CN105277462A - Composition content analysis method of tank bottom aged oil sludge - Google Patents
Composition content analysis method of tank bottom aged oil sludge Download PDFInfo
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- CN105277462A CN105277462A CN201410275339.2A CN201410275339A CN105277462A CN 105277462 A CN105277462 A CN 105277462A CN 201410275339 A CN201410275339 A CN 201410275339A CN 105277462 A CN105277462 A CN 105277462A
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Abstract
The invention relates to a composition content analysis method of tank bottom aged oil sludge. According to the composition content analysis method, petroleum ether extraction weight method and calcine ashing weight method are adopted, and at the same time, hot benzene extraction weight method is adopted to determine oil content of the oil sludge. Hot benzene is capable of dissolving all petroleum matters, so that the composition content analysis method is more accurate. Hot benzene extraction weight method and petroleum ether extraction weight method are combined, so that composition of soluble matters and asphaltene in oil content composition is determined. Calcine ashing weight method and hot benzene extraction weight method are combined for analysis of main decomposable solid content, and processed matters are subjected to XRD characterization analysis, and the composition of the main decomposable matters is speculated and determined based on XRD analysis results and compound chemical properties.
Description
Technical field
The present invention relates to the composition content analysis method of aging greasy filth at the bottom of a kind of tank.
Background technology
Tank bottom oil sludge is the desilting product of all kinds of container in oil field ground disposal system, and in sticky shape, particle is fine and closely woven, and emulsification is serious.The composition of greasy filth generally uses these three index expressions of liquid water content, oil content, solid content, and wherein oil content is most important index in oil-sludge treatment technology.Oil in greasy filth refers to oil, oil is a kind of containing hydro carbons and other organic complex mixtures a small amount of, the hydrocarbon component of typical sample comprises 200 ~ 300 kinds of different hydrocarbon, adhere to alkane, naphthenic hydrocarbon and aromatic hydrocarbon separately, non-hydrocarbons component comprises naphthenic acid, phenol, heterocyclic nitrogen and sulfide, oil in above-mentioned greasy filth is under rainwater soaks, flow into farmland, river, oxygen in water can be made to can not get supplementing, meanwhile, when oil itself is degraded by microorganisms, a large amount of oxygen be consumed, make water body severe depletion of oxygen, aquatic ecosystem wrecks; In addition, many Polycyclic aromatic hydrocarbons have mutagenesis and carcinogenicity, by direct or indirect approach, serious harm is brought to health, after some objectionable impurities enters farmland, absorbed by crops, entered in animal and mankind's body by food chain, cause various disease to occur, the health of the serious threat mankind.
Therefore, analyze the oil content in greasy filth as far as possible accurately, and according to analyzed data, process is carried out to it and seem particularly important.In prior art, the oil content analytical approach of greasy filth mainly contains solvent extraction spectrophotometric method, solvent extraction gravimetric method and calcining ashing gravimetric method, and wherein, the solvent that solvent extraction gravimetric method uses is mainly sherwood oil.Petroleum composition in general greasy filth can represent with Four composition, i.e. stable hydrocarbon, aromatic hydrocarbon, resin and asphalt.For aging greasy filth, bituminous matter is its most important composition, is the key factor affecting its treatment technology.The composition mainly low molecule (C of sherwood oil
5~ C
7) alkane, sherwood oil can extract stable hydrocarbon, aromatic hydrocarbon and colloid in greasy filth, and can not extract bituminous matter, and this just causes the oil content Lower result of petroleum ether extraction method; And calcine ashing gravimetric method and also may calcine weightlessness due to some inorganicss in greasy filth and easily cause the analysis result of oil content higher.
Summary of the invention
Technical matters to be solved by this invention is the present situation for prior art, provides that a kind of method is simple, the composition content analysis method of analysis result aging greasy filth at the bottom of tank accurately.
