CN100357356C - Low fluorescence and sinking-proof type asphalt and its prodn. method - Google Patents
Low fluorescence and sinking-proof type asphalt and its prodn. method Download PDFInfo
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- CN100357356C CN100357356C CNB2006100313035A CN200610031303A CN100357356C CN 100357356 C CN100357356 C CN 100357356C CN B2006100313035 A CNB2006100313035 A CN B2006100313035A CN 200610031303 A CN200610031303 A CN 200610031303A CN 100357356 C CN100357356 C CN 100357356C
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Abstract
The present invention discloses low fluorescence collapse preventing asphalt and a manufacturing method thereof. The low fluorescence collapse preventing asphalt is composed of petroleum asphalt, solvent oil, liquid sulfur trioxide, chlorosulfonic acid, nitric acid and sodium hydroxide. The petroleum asphalt, the solvent oil of which the weight is 100 to 300% of that of the petroleum asphalt, the liquid sulfur trioxide of which the weight is 20 to 90% of that of the petroleum asphalt, the sulfur trioxide of which the weight is 20 to 90% of that of the petroleum asphalt, the chlorosulfonic acid of which the weight is 20 to 90% of that of the petroleum asphalt, the nitric acid of which the weight is 20 to 90% of that of the petroleum asphalt, and the sodium hydroxide of which the weight is 50 to 150% of that of the petroleum asphalt are added into a reaction vessel under the pressure lower than 0.1MPa and at the temperature of 20 to 80 DEG C, and finally, the mixture is dried and ground. The petroleum asphalt is treated by acid for a plurality of times in sulfonation reaction, so that the collapse preventing asphalt not only has a low fluorescent grade, but also has a high content of water soluble and oil soluble substances and a low filter loss of drilling fluid, and the collapse preventing asphalt can not generate fluorescent interference and can rapidly and accurately identify and find new oil and gas layers. Besides, the present invention can enhance the capacity of blocking cracks of a well wall, improve the rheological property of mud fluid of drilling fluid, inhibit the dispersion and the expansion of shale, prevent well wall collapse and enhance the stability of a well wall. The present invention is widely suitable for petroleum well drilling, natural gas well drilling, geological well drilling and exploratory well drilling.
Description
Technical field
The present invention relates to the anti-collapse treatment agent that uses in oil, the Sweet natural gas probing Development Engineering, especially a kind of not only fluorescence grade is low, and good low fluorescence and sinking-proof type asphalt and the manufacture method thereof of integrated performance index.
Background technology
For a long time, hole instability, especially the mud shale stratum borehole instability problems is often run in the oil gas drilling Development Engineering one a very complicated technology problem, and according to the pertinent data introduction, world's oil and gas industry is used to handle accident cost that hole instability causes every year up to 700,000,000 dollars.In recent years, China had carried out systematic research to solving this technical problem of hole instability, comprised research and development and improvement to caving-preventing drilling fluid system and treatment agent thereof, had obtained some achievements, and down-hole accident is constantly reduced, and economic benefit improves rapidly.The anti-collapse treatment agent of petroleum pitch class (claiming shale control agent again) wherein, since have aboundresources and preferably shutoff borehole wall crack ability with can reduce drilling fluid filtration, can improve the characteristics of borehole wall stability, at home and abroad obtain in the oil gas drilling Development Engineering using widely.Because the residual fluorescence grade of petroleum pitch itself is greater than 15 grades, after handling through oversulfonate, though can make in the water-soluble base drilling fluid of petroleum pitch, reach anti-collapse shutoff retaining wall effect, but the fluorescence grade of this common petroleum sulfonated gilsonite and hydrocarbon-bearing pool layer fluorescence grade difference are very little after the sulfonation, easy and hydrocarbon-bearing pool layer fluorescence produces to be obscured, fluorescence interference takes place, to finding new hydrocarbon-bearing pool layer generation erroneous judgement or failing to judge, in the oil gas drilling construction, use and be restricted, therefore, common petroleum sulfonation sinking-proof type asphalt must carry out some art breading, just can make its fluorescence grade less than below 5 grades, also make it have high water and oily molten thing content and low drilling fluid filtration simultaneously, to improve its integrated performance index.Thereby not only can reduce to survey the well logging fluorescence interference, avoid finding new reservoir layer generation erroneous judgement or failing to judge; And can improve anti-collapse shutoff retaining wall action effect, guarantee borehole wall stability.Though the art treatment to the common petroleum sulfonated gilsonite has multiple at present, but common petroleum sulfonation sinking-proof type asphalt is after