CN104697883A - Method for determining aged oil sludge components based on two-time reflux and two-time determination of sample tube weight - Google Patents
Method for determining aged oil sludge components based on two-time reflux and two-time determination of sample tube weight Download PDFInfo
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Abstract
The invention discloses a method for determining aged oil sludge components based on two-time reflux and two-time determination of sample tube weight. The method comprises the following steps: (1) sample loading: by virtue of a reflux device, loading aged oil sludge into a filter paper sample tube, and immobilizing the sample tube on the flask neck of the reflux device; (2) primary refluxing: by virtue of methods of reflux dissolving and carrying, dissolving oil in the oil sludge and taking out water, so that silt and asphaltene leave in the oil sludge, and separating out water in a solvent; (3) primary determination: determining the content of the separated water and the dry weight of the sample tube; (4) secondary refluxing: by virtue of a method of reflux dissolving, dissolving the asphaltene in the silt of the sample tube in the solvent, so that only silt leaves in the oil sludge in the sample tube; and (5) secondary determination: determining the dry weight of the sample tube once again, thus calculating the contents of water, oil, mud and asphaltene in the aged oil sludge.
Description
Technical field
The present invention relates to greasy filth compound mensuration method.
Background technology
Can produce a large amount of waste oil sludges in oil exploitation, storage and process of manufacture, it is reported, every 500 tons of crude oil produce 1 ton of greasy filth, and China Petroleum produces about 300 ten thousand tons of various greasy filth every year.Greasy filth is a potpourri containing petroleum hydrocarbon, water, inorganic solid etc., it is a kind of high-risk pollutant, greasy filth has been listed in " National Hazard refuse catalogue " by China, and China's " solid waste environmental pollution prevention and control method " and " national promotion law on cleaner production " requirement must carry out harmless treatment to greasy filth; Meanwhile, because containing certain petroleum hydrocarbon in greasy filth, greasy filth is also a kind of energy resources of preciousness.Therefore greasy filth resource, innoxious process for treating research be in recent years everybody pay close attention to focus.Current oil-sludge treatment technology mainly contains solvent extraction method, thermochemistry washing methods, coking disposal route, thermal desorption disposal route etc., and the oil-sludge treatment choice of technology and oil-sludge treatment difficulty or ease and greasy filth form closely related.
Greasy filth composition is generally expressed as liquid water content, oil content, solid (mud) content, and greasy filth PetroChina Company Limited. composition generally represents with Four composition, i.e. saturated point (alkane), fragrant point, colloid, bituminous matter.Generally being insoluble to low molecule (C5 ~ C7) n-alkane in oil but the material that can be dissolved in hot benzene calls bituminous matter, can be dissolved in the material that benzene can be dissolved in again low molecule (C5 ~ C7) n-alkane and be called solvend, solvend comprises saturated point, fragrance point and colloid.When greasy filth oil content is higher, be suitable for solvent extraction method process greasy filth, but solvent is selected to form relevant with oil in greasy filth, namely greasy filth studies on asphaltene content is high, should select the solvent that aromaticity is higher.When the oil content of greasy filth is lower, available thermochemistry washing method process greasy filth, but the asphalt content in greasy filth affects the difficulty or ease that in greasy filth, oil reclaims, and the difficulty of the more washing separating oil-sand of bituminous matter strengthens.When in greasy filth, higher, the liquid water content of oil content is lower, be suitable for by coking method and THE METHOD OF THERMAL DESORPTION, but when asphalt content height in greasy filth, coke (economic worth of coke the is low) amount of generation is large, light oil amount is low, affects the economic benefit of oil-sludge treatment.Therefore, the oil content of greasy filth, oily studies on asphaltene content have significant impact to oil-sludge treatment method choice and process economic benefit etc.
At present, the constitutes analysis method such as oil content, liquid water content, solid content of greasy filth mainly contains solvent extraction-gravimetric method, high temperature gravimetric method, solvent extraction spectrophotometric method etc., also needs to adopt other method to the content analyzing greasy filth studies on asphaltene.Solvent extraction-gravimetric method, namely utilize organic solvent by after oil extraction in silt particle, volatilization desolventizes oil content of weighing to obtain, and extract remaining silt particle and dry weigh to obtain cement content or solid content, difference is liquid water content; Or at 105 DEG C ~ 110 DEG C dry constant weight greasy filth, dendrometry weight obtains the liquid water content of greasy filth, utilizes solvent extraction silt particle, and oil content of weighing to obtain after solvent is removed in volatilization, and all the other are cement content.High temperature gravimetric method, calcines constant weight by greasy filth, records solid content at 500 DEG C ~ 600 DEG C, and utilize loss on drying at carrying agent circumfluence method analysis liquid water content or 105 DEG C ~ 110 DEG C to record liquid water content, oil content is then for sample deducts the amount after water, mud.Solvent extraction spectrophotometric method, after namely using petroleum ether extraction greasy filth, with the oil content in spectrophotometric analysis solvent, thus obtains the oil content of greasy filth.Oil studies on asphaltene composition mainly utilizes low molecule n-alkane (as normal heptane) and light aromatic hydrocarbons (as benzene or toluene) to measure asphaltene dissolution capacity variance.
