CN101940917B - Processing method of adsorbent - Google Patents
Processing method of adsorbent Download PDFInfo
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- CN101940917B CN101940917B CN 200910012484 CN200910012484A CN101940917B CN 101940917 B CN101940917 B CN 101940917B CN 200910012484 CN200910012484 CN 200910012484 CN 200910012484 A CN200910012484 A CN 200910012484A CN 101940917 B CN101940917 B CN 101940917B
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Abstract
The invention discloses a processing method of an adsorbent, comprising the following steps: desorbing the water adsorbed by the adsorbent; soaking by adopting ketone of C3-C6; and finally drying and roasting. The adsorbent processed by the method of the invention is preferentially selected as magnesium silicate adsorbent for processing petroleum hydrocarbon analysis; the processed magnesium silicate can effectively adsorb and eliminate the interference of the polar nonhydrocarbon organic matter in water, soil or solid waste sample extract to the petroleum hydrocarbon detection. The method of the invention is as follows: (1) the organic solvent is used for soaking the adsorbent, thus eliminating the differences in the properties of the magnesium silicate adsorbent brought by impurity adsorption, and improving the adsorption stability and the repetitiveness of the adsorbent; (2) the adsorbent adopts an activated manner; the adsorption efficiency of the adsorbent to the polar matter is higher at the activated state; the recovery of the nonpolar matters, such as petroleum and the like is higher; and (3) the time of activating treatment process is shorter than that of deactivating treatment proce4ss, thus saving a great amount of time.
Description
Technical field
The present invention relates to a kind of processing method of adsorbent, the processing method of the magnesium silicate adsorbent that uses during particularly water quality PetroChina Company Limited. class and vegetable and animals oils are measured.The magnesium silicate adsorbent that the present invention handles can effectively adsorb and eliminate the interference that water, soil or solid waste sample extraction liquid Semi-polarity nonhydrocarbon organic matter are measured petroleum hydrocarbon.
Background technology
Oily substance is the problem of global concern to the pollution of water body, the water that polluted by petroleum-type has the oil flavor, toxic to biology, the water surface can form oil film, destroy its dissolved oxygen balance, oily substance is a kind of major pollutants concerning water environment, and wherein petroleum substance is the most outstanding organic pollution.Therefore, the degree of accuracy of water quality PetroChina Company Limited. class mensuration is most important to environmental monitoring, assessment and improvement.
At present, the standard method that China measures water quality PetroChina Company Limited. class is " the mensuration infrared spectrophotometry of GB/T 16488-1996 water quality petroleum-type and vegetable and animals oils ", wherein the processing procedure of employed magnesium silicate adsorbent is: get 60～100 order magnesium silicates in porcelain evaporating dishes, place 500 ℃ of heating 2h in the high temperature furnace, move in the drier after in stove, being chilled to about 200 ℃ and be chilled to room temperature, in ground glass stoppered bottle, preserve.During use, take by weighing an amount of dry magnesium silicate and place ground glass stoppered bottle, according to the weight of dry magnesium silicate, add an amount of distilled water in the ratio of 6% (m/m) and carry out deactivation, Mi Sai and fully vibration several minutes are used after placing about 12h.
Because the difference of production and laboratory environment, the pollution that brings in magnesium silicate preparation and the put procedure has nothing in common with each other, and this will directly affect repeatability and the accuracy of petroleum substance measurement result.Magnesium silicate needs time of placing longer in the deactivation process, and the magnesium silicate after the deactivation weakens greatly to the adsorption efficiency of water quality Semi-polarity material, cause the measurement result of petroleum-type higher, thereby influenced the accuracy of environment measuring and assessment, brought inconvenience to environmental improvement.
Summary of the invention
Deficiency at existing magnesium silicate sorbent treatment process, the invention provides the processing method of using the magnesium silicate adsorbent in a kind of water quality PetroChina Company Limited.'s class and the vegetable and animals oils mensuration process, the magnesium silicate adsorbent that the inventive method is handled has the measurement result good reproducibility, to the absorption efficiency advantages of higher of polar substances.
The processing method process of adsorbent of the present invention is as follows: at first remove adsorbent water, adopt the ketone dipping of C3～C6 then, carry out drying and calcination process at last.Wherein said adsorbent is magnesium silicate adsorbent, silica gel absorber, adsorbent of molecular sieve etc.
In the processing method of adsorbent of the present invention, the method for operating that removes adsorbents adsorb water is the low-temperature bake method, as getting final product at 100～140 ℃ of following roasting 2～6h.
