CN103554126B - The fluorescein derivative preparation method of oil field tracer agent and application - Google Patents
The fluorescein derivative preparation method of oil field tracer agent and application Download PDFInfo
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- CN103554126B CN103554126B CN201310571034.1A CN201310571034A CN103554126B CN 103554126 B CN103554126 B CN 103554126B CN 201310571034 A CN201310571034 A CN 201310571034A CN 103554126 B CN103554126 B CN 103554126B
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- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical class O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 239000000700 radioactive tracer Substances 0.000 title claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 52
- 239000003513 alkali Substances 0.000 claims abstract description 29
- -1 benzaldehyde compound Chemical class 0.000 claims abstract description 29
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzenecarboxaldehyde Natural products O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 29
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 150000003839 salts Chemical class 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 29
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000004090 dissolution Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000010992 reflux Methods 0.000 claims abstract description 15
- 230000000630 rising effect Effects 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims description 38
- 238000006243 chemical reaction Methods 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 10
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 10
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 10
- 239000008399 tap water Substances 0.000 claims description 10
- 235000020679 tap water Nutrition 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- 230000003203 everyday effect Effects 0.000 claims description 8
- 238000005558 fluorometry Methods 0.000 claims description 8
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 claims description 6
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- 229920002866 paraformaldehyde Polymers 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 235000015320 potassium carbonate Nutrition 0.000 claims description 4
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 4
- 235000019252 potassium sulphite Nutrition 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000008098 formaldehyde solution Substances 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000003921 oil Substances 0.000 abstract description 25
- 238000000034 method Methods 0.000 abstract description 5
- 239000005864 Sulphur Substances 0.000 abstract description 4
- 239000010779 crude oil Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000011435 rock Substances 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/10—Spiro-condensed systems
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B47/00—Survey of boreholes or wells
- E21B47/10—Locating fluid leaks, intrusions or movements
- E21B47/11—Locating fluid leaks, intrusions or movements using tracers; using radioactivity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mining & Mineral Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Fluid Mechanics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geophysics (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The fluorescein derivative preparation method of oil field tracer agent and application, fluorescein first adds in reactor by preparation method, add dissolution with solvents, alkali is added under stirring, then add with fluorescein containing benzaldehyde compound and sulphite, temperature rising reflux, again reactor is cooled to room temperature, boil off solvent, add salt, mixed grinding, namely the fluorescein derivative of oil field tracer agent is obtained, during use, this fluorescein derivative is mixed with solution, treating that well logging is injected, gather water sample and carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative, because fluorescein adds sulphur methyl after above-mentioned process, enhance it water-soluble, reduce its solubleness in crude oil, sulphur methyl has been full-ionized group simultaneously, with strong electronegativity, produces strong electrostatic repulsion, greatly reduce the absorption consumption of fluorescein on stratum, can reduce the consumption as tracer agent thus with aquation rock target negative charge in stratum.
Description
Technical field
The present invention relates to the fluorescein derivative technical field of oil field tracer agent, be specifically related to fluorescein derivative preparation method and the application of oil field tracer agent.
Background technology
Oil-field flooding tracer technique is one of situ production measuring technology, its technology injects tracer agent from Injection Well, thereafter be defined in withdrawal well sampling around by certain sampling, monitor its tracer agent over time, the design of oil mining and the adjustment of latter period of oilfield development can be instructed.Due to the restriction by reservoir media, tracer agent must meet the requirement of chemical stability, physical stability and biologically stable three aspects.For a long time, tracer agent the most frequently used in oil-field development mainly contains chemical tracer and isotopic tracer, although these tracer techniques are widely used in each oil field, also there is shortcoming in various degree.
Fluorescent tracer technique has been used widely in fields such as medical science, biology and water treatments, and fluorescent substance is as the application of oil field tracer, the novelty teabag particularly will being fluorescent substance application in well-to-well test ground water movement direction, oil field and reservoir heterogeneity etc.The material that can produce fluorescence is more, mostly is some organic compound, carries out quick, easy, highly sensitive detection, can reach the object of spike by spectrophotofluorometer with regard to it.Fluorescein is the most frequently used fluorescent reagent, and fluorescence efficiency is high.Under optimal conditions, the linearity range detected fluorescein is 1 × 10
-8~ 1 × 10
-10mol/L, detects and is limited to 7.5 × 10
-11mol/L, emission wavelength is comparatively strong in 500-500 nanometer range, differs greatly, not easily cause interference with fluorescent components in crude oil.But because fluorescein itself has hydroxyl, carboxyl etc. on the one hand in order to form the functional group of hydrogen bond and to be easily dissolved in the aromatic ring of crude oil, therefore there is stratum absorption and consume larger, water-soluble shortcoming on the weak side.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide fluorescein derivative preparation method and the application of oil field tracer agent, resulting product good water solubility, stability are adsorbed on stratum by force, not easily, are suitable for practical application.
In order to achieve the above object, the technical solution used in the present invention is:
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 10-100 times quality, and described solvent is the water of technical grade and above purity, methyl alcohol, ethanol and mixed solution thereof;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1-2.5, described alkali is the sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, salt of wormwood, Trimethylamine 99, triethylamine, pyridine and composition thereof of technical grade and above purity;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1-3:1 for 1-4:1, temperature rising reflux 2-6 hour, described is the formaldehyde solution, trioxymethylene, paraformaldehyde, hexamethylenetetramine and composition thereof of technical grade and above purity containing benzaldehyde compound, and sulphite is the S-WAT, potassium sulfite, ammonium sulphite and composition thereof of technical grade and above purity;
4th step, is cooled to room temperature by reactor, boils off solvent, add the salt of gained material 2-20 times of quality, more than mixed grinding to 40 order, namely obtain the fluorescein derivative of oil field tracer agent, described salt is the sodium-chlor, Repone K and composition thereof of technical grade and above purity.