carrying out art breading, all also have following problems at present: the common sulfonation sinking-proof type asphalt fluorescence grade after handling is less than below 5 grades the time, water and oily molten thing content are lower, or drilling fluid filtration is big, can not reach technical requirements, its shutoff crack, the performance that prevents to cave in are bad; Dang Shui and oily molten thing content height, drilling fluid filtration is little, shutoff crack, when the performance that prevents to cave in is good, the common sulfonation sinking-proof type asphalt fluorescence grade after it is handled is but greater than 5 grades.KT-1 sulfonated gilsonite as the production of the 7th chemical plant, Xinxiang City, Henan, the FH-1 sulfonated gilsonite that KTU-18 sulfonated gilsonite that the chemical company limited of the triumphant Thailand in Chengdu produces and Xinjiang Bei Ken Development Co., Ltd produce, its water solubles content height, filter loss is little, but their fluorescence grade is all greater than 5 grades, and the oily molten thing content of the FH-1 sulfonated gilsonite of Xinjiang production also is lower than technical requirements; And HFT-102 that Henan Renqiu City all places chemical industry company limited and Henan, Zhengzhou China auxiliary agent company limited produce and DSA-2 sulfonated gilsonite fluorescence grade are less than 5 grades, but their oily molten thing or water solubles index are lower than technical requirements again, thereby influence anti sloughing effectiveness and reduce fluid loss performance, therefore, its over-all properties of oil sulfonation sinking-proof type asphalt as in the drilling fluid system of using at present is bad.
Technology contents
In above-mentioned present prior art, the bad problem of over-all properties of oil sulfonation sinking-proof type asphalt, the invention provides and a kind ofly not only have lower fluorescence grade, and have water again and oily molten thing content is high and drilling fluid filtration is little, the low fluorescence and sinking-proof type asphalt that its integrated performance index is good.
The technical scheme that the technical problem to be solved in the present invention is taked is: described low fluorescence and sinking-proof type asphalt, it is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on is that the 100-300%, the 20-90% that the liquid sulphur trioxide add-on is petroleum pitch, the 20-90% that the chlorsulfonic acid add-on is petroleum pitch, 20-90%, the caustic soda add-on that the nitric acid add-on is petroleum pitch of petroleum pitch is the 50-150% of petroleum pitch.
The present invention compares with the oil sulfonation sinking-proof type asphalt after the existing art breading, its innovation part is: replace originally using the vitriol oil with liquid sulphur trioxide earlier, S-WAT and oleum carry out sulfonation, to improve its sulfonation effect, reduce the caustic soda consumption of the residual acid of neutralization, most critical is in liquid sulphur trioxide sulfonation treating processes, add chlorsulfonic acid and nitric acid and produce concerted reaction, carry out the polyacid art breading, thereby can not only reduce the fluorescence grade of oil sulfonated gilsonite greatly, and can improve Qi Shui and oily molten thing content, improve anti sloughing effectiveness, reduce drilling fluid filtration, improved its over-all properties.
Described solvent oil is that boiling range is 60-90 ℃, and label is 10-16 number a low melting point industry solvent for extraction (GB1922-88), and described chlorsulfonic acid (molecular formula HSO3CL, GB13549-92) content is 97%, and nitric acid is concentrated nitric acid, and liquid sulphur trioxide content is 99%.
Low fluorescence and sinking-proof type asphalt of the present invention forms mechanism: petroleum pitch is the byproduct of refining oil, by multiple hydrocarbon polymer and nonmetal the composition, its composition mainly is carbon (80-87%) and hydrogen (10-15%), its chemical combination structure is the highly condensed cycloalkanes and the aromatic nucleus of band alkane side chain, promptly by paraffinic hydrocarbons, naphthenic hydrocarbon and aromatic hydrocarbon three classes are formed, after petroleum pitch melts, feed liquid sulphur trioxide, sulfonation reaction takes place, sulphur trioxide progressively is grafted on the side chain, make water-fast petroleum pitch have high (greater than more than 90%) water and oily molten thing content, improved the sulfonation effect, reduced the caustic soda consumption of the residual acid that neutralizes, thereby can be used for a large amount of at present water base brill and liquid that use, and in sulfonation reaction, add chlorsulfonic acid and nitric acid and carry out polyacid and handle, make chlorsulfonic acid and nitric acid produce concerted reaction, not only can reduce the fluorescence grade of petroleum pitch greatly, make its fluorescence grade less than 5 grades, be generally the 2-3 level, and can improve the molten thing content of water oil, make its water, the molten thing content of oil and can reduce drilling fluid filtration (filter loss is less than 25ml) respectively greater than 75% and 15%, improves drilling fluid filtration reduced rate (reduced rate is greater than more than 40%).