In the processing method of adsorbent of the present invention, adsorbent after the dehydration adopts the ketone dipping of C3～C6, and dipping can adopt saturated dipping, also can adopt the supersaturation dipping, below the boiling temperature of dipping temperature for the ketone of use C3～C6, dip time is 40～120min.The ketone dipping of C3～C6 can adopt dry mode that the ketone of C3～C6 is removed later, and drying can adopt constant pressure and dry or vacuum drying, and dry temperature is generally 20～200 ℃, is generally drying time 1～5 hour.Dried calcination process condition is 450～550 ℃ of following roastings 1～4 hour.When being cooled to 100～250 ℃ after the roasting, put into drier cooling cooling.The preferred acetone of the ketone of C3～C6, MEK, 2 pentanone, propione, methyl iso-butyl ketone (MIBK) etc.
The processing method of adsorbent of the present invention has the most outstanding treatment effect when being used for the processing of magnesium silicate adsorbent.Key is that (1) with an organic solvent carry out impregnation process to adsorbent, can eliminate different production and the qualitative difference of magnesium silicate adsorbent that environment for use is brought like this, has improved absorption stability and the repeatability of adsorbent.(2) magnesium silicate adopts activation method.Magnesium silicate is higher to the adsorption efficiency of polar substances under the state of activation, and also higher to the rate of recovery of apolar substance (petroleum-type).(3) the activation processing process is shorter than the deactivation processing procedure time, has saved a large amount of time.
In the processing method of adsorbent of the present invention, be greatly improved through stability and the repeatability of the magnesium silicate behind the organic solvent dipping to measurement result, and the magnesium silicate after the activation is to the also raising greatly of absorption efficiency of polar substances.Experiment shows, to the relative standard deviation of measuring petroleum-type can reach＜0.3%, to the relative standard deviation of measuring polar substances can reach＜0.6%.And the magnesium silicate that soaks through organic solvent is 1.36%～14.6% to the relative standard deviation of petroleum-type, is 1.07%～7.80% to the relative standard deviation of polar substances; Magnesium silicate after activated can reach 99.5%～100% to the rate of recovery of petroleum-type, can reach 96.3%～100% to the adsorption efficiency of polar substances.Magnesium silicate after the deactivation can reach 97.6%～99.5% to the rate of recovery of petroleum-type, and the adsorption efficiency of polar substances is had only 51.3%～53.5%.
Description of drawings
Fig. 1 is the glass chromatography column schematic diagram that adsorbent is housed.
Among the figure: 1-adsorbent, 2-mineral wool, 3-glass chromatography column.
The specific embodiment
Be example with the magnesium silicate adsorbent below, specify the operating procedure of the processing method of adsorbent of the present invention.
(1) get 60～100 order magnesium silicate adsorbents in porcelain evaporating dishes, 100～140 ℃ of drying 2～6h of low temperature remove physical absorption water.
(2) magnesium silicate after will dewatering floods with the ketone of C3～C6, and its volume ratio is: V
Ketone: V
Absorption Agent=2: 1～3: 1, dip time is preferably 1～2h.
(3) will flood to be put in after good magnesium silicate drains and carry out drying at room temperature in the drier that vacuumizes, be preferably 1～3h drying time.
(4) dried magnesium silicate is carried out high-temperature roasting, temperature is 450～550 ℃, and the time is preferably 1～3h.
(5) move in the drier after in stove, being chilled to about 200 ℃ after the magnesium silicate roasting is finished and be chilled to room temperature, in ground glass stoppered bottle, preserve, stand-by.
With above-mentioned magnesium silicate load map 1 glass chromatography column of handling well (
) in, the magnesium silicate packed height is 80mm, a small amount of mineral wool is clogged in the glass chromatography column exit.
The light diesel fuel (200～350 ℃ of boiling range scopes) that nonpolar standard sample selects Russian imported crude oil straight run to go out.The above-mentioned light diesel fuel of 5 same concentrations of preparation respectively by above-mentioned magnesium silicate glass chromatographic column, is measured the light diesel fuel after absorption they respectively with chromatography then, verifies that by measurement result magnesium silicate is to the repeatability of apolar substance absorption.
Polarity standard's sample is selected methyl oleate.The methyl oleate of 5 same concentrations of preparation respectively by above-mentioned magnesium silicate glass chromatographic column, is measured the methyl oleate after absorption they respectively with chromatography then, verifies that by measurement result magnesium silicate is to the repeatability of polar substances absorption.
The nonpolar standard sample of 3 variable concentrations of preparation, with them respectively by above-mentioned magnesium silicate glass chromatographic column, then the light diesel fuel after absorption is measured respectively with chromatography, verified that by measurement result magnesium silicate is to the rate of recovery of variable concentrations apolar substance.