The present invention solves the problems of the technologies described above adopted technical scheme: the composition content analysis method of aging greasy filth at the bottom of a kind of tank, is characterized in that comprising the following steps:
(1) oil content and the composition measurement of major oil content:
Oil content measures:
A, get greasy filth sample 5g ~ 10g in the cucurbit of 50mL ~ 100mL, add benzene 15mL ~ 25mL, then add the H that volumetric concentration is 40% ~ 60%
2sO
42mL ~ 5mL, reflux at 80 DEG C 25min ~ 40min, leaves standstill and be cooled to room temperature, filters, and collects filtrate;
B, filter residue is joined in the cucurbit of 50mL ~ 100mL, add benzene 15mL ~ 25mL, then add the H that volumetric concentration is 40% ~ 60%
2sO
42mL ~ 5mL, reflux at 80 DEG C 25min ~ 40min, leaves standstill and be cooled to room temperature, filters, and collects filtrate;
C, by the mixing of the filtrate of above-mentioned collection and stratification, collect upper strata solvent phase, by this solvent evaporative removal solvent benzol at 80 DEG C, then at 105 DEG C, be dried to constant weight, obtain oily weight;
Oil content A: oil content A (%)=(oil weight/greasy filth sampling amount) × 100% of d, calculating greasy filth;
Oil content Principle components analysis:
A, utilize the oil content B (%) of petroleum ether extraction gravimetric determination greasy filth;
In b, oil content, the total content of stable hydrocarbon, aromatic hydrocarbon and colloid is oil content B (%), and the content of oil content studies on asphaltene is:
Asphalt content (%)=oil content A (%)-oil content B (%);
(2) Water content determination:
Measure dry greasy filth sample at the thermal gravimetric analysis curve of 110 DEG C, calculate the liquid water content (%) of greasy filth according to fluid loss;
(3) solid content and main decomposable asymmetric choice net solid content are analyzed:
Solid content (%)=100%-oil content A (%)-liquid water content (%);
Main decomposable asymmetric choice net solid content is analyzed:
A, get greasy filth sample 5g ~ 10g in 600 DEG C calcining ashing obtain residual mud;
Filter residue in b, the residual mud above-mentioned calcining ashing obtained and step (1) carries out XRD phenetic analysis respectively;
C, XRD characterization result in conjunction with two kinds of materials in b, analyze the main decomposable asymmetric choice net material composition of solid content.
In such scheme, the water containing 2mL ~ 5mL in filtrate collected in step (1) a, solvent benzol and the oil be dissolved in benzene.
As preferably, in step (1) use H
2sO
4volumetric concentration be 50%.
Compared with prior art, the invention has the advantages that:
1) in prior art, generally being insoluble to low molecule (C5 ~ C in oil
7) n-alkane but the material that can be dissolved in hot benzene is called bituminous matter, low molecule (C can be dissolved in
5~ C
7) material of n-alkane is called solvend, solvend comprises stable hydrocarbon, aromatic hydrocarbon and colloid; General heavy crude forms available Four composition and represents, i.e. stable hydrocarbon, aromatic hydrocarbon, resin and asphalt, and bituminous matter is most important component in aging greasy filth, is the key factor affecting oil-sludge treatment technology.Hot benzene extraction of the present invention can extract petroleum components all in greasy filth, and sherwood oil mainly low molecule (C conventional in prior art
5~ C
7) alkane, petroleum ether extract mainly extracts stable hydrocarbon, aromatic hydrocarbon and colloid in greasy filth, therefore causes the oil content measured by petroleum ether extraction on the low side, and hot benzene extraction gravimetric method of the present invention then can record oil content numerical value more accurately;
2) by being combined with petroleum ether extraction gravimetric method by hot benzene extraction gravimetric method, thus solvend and bitum component in oil content constituent is determined, so that determine oil-sludge treatment route more targetedly;
3) the present invention is when analyzing main decomposable asymmetric choice net solid content, calcining ashing gravimetric method is combined with hot benzene extraction gravimetric method, XRD phenetic analysis is carried out to the material after its process, and the main decomposable asymmetric choice net material composition of chemistry analysis solid content of the result characterized according to XRD and compound itself.
Accompanying drawing explanation
Fig. 1 is the thermal gravimetric analysis curve figure of greasy filth in the embodiment of the present invention;
Fig. 2 is the XRD spectra calcining the residual mud of ashing gained and this extraction of heat filter residue in the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
At the bottom of the tank of the present embodiment, the composition content analysis method of aging greasy filth comprises the following steps:
(1) oil content and the composition measurement of major oil content:
Oil content measures:
A, get greasy filth sample 10g in the cucurbit of 100mL, add benzene 20mL, then add the H that volumetric concentration is 50%
2sO
45mL, reflux at 80 DEG C 30min, leaves standstill and be cooled to room temperature, filters, and collects filtrate;
B, filter residue is joined in the cucurbit of 100mL, add benzene 20mL, then add the H that volumetric concentration is 50%
2sO
45mL, reflux at 80 DEG C 30min, leaves standstill and be cooled to room temperature, filters, and collects filtrate;
C, by the mixing of the filtrate of above-mentioned collection and stratification, collect upper strata solvent phase, by this solvent evaporative removal solvent benzol at 80 DEG C, then at 105 DEG C, be dried to constant weight, obtain oily weight;
Oil content A: oil content A (%)=(oil weight/greasy filth sampling amount) × 100% of d, calculating greasy filth;
Oil content Principle components analysis:
A, utilize the oil content B (%) of petroleum ether extraction gravimetric determination greasy filth;
In b, oil content, the total content of stable hydrocarbon, aromatic hydrocarbon and colloid is oil content B (%), and the content of oil content studies on asphaltene is:
Asphalt content (%)=oil content A (%)-oil content B (%);
(2) Water content determination:
Measure dry greasy filth sample at the thermal gravimetric analysis curve of 110 DEG C, calculate the liquid water content (%) of greasy filth according to fluid loss; As shown in Figure 1, the boiling point due to water under normal pressure is 100 DEG C, so according to the weight-loss curve of dry sample, can record the water cut of sample at 110 DEG C, and greasy filth starts weightless at 200 DEG C, and therefore the mensuration of above-mentioned liquid water content does not affect the mensuration of oil content; Can find out according to Fig. 1, maximum weightlessness mainly concentrates between 350 DEG C ~ 500 DEG C, and greasy filth quality remain unchanged substantially after 600 DEG C, therefore in the present embodiment when utilizing calcining ash purification determining oil content and solid content, calcining heat is 600 DEG C;
(3) solid content and main decomposable asymmetric choice net solid content are analyzed:
Solid content (%)=100%-oil content (%)-liquid water content (%);
Main decomposable asymmetric choice net solid content is analyzed:
A, get greasy filth sample 10g in 600 DEG C calcining ashing obtain residual mud;
Filter residue in b, the residual mud above-mentioned calcining ashing obtained and step (1) carries out XRD phenetic analysis respectively;
C, XRD characterization result in conjunction with two kinds of materials in b, analyze the main decomposable asymmetric choice net material composition inferring solid content.