The manufacture method step of low fluorescence and sinking-proof type asphalt of the present invention is:
1, in reactor, add quantitative petroleum pitch, add the 10-16 solvent oil of the 100-300% of its petroleum pitch weight again, be heated to 20-60 ℃,
2, adding the liquid sulphur trioxide of the 20-90% of petroleum pitch weight again in reactor, is 20-80 ℃ in temperature, and pressure kept 3-15 hour less than under the 0.1MPa,
3, adding the chlorsulfonic acid of the 20-90% of petroleum pitch weight again in reactor, is 20-70 ℃ in temperature, and pressure kept 2-12 hour less than under the 0.05MPa,
4, adding the concentrated nitric acid of the 20-90% of petroleum pitch weight again in reactor, is 20-80 ℃ in temperature, and pressure kept 2-10 hour less than under the 0.05MPa,
5, the last caustic soda that adds the 50-150% of petroleum pitch weight again in reactor is 30-80 ℃ in temperature, and pressure carries out neutralization reaction less than under the 0.05MPa, kept 3-8 hour,
6, the solvent oil in the cleaning reaction still is sent into reaction product in the roller dryer of vapor source heating,
7, after the drying, sending into and being ground into granularity in the raymond mill is 80 order meals, the packing warehouse-in.
Low fluorescence and sinking-proof type asphalt of the present invention after testing, its every technical indicator scope is:
PH value: 8-9 water solubles content %: 〉=75
Moisture content % :≤12 oily molten thing content %: 〉=15
Fluorescence grade :≤5 grades of high temperature and high pre ssure filtration reduced rate %: 〉=40
Low fluorescence and sinking-proof type asphalt of the present invention, because petroleum pitch is carrying out having added chlorsulfonic acid and nitric acid in the sulfonation reaction with liquid sulphur trioxide, carried out multiple sour concerted reaction, thereby make sinking-proof type asphalt not only have lower fluorescence grade, and has the molten thing content of high water oil, low drilling fluid filtration, not only can guarantee in drilling process, can not produce hydrocarbon-bearing pool layer fluorescence interference, solved finding that new hydrocarbon-bearing pool layer produces the erroneous judgement or the problem of failing to judge, and can quick and precisely discern and find new oil reservoir; And can improve shutoff borehole wall crack ability, and improve the drilling fluid rheology and the mud cake quality of drilling fluid, reduce and degrade piece, suppressing shale disperses to expand, prevent slump in, improved borehole wall stability, be widely used in oil, Sweet natural gas, geological drilling and prospect drilling.
Embodiment
Embodiment 1, described low fluorescence and sinking-proof type asphalt is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on be petroleum pitch 200%, the liquid sulphur trioxide add-on be petroleum pitch 50%, the chlorsulfonic acid add-on be petroleum pitch 50%, the concentrated nitric acid add-on be petroleum pitch 50%, the caustic soda add-on is 100% of petroleum pitch.Be made as follows that method steps is formulated:
1, in reactor, add quantitative petroleum pitch, add solvent oil more according to the above ratio No. 10, be heated to 40 ℃,
2, adding liquid sulphur trioxide more according to the above ratio in reactor, is 50 ℃ in temperature, and pressure kept 8 hours less than under the 0.1MPa,
3, adding chlorsulfonic acid more according to the above ratio in reactor, is 45 ℃ in temperature, and pressure kept 7 hours less than under the 0.05MPa,
4, adding concentrated nitric acid more according to the above ratio in reactor, is 50 ℃ in temperature, and pressure kept 6 hours less than under the 0.05Mpa,
5, adding caustic soda more according to the above ratio in reactor, is 60 ℃ in temperature, and pressure is less than under the 0.05MPa, carries out neutralization reaction, kept 5 hours,
6, the solvent oil in the cleaning reaction still is sent into reaction product in the roller dryer of vapor source heating,
7, after the drying, sending into and being ground into granularity in the raymond mill is 80 order meals, the packing warehouse-in.