Polarity standard's sample of 3 variable concentrations of preparation, with them respectively by above-mentioned magnesium silicate glass chromatographic column, then the methyl oleate after absorption is measured respectively with chromatography, verified that by measurement result magnesium silicate is to the absorption efficiency of variable concentrations polar substances.
Chromatographic condition: 280 ℃ of injector temperatures, 300 ℃ of detector temperatures, 45 ℃ of column temperatures (3min), rise to 280 ℃ (30min) with 12 ℃/min, flow rate of carrier gas 1.5mL/min, split sampling (not shunting time 0.75min) not, hydrogen flow rate 35mL/min, air velocity 400mL/min, sample size 1 μ L.
Set forth technical scheme of the present invention below in conjunction with embodiment, but be not limited to the embodiment of the invention.
Embodiment 1
(1) get 50g 60～100 order magnesium silicates in porcelain evaporating dishes, 140 ℃ of dry 4h of low temperature remove physical absorption water.
(2) magnesium silicate is carried out saturated immersion with acetone, its volume ratio is: V
Acetone: V
Magnesium silicate=3: 1, dip time is 1h.
(3) will flood good magnesium silicate and be put in and carry out drying at room temperature in the drier that vacuumizes, be 2h drying time.
(4) dried magnesium silicate is carried out high-temperature roasting, temperature is 500 ℃, and the time is 2h.
(5) move in the drier after in stove, being chilled to about 200 ℃ after the magnesium silicate roasting is finished and be chilled to room temperature, in ground glass stoppered bottle, preserve, stand-by.
(6) magnesium silicate after the above-mentioned processing is slowly poured in Fig. 1 glass chromatography column, the limit bevelling beats gently, and the packed height of magnesium silicate is 80mm.A small amount of mineral wool is clogged in the glass chromatography column exit.
(7) the nonpolar standard sample of weighing 0.1204g is settled to 50mL with carrene, and making 5 concentration altogether with quadrat method is 2.41 * 10
3The light diesel fuel of ng/ μ L.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Diesel oil after magnesium silicate absorption is measured respectively with chromatography, and repeatability the results are shown in Table 1.
Table 1 magnesium silicate absorption diesel oil repeatability
(8) weighing 0.2177g polarity standard sample is settled to 50mL with carrene, and preparing 5 concentration altogether with quadrat method is 4.35 * 10
3The polarity standard specimen methyl oleate of ng/ μ L.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Methyl oleate after magnesium silicate absorption is measured respectively with chromatography, and repeatability the results are shown in Table 2.
Table 2 is methyl oleate concentration repeatability after adsorbing
(9) difference weighing 0.1107g, the nonpolar standard sample of 0.2057g, 0.3125g are settled to 50mL respectively with carrene, are mixed with 3 variable concentrations light diesel fuels.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Diesel oil is measured respectively with chromatography after magnesium silicate absorption, and the rate of recovery the results are shown in Table 3.
The rate of recovery of table 3 pair variable concentrations light diesel fuel
| Concentration before the absorption, ng/ μ L | Absorption back concentration, ng/ μ L | The rate of recovery, % |
| 2.21×10 3 | 1.11×10 3 | 100 |
| 4.11×10 3 | 2.05×10 3 | 99.8 |
| 6.25×10 3 | 3.11×10 3 | 99.5 |
(10) difference weighing 0.0707g, 0.1219g, 0.2177g polarity standard sample are settled to 50mL respectively with carrene, are mixed with the polarity standard specimen methyl oleate of 3 variable concentrations.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Methyl oleate is measured respectively with chromatography after magnesium silicate absorption, and absorption efficiency the results are shown in Table 4.
The absorption efficiency of table 4 pair variable concentrations polarity standard specimen methyl oleate
| Concentration before the absorption, ng/ μ L | Absorption back concentration, ng/ μ L | Absorption efficiency, % |
| 1.41×10 3 | 2.12 | 99.7 |
| 2.44×10 3 | 8.53 | 99.3 |
| 4.35×10 3 | 52.3 | 97.6 |
(1) get 50g 60～100 order magnesium silicates in porcelain evaporating dishes, 130 ℃ of dry 3h of low temperature remove physical absorption water.
(2) magnesium silicate after will dewatering carries out saturated immersion, V with MEK
MEK: V
Magnesium silicate=2: 1.Soak time is 90min.
(3) will flood good magnesium silicate be put in the drier that vacuumizes 80 ℃ dry down, be 1.5h drying time.
(4) dried magnesium silicate is carried out high-temperature roasting, temperature is 500 ℃, and the time is 2.5h.
(5) move in the drier after in stove, being chilled to about 200 ℃ after the magnesium silicate roasting is finished and be chilled to room temperature, in ground glass stoppered bottle, preserve, stand-by.
