28 |
| Paracresol | 4.66 | 33.15 |
| 1.2.4-trimethylbenzene | 6.23 | 6.27 |
| N-decane | 5.48 | 154.04 |
| Metacresol | 6.60 | 15.71 |
| N-undecane | 8.47 | 181.49 |
| Naphthalene | 11.25 | 4.84 |
| N-dodecane | 11.54 | 4.03 |
| N-tridecane | 14.46 | 33.80 |
| Beta-methylnaphthalene | 15.03 | 12.24 |
| The 1-methyl naphthalene | 16.19 | 14.56 |
| Biphenyl | 16.54 | 16.49 |
| N-tetradecane | 17.17 | 158.73 |
| N-pentadecane | 19.70 | 165.35 |
| Hexadecane | 22.08 | 180.70 |
| N-heptadecane | 24.33 | 202.00 |
| N-octadecane | 26.45 | 203.63 |
| NSC 77136 | 28.48 | 205.27 |
| N-eicosane | 30.59 | 157.53 |
| Heneicosane | 33.34 | 111.07 |
| Total hydrocarbon | 3014.58 |
The different proportioning throwing of table 3 inorganic bond method GC-MS analyzes the content contrast
μg/kg
The different degree of grinding active carbon of table 4 throwing method GC-MS analyzes the content contrast
μg/kg
Table 5 active carbon and inorganic bond different proportion throwing method GC-MS analyze the content contrast
μg/kg
Claims (8)
1. charcoal absorption silk is characterized in that: prepare according to the following steps:
(1) water and sodium metasilicate are mixed with inorganic bond, and the weight ratio of water and sodium metasilicate is (1～5): (0.1～3);
(2) active carbon is ground to below 80 orders, and the inorganic bond that makes with step (1) is by weight (3～7): (6～10) stir and make mixed colloidal solution;
(3) wire immerses after polishing in the mixed colloidal solution that step (2) makes, and leaves standstill the back and takes out natural air drying;
(4) vacuum purification, sealing is preserved.
2. charcoal absorption silk as claimed in claim 1 is characterized in that:
The weight ratio of water and sodium metasilicate is: (2～4): (1～3).
3. charcoal absorption silk as claimed in claim 1 is characterized in that:
The weight ratio of described active carbon and inorganic bond is: (4～6): (7～9).
4. as the described charcoal absorption silk of one of claim 1～3, it is characterized in that:
Wire is iron wire or nickel wire in the described step (3), and the wire length that enters in the mixed colloidal solution is 0.5-3cm.
5. as the preparation method of the described charcoal absorption silk of one of claim 1～4, comprise following steps:
(1) water and sodium metasilicate are mixed with inorganic bond by described weight ratio;
(2) after active carbon ground, the inorganic bond that makes with step (1) stirred by described weight ratio and makes mixed colloidal solution;
(3) wire immerses after polishing in the mixed colloidal solution that step (2) makes, and takes out natural air drying;
(4) vacuum purification, sealing is preserved.
6. preparation method as claimed in claim 5 is characterized in that:
The vacuum purification temperature is 180-300 ℃ in the described step (4), vacuum is-and 0.05MPa～-0.1MPa, the clarification time is 1～5h.
7. preparation method as claimed in claim 6 is characterized in that:
The vacuum purification temperature is 250 ℃ in the described step (4).
8. as the using method of the described charcoal absorption silk of one of claim 1～4, adopt one of following two kinds of methods:
A) absorption of solid sample
The solid sample of packing in port grinding bottle is inserted in the charcoal absorption silk in the sample, covers the ground bottle stopper, puts into baking oven, and baking is 16-48 hour under 40-60 ℃ of condition, the C in the sample bottle
5-C
21Hydrocarbons will desorb and be adsorbed an adsorption and enrichment;
B) absorption of fluid sample
The fluid sample of packing in the fluid sample air-tight bottle, certain space is left on top, the charcoal absorption silk is not coated with the adsorbent end is fixed on the bottle stopper, makes to be coated with the adsorbent end and to be placed on the fluid sample upper space, 40-60 ℃ of following adsorption and enrichment 16-48h of water-bath heating.
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| 冯建跃 等.一种新颖的色谱采样器——吸附丝的研究.《浙江大学学报》.1992,第26卷(第1期),第76-79页. |
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