General tank bottom oil sludge is higher than the oil content of ground sludge, and the oil content of tank bottom oil sludge is generally 15 ~ 50% (liquid water content, solid content are respectively 30 ~ 85% and 5 ~ 46%).General greasy filth PetroChina Company Limited. consists of saturated point (alkane) of 40 ~ 52%, the fragrance of 28 ~ 31% divides, the colloid of 7 ~ 22.4%, the bituminous matter of 8-10%.Therefore, generally the asphalt content of greasy filth is little, little on oil-sludge treatment impact.Greasy filth is transformed into bituminous matter due to volatilization such as 1. light hydrocarbon component and moisture etc., 2. colloid depositing process, such that greasy filth liquid water content reduces, oil content increases and oil studies on asphaltene content increases, and greasy filth occurs aging.The technical foundation to treatment of aged greasy filth to the analysis of the composition analysis (comprising asphalt content) of aging greasy filth.Because the asphalt content of general heavy oil is high, therefore, for heavy oil greasy filth, the greasy filth composition analysis comprising asphalt content is also very necessary.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides a kind of simply based on the method for the aging greasy filth component of twice backflow and twice working sample pipe weight.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
Based on a method for the aging greasy filth component of twice backflow and twice working sample pipe weight, comprise the steps:
1) fill sample: utilize reflux, aging greasy filth (heavy W) is loaded the flask neck place that filter paper sample pipe (the heavy Ws of sample hose) is fixed on reflux;
2) first time backflow: first by the method that backflow is dissolved and carried, dissolves the oil content in greasy filth and moisture is taken out of, makes greasy filth be left silt and bituminous matter, then isolates the moisture in solvent;
3) first time measures: the dry weight (sample hose and silt, bitum general assembly (TW) W1) measuring isolated moisture (volume of moisture is the density p of V, water), sample hose;
4) second time backflow: again by the method that backflow is dissolved, by the asphaltene dissolution in sample hose in solvent, makes the only remaining silt of the greasy filth in sample hose;
5) second time measures: the dry weight (the general assembly (TW) W1 of sample hose and silt) of random sample QC again, can calculate the water in aging greasy filth, oil, cement content and asphalt content or oily studies on asphaltene content.
Specifically be calculated as follows:
Volume V according to greasy filth example weight W and water can calculate greasy filth liquid water content; The difference of W2 and Ws is the quality of silt particle, can calculate the cement content of greasy filth divided by greasy filth weight W; The liquid water content of greasy filth and the remaining content of cement content are then oil content; The difference of W1 and W2 is bituminous matter weight, can calculate greasy filth studies on asphaltene content divided by greasy filth weight W, or can calculate oily studies on asphaltene content divided by oil heavy (W-(V/ ρ)-(W2-Ws)).
Preferably, described step 1) in, blue bottleneck sample being fixed on flask is hung by cross, described sample hose is the test tube that filter paper makes, described cross hanging basket is obtained by iron wire, sample device is placed in sample hose, hangs indigo plant at the cross that is placed in of being fitted by sample organ pipe, cross hangs the junction that indigo plant is hung on flask mouth and receiver.
Preferably, described step 2) in, adopt sherwood oil as solvent, backflow 2-3h; Preferred backflow 2h.
Preferably, described step 2) in, the method isolating the moisture in solvent is:
Utilize receiver to receive condensation is got off from condenser pipe moisture and oil content, receiver is arranged to be communicated with by moisture receiving tube and arm the mode formed, arm is arranged at the top of moisture receiving tube, meeting AUTOMATIC ZONING after the moisture with solvent received flows into moisture receiving tube, make sedimentation in moisture receiving tube go out moisture, the solvent being arranged in upper strata flows into flask by arm.
Preferably, described step 3) in, determination step 2) in isolated moisture time, adopt and moisture receiving tube be provided with high precision scale mark, directly read moisture by scale mark.
Preferably, described step 3) in, after backflow terminates, naturally cool, take out sample hose, dry, weigh, be the silt in sample hose, greasy filth and bitum gross weight.
Preferably, described step 4) in, by step 3) in silt and bitum sample hose are housed from the bottleneck being newly placed on flask, adopt toluene as solvent, backflow 2-3h, brings into asphaltene dissolution in solvent; Preferred backflow 2h.
Preferably, described step 5) in, backflow terminates, and naturally cools, and takes out sample hose, drying, weighs.