Present embodiment 1, described low fluorescence and sinking-proof type asphalt after testing, its every technical indicator is:
PH value: 8 water solubles content %:77
The molten thing content %:19 of moisture content %:5.52 oil
Fluorescence grade: 3 grades of high temperature and high pre ssure filtration reduced rate %:45.5
Embodiment 2, described low fluorescence and sinking-proof type asphalt is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on be petroleum pitch 100%, the liquid sulphur trioxide add-on be petroleum pitch 20%, the chlorsulfonic acid add-on be petroleum pitch 90%, the concentrated nitric acid add-on be petroleum pitch 90%, the caustic soda add-on is 50% of petroleum pitch.Formulated by following method steps:
1, in reactor, add quantitative petroleum pitch, add solvent oil more according to the above ratio No. 16, be heated to 20 ℃,
2, adding liquid sulphur trioxide more according to the above ratio in reactor, is 20 ℃ in temperature, and pressure kept 4 hours less than under the 0.1MPa,
3, adding chlorsulfonic acid more according to the above ratio in reactor, is 30 ℃ in temperature, and pressure kept 2 hours less than under the 0.05MPa,
4, adding concentrated nitric acid more according to the above ratio in reactor, is 80 ℃ in temperature, and pressure kept 10 hours less than under the 0.05Mpa,
5, adding caustic soda more according to the above ratio in reactor, is 30 ℃ in temperature, and pressure is less than under the 0.05MPa, carries out neutralization reaction, kept 3 hours,
6, the solvent oil in the cleaning reaction still is sent into reaction product in the roller dryer of vapor source heating,
7, after the drying, sending into and being ground into granularity in the raymond mill is 80 order meals, the packing warehouse-in.
Present embodiment 2 described low fluorescence and sinking-proof type asphalts after testing, its every technical indicator is:
PH value: 8.5 water solubles content %:82.2
The molten thing content %:16.5 of moisture content %:7.8 oil
Fluorescence grade: 2.5 grades of high temperature and high pre ssure filtration reduced rate %:44
Embodiment 3, described low fluorescence and sinking-proof type asphalt is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on be petroleum pitch 300%, the liquid sulphur trioxide add-on be petroleum pitch 90%, the chlorsulfonic acid add-on be petroleum pitch 20%, the concentrated nitric acid add-on be petroleum pitch 20%, the caustic soda add-on is 150% of petroleum pitch.Formulated by following manufacture method step:
1, in reactor, add quantitative petroleum pitch, add solvent oil more according to the above ratio No. 12, be heated to 60 ℃,
2, adding liquid sulphur trioxide more according to the above ratio in reactor, is 80 ℃ in temperature, and pressure kept 15 hours less than under the 0.1MPa,
3, adding chlorsulfonic acid more according to the above ratio in reactor, is 70 ℃ in temperature, and pressure kept 12 hours less than under the 0.054MPa,
4, adding concentrated nitric acid more according to the above ratio in reactor, is 20 ℃ in temperature, and pressure kept 2 hours less than under the 0.05Mpa,
5, adding caustic soda more according to the above ratio in reactor, is 80 ℃ in temperature, and pressure is less than under the 0.05MPa, carries out neutralization reaction, kept 8 hours,
6, the solvent oil in the cleaning reaction still is sent into reaction product in the roller dryer of vapor source heating,
7, after the drying, sending into and being ground into granularity in the raymond mill is 80 order meals, the packing warehouse-in.
Present embodiment 3 described low fluorescence and sinking-proof type asphalts after testing, its every technical indicator is:
PH value: 8.2 water solubles content %:76
The molten thing content %:20.8 of moisture content %:8 oil
Fluorescence grade: 3 grades of high temperature and high pre ssure filtration reduced rate %:41
Claims (5)
1, a kind of low fluorescence and sinking-proof type asphalt, it is characterized in that: it is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on is that the 100-300%, the 20-90% that the liquid sulphur trioxide add-on is petroleum pitch, the 20-90% that the chlorsulfonic acid add-on is petroleum pitch, 20-90%, the caustic soda add-on that the nitric acid add-on is petroleum pitch of petroleum pitch is the 50-150% of petroleum pitch.