Petroleum ether extraction gravimetric method, hot benzene extraction gravimetric method and the oil content analysis result of calcining ashing gravimetric method to greasy filth are as shown in table 1:
Table 1
As shown in Table 1, the oil content data difference of three kinds of analytical approachs is comparatively large, and petroleum ether extraction gravimetric method is 19.8%, hot benzene extraction gravimetric method is 25.6%, ashing gravimetric method is 37.1%.Generally being insoluble to low molecule (C in oil
5~ C
7) n-alkane but the material that can be dissolved in hot benzene is called bituminous matter, benzene can be dissolved in and can be dissolved in low molecule (C again
5~ C
7) material of n-alkane is called solvend, solvend comprises saturated point, fragrance point and colloid.Oil Four composition is stable hydrocarbon, aromatic hydrocarbon, resin and asphalt, and bituminous matter is component the heaviest in oil, and therefore, hot benzene [soluble can extract oil all in greasy filth; Sherwood oil is low molecule (C mainly
5~ C
7) alkane, petroleum ether extract can think stable hydrocarbon, aromatic hydrocarbon and colloid in main extraction greasy filth.Therefore herein the oil content of greasy filth sample is 25.6%, stable hydrocarbon wherein, aromatic hydrocarbon and colloid account for altogether greasy filth content 19.8%, bituminous matter accounts for 5.8% of greasy filth content, namely oily studies on asphaltene content is 22.6%.
Usually, in greasy filth, oil content consists of the stable hydrocarbon of 40% ~ 52%, aromatic hydrocarbon, the colloid of 7% ~ 22.4%, the bituminous matter of 8% ~ 10% of 28% ~ 31%, China's From Liaohe Heavy Crude is filled with clearly in the Four composition of greasy filth recovered oil, bituminous matter accounts for 11.01%, and the asphalt content of the present embodiment greasy filth oil is approximately 2 ~ 4 times of other greasy filth oil, content is higher, supposition may be that greasy filth is aging in drying bed, in greasy filth oil some heavy constituent be converted into bituminous matter or some light constituent volatilization loss make the asphalt content of greasy filth oil higher caused by.
Because some inorganics in greasy filth just starts 400 DEG C time to decompose, as shown in Figure 2, as can be seen from a spectrogram in Fig. 2, hot benzene extracts in residual mud exists moisture mineral compound, i.e. Fe (OH) OH
2o, as can be seen from b spectrogram in Fig. 2,600 DEG C of residual mud of calcining are then obviously containing anhydrous oxide Fe
2o
3, in greasy filth, a large amount of ferro element may be mainly derived from crude oil and store transportation equipment, moisture mineral compound Fe (OH) OH in greasy filth
2o can decompose weightlessness and be converted into oxide Fe at 600 DEG C
2o
3, visible, containing Fe (OH) OH in the principal ingredient of greasy filth solid content
2o.
The greasy filth that the present embodiment is selected is before treatment in the glossy black look of bonding shape, after 600 DEG C of calcining ashing, residual mud loosens, in rust, shows the high temperature ashing oil eliminating black of greasy filth, there is the iron oxide of a large amount of rust in ashing product, it can thus be appreciated that, the main cause one of greasy filth calcining ashing weightlessness is greasy filth petroleum oxidation burning weight loss, and two is that fraction solids inorganics decomposes weightlessness, so, associative list 1, the solid inorganic thing that can decompose at 600 DEG C in greasy filth is:
Weight loss (%)=hot benzene extraction gravimetric method gained solid content (%)-calcining ashing gravimetric method gained solid content (%)=64.6%-53.1%=11.5% can be decomposed at 600 DEG C in greasy filth.