Preferably, described step 1) in, aging for 10g greasy filth is put into sample organ pipe; Adding solvent during first time backflow is 200mL; Adding solvent during second time backflow is 200mL.
The principle of the inventive method:
In aging greasy filth, greasy filth forms: water+oil+silt, oily and bitum relation is relation of inclusion, wherein oil=saturated part+fragrant part+colloid+bituminous matter.Sherwood oil boiling cooling for reflux, greasy filth in drip washing sample hose, solvable point (saturated point, fragrant point, colloid) in greasy filth is dissolved in sherwood oil, sherwood oil reduces the viscosity of greasy filth simultaneously, the water in greasy filth can be made to be released, be dissolved with the sample hose that the sherwood oil of solvable point and water makes through filter paper and fall into flask, the silt particle in greasy filth and the bituminous matter in oil are then intercepted at sample hose.Water can seethe with excitement and steam together with sherwood oil, and after condensation, condensed fluid to flow on the left of receptacle in the graduated pipe of tool.Because the density of the density ratio sherwood oil of water is large, moisture just can be deposited to the bottom of the moisture receiving tube of receptacle, and the sherwood oil on receptacle moisture receiving tube top returns flask.Along with constantly refluxing and distilling, solvable point in greasy filth is constantly leached out, and moisture is constantly carried out by sherwood oil and is constantly deposited to moisture receptacle moisture receiving tube bottom.According to the amount of greasy filth and the volume V of moisture that steams, the liquid water content of greasy filth can be calculated.Taking-up sample hose is weighed, and obtains sample hose and silt particle and bituminous matter total amount W1.
After sherwood oil in withdrawing device and solvable point of oil, add toluene, sample hose (containing silt particle and bituminous matter) is put back in device, adds hot reflux.Toluene dissolved bitumen matter, is dissolved with bitum toluene solvant and gets back in flask through papery sample hose, and silt particle is trapped within sample hose.After backflow terminates, naturally cool to room temperature, take out sample hose and weigh, sample hose and silt particle total amount W2.Therefore, (W1-W2) is bituminous matter weight; (W2-Ws) be silt particle weight, (W-(V/ ρ)-(W2-Ws)) is weight of oil, can calculate cement content, oil content, greasy filth asphalt content or oily studies on asphaltene content thus.Beneficial effect of the present invention:
The present invention provides a kind of method of water that can measure in aging greasy filth, oil, mud, pitch first, by twice backflow and twice mensuration, simple to operate, design ingenious, water in aging greasy filth, oil, silt particle are separated with bituminous matter, and measure the content of these four components accurately, error is little.This method is not only simple to operate, overcome a difficult problem for the complicated operation that spectrophotometric method in prior art needs standard sample to cause, and the difficult problem that the complex steps of high temperature gravimetric method and solvent extraction is loaded down with trivial details with calculating, and instrument equipment is few, a reflux.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for instructions, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural representation of the embodiment of the present invention 1;
In figure, the wide mouth round-bottomed flask with long neck of 1--, 2--sample hose, 3--receiver, 31-moisture receiving tube, 32--arm, 33--spherical valve, 4--condenser pipe, 5--cross hangs indigo plant, 6--adapter.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1:
Based on a method for the aging greasy filth component of twice backflow and twice working sample pipe weight, adopt device as shown in Figure 1, analyze the asphalt content of the liquid water content of greasy filth, oil content, solid content and greasy filth.
The present invention's reflux used, as Fig. 1, comprises wide mouth round-bottomed flask with long neck 1, sample hose 2, receiver 3, condenser pipe 4, cross hangs blue 5, adapter 6.Described receiver 3 to be communicated with the arm 32 on the top being positioned at water receiving tube by water receiving tube 31 and to form (as shown in Figure 1), described moisture receiving tube 31 is provided with scale, scale range 0 ~ 10ml, pin-point reading is 0.1ml, spherical valve 33 is provided with, for releasing the liquid of the reception in moisture receiving tube at the lower port place of moisture receiving tube.
Concrete operations are:
The first step: get sherwood oil (boiling range 60-90 DEG C) 200ml, greasy filth sampling 10g puts into sample hose (sample hose weight Ws), backflow 2h, naturally cool, read the water volume V of receiving tube, take out the sherwood oil that absorption is removed in sample hose drying (105 DEG C) volatilization, weigh to obtain sample hose and silt particle and bituminous matter total amount W1; Solvent in flask is taken out, the solvent in emptying receiver.