(6) magnesium silicate after the above-mentioned processing is slowly poured in Fig. 1 glass chromatography column, the limit bevelling beats gently, and the packed height of magnesium silicate is 80mm.A small amount of mineral wool is clogged in the glass chromatography column exit.
(7) the nonpolar standard sample of weighing 0.1805g is settled to 50mL with carrene, and making 5 concentration altogether with quadrat method is 3.61 * 10
3The light diesel fuel of ng/ μ L.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Diesel oil after magnesium silicate absorption is measured respectively with chromatography, and repeatability the results are shown in Table 5.
Table 5 is diesel oil concentration repeatability after adsorbing
(8) weighing 0.1235g polarity standard sample is settled to 50mL with carrene, and preparing 5 concentration altogether with quadrat method is 2.47 * 10
3The polarity standard specimen methyl oleate of ng/ μ L.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Methyl oleate after magnesium silicate absorption is measured respectively with chromatography, and repeatability the results are shown in Table 6.
Table 6 is methyl oleate concentration repeatability after adsorbing
(9) difference weighing 0.0711g, the nonpolar standard sample of 0.1623g, 0.2712g are settled to 50mL respectively with carrene, are mixed with 3 variable concentrations light diesel fuels.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Diesel oil is measured respectively with chromatography after magnesium silicate absorption, and the rate of recovery the results are shown in Table 7.
The rate of recovery of table 7 pair variable concentrations light diesel fuel
| Concentration before the absorption, ng/ μ L | Absorption back concentration, ng/ μ L | The rate of recovery, % |
| 1.42×10 3 | 711 | 100 |
| 3.25×10 3 | 1.62×10 3 | 99.7 |
| 5.42×10 3 | 2.70×10 3 | 99.6 |
(10) difference weighing 0.1621g, 0.2895g, 0.3345g polarity standard sample are settled to 50mL respectively with carrene, are mixed with the polarity standard specimen methyl oleate of 3 variable concentrations.They are crossed above-mentioned magnesium silicate glass chromatographic column respectively, filtrate is settled to 100mL respectively with carrene.
Methyl oleate is measured respectively with chromatography after magnesium silicate absorption, and absorption efficiency the results are shown in Table 8.
The absorption efficiency of table 8 pair variable concentrations polarity standard specimen methyl oleate
| Concentration before the absorption, ng/ μ L | Absorption back concentration, ng/ μ L | Absorption efficiency, % |
| 3.24×10 3 | 17.8 | 98.9 |
| 5.79×10 3 | 81.2 | 97.2 |
| 6.69×10 3 | 118 | 96.5 |
Claims (7)
1. the processing method of an adsorbent is characterized in that: at first remove adsorbent water, adopt the ketone dipping of C3～C6 then, carry out drying and calcination process at last; Described adsorbent is the magnesium silicate adsorbent; Wherein dried calcination process condition is 450～550 ℃ of following roastings 1～4 hour, when being cooled to 100～250 ℃ after the roasting, puts into drier cooling cooling.
2. it is characterized in that in accordance with the method for claim 1: described adsorbent is the magnesium silicate adsorbent that uses during water quality PetroChina Company Limited. class and vegetable and animals oils are measured.
3. it is characterized in that in accordance with the method for claim 1: the method for operating that removes adsorbents adsorb water is the low-temperature bake method; Low-temperature bake is at 100～140 ℃ of following roasting 2～6h.
4. in accordance with the method for claim 1, it is characterized in that: the adsorbent after the dehydration adopts the ketone dipping of C3～C6, and dipping adopts saturated dipping, perhaps adopts the supersaturation dipping.
5. according to claim 1 or 4 described methods, it is characterized in that: below the boiling temperature of dipping temperature for the ketone of use C3～C6, dip time is 40～120min.
6. according to claim 1 or 4 described methods, it is characterized in that: during dipping, the volume ratio V of ketone and adsorbent
Ketone: V
Adsorbent=2: 1～3: 1.
7. in accordance with the method for claim 1, it is characterized in that: dry employing constant pressure and dry or vacuum drying, dry temperature is 20～200 ℃, be 1～5 hour drying time.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1343204A (en) * | 1999-03-16 | 2002-04-03 | 国际壳牌研究有限公司 | Process for purification of propylene oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1343204A (en) * | 1999-03-16 | 2002-04-03 | 国际壳牌研究有限公司 | Process for purification of propylene oxide |
Non-Patent Citations (1)
| Title |
|---|
| 夏晓萍等.红外光谱法测定城市污泥中油类的方法探讨.《市政技术》.2008,第26卷(第3期),218-220. * |
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