To sum up analyze known, the greasy filth selected by the present embodiment consists of liquid water content 9.8%, oil content 25.6% (its studies on asphaltene accounts for 22.6% of greasy filth oil), solid content 64.6% (wherein main decomposable solid content is 11.5% below 600 DEG C).
Claims (3)
1. a composition content analysis method for aging greasy filth at the bottom of tank, is characterized in that comprising the following steps:
(1) oil content and the composition measurement of major oil content:
Oil content measures:
A, get greasy filth sample 5g ~ 10g in the cucurbit of 50mL ~ 100mL, add benzene 15mL ~ 25mL, then add the H that volumetric concentration is 40% ~ 60%
2sO
42mL ~ 5mL, reflux at 80 DEG C 25min ~ 40min, leaves standstill and be cooled to room temperature, filters, and collects filtrate;
B, filter residue is joined in the cucurbit of 50mL ~ 100mL, add benzene 15mL ~ 25mL, then add the H that volumetric concentration is 40% ~ 60%
2sO
42mL ~ 5mL, reflux at 80 DEG C 25min ~ 40min, leaves standstill and be cooled to room temperature, filters, and collects filtrate;
C, by the mixing of the filtrate of above-mentioned collection and stratification, collect upper strata solvent phase, by this solvent evaporative removal solvent benzol at 80 DEG C, then at 105 DEG C, be dried to constant weight, obtain oily weight;
Oil content A: oil content A (%)=(oil weight/greasy filth sampling amount) × 100% of d, calculating greasy filth;
Oil content Principle components analysis:
A, utilize the oil content B (%) of petroleum ether extraction gravimetric determination greasy filth;
In b, oil content, the total content of stable hydrocarbon, aromatic hydrocarbon and colloid is oil content B (%), and the content of oil content studies on asphaltene is:
Asphalt content (%)=oil content A (%)-oil content B (%);
(2) Water content determination:
Measure dry greasy filth sample at the thermal gravimetric analysis curve of 110 DEG C, calculate the liquid water content (%) of greasy filth according to fluid loss;
(3) solid content and main decomposable asymmetric choice net solid content are analyzed:
Solid content (%)=100%-oil content (%)-liquid water content (%);
Main decomposable asymmetric choice net solid content is analyzed:
A, get greasy filth sample 5g ~ 10g in 600 DEG C calcining ashing obtain residual mud;
Filter residue in b, the residual mud above-mentioned calcining ashing obtained and step (1) carries out XRD phenetic analysis respectively;
C, XRD characterization result in conjunction with two kinds of materials in b, analyze the main decomposable asymmetric choice net material composition inferring solid content.
2. the composition content analysis method of aging greasy filth at the bottom of tank according to claim 1, is characterized in that: the water containing 2mL ~ 5mL in filtrate collected in step (1) a, solvent benzol and the oil be dissolved in benzene.
3. the composition content analysis method of aging greasy filth at the bottom of tank according to claim 1, is characterized in that: in step (1) use H
2sO
4volumetric concentration be 50%.
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Cited By (6)
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| CN105895885A (en) * | 2016-06-17 | 2016-08-24 | 上海应用技术学院 | Method for preparing cobalt ferrite-graphene lithium ion battery by using steel rolling oil sludge |
| CN108051392A (en) * | 2017-11-30 | 2018-05-18 | 广东电网有限责任公司电力科学研究院 | A kind of detection method of transformer greasy filth aging composition |
| CN109632989A (en) * | 2018-12-18 | 2019-04-16 | 陕西延长石油（集团）有限责任公司 | A kind of four compound mensuration device and method of heavy oil of high throughput |
| CN109725022A (en) * | 2018-12-27 | 2019-05-07 | 湖南科技大学 | A kind of method for fast measuring of combination water content |
| CN112557250A (en) * | 2020-12-29 | 2021-03-26 | 天津市生态环境监测中心 | Gravimetric method for measuring petroleum and animal and vegetable oils in high-concentration wastewater |
| CN113092612A (en) * | 2021-03-31 | 2021-07-09 | 武汉钢铁有限公司 | Method for detecting oil content in cold rolling oil sludge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112557250A (en) * | 2020-12-29 | 2021-03-26 | 天津市生态环境监测中心 | Gravimetric method for measuring petroleum and animal and vegetable oils in high-concentration wastewater |
| CN113092612A (en) * | 2021-03-31 | 2021-07-09 | 武汉钢铁有限公司 | Method for detecting oil content in cold rolling oil sludge |
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Application publication date: 20160127 |