Second step: get toluene (boiling point 110 DEG C) 200ml, the sample hose (containing greasy filth silt particle and bituminous matter) of first step drip washing is put back in device, backflow 2h, naturally cool, take out the toluene that absorption is removed in sample hose drying (115 DEG C) volatilization, weigh to obtain sample hose and silt particle total amount W2
3rd step: the liquid water content, cement content, oil content, the asphalt content that calculate greasy filth.In table 1
Table 1 greasy filth forms
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1., based on a method for the aging greasy filth component of twice backflow and twice working sample pipe weight, it is characterized in that: comprise the steps:
1) sample is filled: utilize reflux, aging greasy filth dress filter paper sample pipe is fixed on the flask neck place of reflux;
2) first time backflow: first by the method that backflow is dissolved and carried, dissolves the oil content in greasy filth and moisture is taken out of, makes greasy filth be left silt and bituminous matter, then isolates the moisture in solvent;
3) first time measures: the dry weight measuring isolated moisture, sample hose;
4) second time backflow: again by the method that backflow is dissolved, by the asphaltene dissolution in sample hose silt in solvent, makes the only remaining silt of the greasy filth in sample hose;
5) second time measures: the dry weight of random sample QC again, can calculate the water in aging greasy filth, oil, mud, bitum content.
2. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, it is characterized in that: described step 1) in, blue bottleneck sample being fixed on flask is hung by cross, described sample hose is the test tube that filter paper makes, described cross hanging basket is obtained by iron wire, sample is placed in sample hose, hangs indigo plant at the cross that is placed in of being fitted by sample hose, cross hangs the junction that indigo plant is hung on flask mouth and receiver.
3. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, is characterized in that: described step 2) in, adopt sherwood oil as solvent, backflow 2-3h; Preferred backflow 2h.
4. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, is characterized in that: described step 2) in, the method isolating the moisture in solvent is:
Utilize receiver to receive condensation is got off from condenser pipe moisture and oil content, receiver is arranged to be communicated with by moisture receiving tube and arm the mode formed, arm is arranged at the top of moisture receiving tube, meeting AUTOMATIC ZONING after the moisture with solvent received flows into moisture receiving tube, make sedimentation in moisture receiving tube go out moisture, the solvent being arranged in upper strata flows into flask by arm.
5. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 4, it is characterized in that: described step 3) in, determination step 2) in isolated moisture time, adopt and moisture receiving tube is provided with high precision scale mark, directly read moisture by scale mark.
6. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, it is characterized in that: described step 3) in, after backflow terminates, naturally cool, take out sample hose, drying, weighs, and is the silt in sample hose, greasy filth and bitum gross weight.
7. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, it is characterized in that: described step 4) in, by step 3) in silt and bitum sample hose are housed from the bottleneck being newly placed on flask, adopt toluene as solvent, backflow 2-3h, brings into asphaltene dissolution in solvent; Preferred backflow 2h.
8. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, is characterized in that: described step 5) in, backflow terminates, and naturally cools, and takes out sample hose, drying, weighs.
9. the method for the aging greasy filth component based on twice backflow and twice working sample pipe weight according to claim 1, is characterized in that: described step 1) in, aging for 10g greasy filth is put into sample organ pipe; Adding solvent during first time backflow is 200mL; Adding solvent during second time backflow is 200mL.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101852708A (en) * | 2010-04-30 | 2010-10-06 | 武汉钢铁(集团)公司 | Method for detecting oil content in multiphase body |
| CN102455346A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Asphalt analysis apparatus and use of the asphalt analysis apparatus in asphalt determination |
| CN102645447A (en) * | 2012-05-10 | 2012-08-22 | 大连交通大学 | Device and method for measuring water content in crude oil by means of distillation method |
| CN103048164A (en) * | 2013-01-08 | 2013-04-17 | 长安大学 | Sampling method of solution method for asphalt component separation |
| CN203785942U (en) * | 2014-01-28 | 2014-08-20 | 中国石油化工股份有限公司 | Receiver for testing water content of high-water-content crude oil |
-
2015
- 2015-02-10 CN CN201510069911.4A patent/CN104697883A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101852708A (en) * | 2010-04-30 | 2010-10-06 | 武汉钢铁(集团)公司 | Method for detecting oil content in multiphase body |
| CN102455346A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Asphalt analysis apparatus and use of the asphalt analysis apparatus in asphalt determination |
| CN102645447A (en) * | 2012-05-10 | 2012-08-22 | 大连交通大学 | Device and method for measuring water content in crude oil by means of distillation method |
| CN103048164A (en) * | 2013-01-08 | 2013-04-17 | 长安大学 | Sampling method of solution method for asphalt component separation |
| CN203785942U (en) * | 2014-01-28 | 2014-08-20 | 中国石油化工股份有限公司 | Receiver for testing water content of high-water-content crude oil |
Non-Patent Citations (3)
| Title |
|---|
| 许修强，等: "油砂油泥含油率测定方法研究", 《化工科技》 * |
| 车泽永、罗爱兰: "《中华人民共和国石油化工行业标准》", 1 July 1993 * |
| 陈英，等: "干化罐底油泥的溶剂萃取_海水洗涤工艺", 《环境科学研究》 * |
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Application publication date: 20150610 |