2, a kind of low fluorescence and sinking-proof type asphalt according to claim 1, it is characterized in that: it is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on be petroleum pitch 200%, the liquid sulphur trioxide add-on be petroleum pitch 50%, the chlorsulfonic acid add-on be petroleum pitch 50%, the nitric acid add-on be petroleum pitch 50%, the caustic soda add-on is 100% of petroleum pitch.
3, a kind of low fluorescence and sinking-proof type asphalt according to claim 1, it is characterized in that: it is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on be petroleum pitch 100%, the liquid sulphur trioxide add-on be petroleum pitch 20%, the chlorsulfonic acid add-on be petroleum pitch 90%, the nitric acid add-on be petroleum pitch 90%, the caustic soda add-on is 50% of petroleum pitch.
4, a kind of low fluorescence and sinking-proof type asphalt according to claim 1, it is characterized in that: it is made up of petroleum pitch, solvent oil, liquid sulphur trioxide, chlorsulfonic acid, nitric acid and caustic soda, and the weight ratio of each component is: the solvent oil add-on be petroleum pitch 300%, the liquid sulphur trioxide add-on be petroleum pitch 90%, the chlorsulfonic acid add-on be petroleum pitch 20%, the nitric acid add-on be petroleum pitch 20%, the caustic soda add-on is 150% of petroleum pitch.
5, a kind of method of making the described low fluorescence and sinking-proof type asphalt of claim 1 is characterized in that being made as follows that method steps carries out:
(1), in reactor, add quantitative petroleum pitch, add the 10-16 solvent oil of the 100-300% of its petroleum pitch weight again, be heated to 20-60 ℃,
(2), again adding the liquid sulphur trioxide of the 20-90% of petroleum pitch weight in reactor, is 20-80 ℃ in temperature, and pressure kept 3-15 hour less than under the 0.1MPa,
(3), again adding the 20-90% chlorsulfonic acid of petroleum pitch weight in reactor, is 20-70 ℃ in temperature, and pressure kept 2-12 hour less than under the 0.05MPa,
(4), again adding the concentrated nitric acid of the 20-90% of petroleum pitch weight in reactor, is 20-80 ℃ in temperature, and pressure kept 2-10 hour less than under the 0.05MPa,
(5), again adding the caustic soda of the 50-150% of petroleum pitch weight in reactor, is 30-80 ℃ in temperature, and pressure is less than under the 0.05MPa, carries out neutralization reaction, kept 3-8 hour,
(6), the solvent oil in the cleaning reaction still, reaction product is sent in the roller dryer of vapor source heating,
(7), after the drying, sending into and being ground into granularity in the raymond mill is 80 order meals, the packing warehouse-in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100313035A CN100357356C (en) | 2006-03-06 | 2006-03-06 | Low fluorescence and sinking-proof type asphalt and its prodn. method |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100313035A CN100357356C (en) | 2006-03-06 | 2006-03-06 | Low fluorescence and sinking-proof type asphalt and its prodn. method |
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| CN1831042A CN1831042A (en) | 2006-09-13 |
| CN100357356C true CN100357356C (en) | 2007-12-26 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733525B (en) * | 2016-03-15 | 2018-05-08 | 萍乡市汇鑫化工科技有限公司 | The molten sulfonated gilsonite of drilling fluid peracid |
| CN115772390B (en) * | 2022-12-02 | 2023-09-08 | 湖北龙海化工有限公司 | Low-fluorescence blocking anti-collapse asphalt for drilling fluid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60238129A (en) * | 1984-05-14 | 1985-11-27 | Fuji Sekiyu Kk | Surface active substance and preparation thereof |
| CN1037916A (en) * | 1988-05-26 | 1989-12-13 | 石油工业部石油勘探开发科学研究院钻井工艺研究所 | The preparation technology of sulfonated asphalt treating agent of drilling mud |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60238129A (en) * | 1984-05-14 | 1985-11-27 | Fuji Sekiyu Kk | Surface active substance and preparation thereof |
| CN1037916A (en) * | 1988-05-26 | 1989-12-13 | 石油工业部石油勘探开发科学研究院钻井工艺研究所 | The preparation technology of sulfonated asphalt treating agent of drilling mud |
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