During use, this fluorescein derivative is mixed with the solution of mass concentration 0.1-10mg/L, solvent for use is use by oneself water in tap water or oil field, it is being treated that well logging is injected, water sample is gathered by effect well every day subsequently possible, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Because fluorescein adds sulphur methyl after above-mentioned process, enhance that it is water-soluble, reduce its solubleness in crude oil; Sulphur methyl has been full-ionized group simultaneously, with strong electronegativity, produces strong electrostatic repulsion, greatly reduce the absorption consumption of fluorescein on stratum, can reduce the consumption as tracer agent thus with aquation rock target negative charge in stratum.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 10 times of quality, and described solvent is tap water;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1, described alkali is the sodium hydroxide of technical grade;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:1 for 1:1, temperature rising reflux 4 hours, described containing benzaldehyde compound to be concentration be 35% technical grade formalin, sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 2 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the sodium-chlor of technical grade.
During use, this fluorescein derivative is mixed with the solution of mass concentration 0.1mg/L, solvent for use is tap water, it is being treated that well logging is injected, water sample is gathered by effect well every day subsequently possible, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Embodiment 2
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 15 times of quality, and described solvent is technical grade anhydrous methanol;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1.5, described alkali is the potassium hydroxide of technical grade;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:1 for 1:1.2, temperature rising reflux 5 hours, described is technical grade paraformaldehyde containing benzaldehyde compound, and sulphite is technical grade potassium sulfite;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 5 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the Repone K of technical grade.
During use, this fluorescein derivative is mixed with the solution of mass concentration 0.2mg/L, solvent for use is tap water, it is being treated that well logging is injected, water sample is gathered by effect well every day subsequently possible, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Embodiment 3
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 20 times of quality, and described solvent is technical grade dehydrated alcohol;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:2, described alkali is the lithium hydroxide of technical grade;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:1.5 for 1:1.5, temperature rising reflux 3 hours, described is chemical pure trioxymethylene containing benzaldehyde compound, and sulphite is technical grade ammonium sulphite;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 8 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the sodium-chlor of technical grade.
During use, this fluorescein derivative is mixed with the solution of mass concentration 0.5mg/L, solvent for use is tap water, it is being treated that well logging is injected, water sample is gathered by effect well every day subsequently possible, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Embodiment 4
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 50 times of quality, and described solvent is technical grade 95# ethanol;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:2.1, described alkali is chemical pure triethylamine;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:2.1 for 1:2, temperature rising reflux 2 hours, described is technical grade vulkacit H containing benzaldehyde compound, and sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 10 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the sodium-chlor of technical grade.
During use, this fluorescein derivative is mixed with the solution of mass concentration 1mg/L, solvent for use is tap water, and it is being treated that well logging is injected, and gathers water sample every day subsequently possible by effect well, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Embodiment 5
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 80 times of quality, and described solvent is technical grade deionized water;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:2.5, described alkali is analytically pure pyridine;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:2.5 for 1:2.5, temperature rising reflux 4 hours, described is the technical grade formalin of mass concentration 30% containing benzaldehyde compound, and sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, add the salt of gained material 15 times of quality, more than mixed grinding to 40 order, namely obtain the fluorescein derivative of oil field tracer agent, described salt is mass ratio is the sodium-chlor of 1:1 technical grade and the mixture of Repone K.
During use, this fluorescein derivative is mixed with the solution of mass concentration 2mg/L, solvent for use is tap water, and it is being treated that well logging is injected, and gathers water sample every day subsequently possible by effect well, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Embodiment 6
The fluorescein derivative preparation method of oil field tracer agent, comprises the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 100 times of quality, and described solvent is technical grade deionized water;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1.8, described alkali is mass ratio is the sodium hydroxide of the technical grade of 1:1 and the mixture of salt of wormwood;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:3 for 1:3.5, temperature rising reflux 6 hours, described is chemical pure trioxymethylene containing benzaldehyde compound, and sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 20 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the Repone K of technical grade.
During use, this fluorescein derivative is mixed with the solution of mass concentration 10mg/L, solvent for use is tap water, and it is being treated that well logging is injected, and gathers water sample every day subsequently possible by effect well, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
Claims (8)
1. the fluorescein derivative preparation method of oil field tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 10-100 times quality, and described solvent is the water of technical grade and above purity, methyl alcohol, ethanol and mixed solution thereof;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1-2.5, described alkali is the sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, salt of wormwood, Trimethylamine 99, triethylamine, pyridine and composition thereof of technical grade and above purity;
3rd step, stirs in downhill reaction still and adds with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1-3:1 for 1-4:1, temperature rising reflux 2-6 hour,
describedcontaining formaldehyde solution, trioxymethylene, paraformaldehyde, hexamethylenetetramine and composition thereof that benzaldehyde compound is technical grade and above purity, sulphite is the S-WAT, potassium sulfite, ammonium sulphite and composition thereof of technical grade and above purity;
4th step, is cooled to room temperature by reactor, boils off solvent, add the salt of gained material 2-20 times of quality, more than mixed grinding to 40 order, namely obtain the fluorescein derivative of oil field tracer agent, described salt is the sodium-chlor, Repone K and composition thereof of technical grade and above purity.
2. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, it is characterized in that: solution during use, this fluorescein derivative being mixed with mass concentration 0.1-10mg/L, solvent for use is use by oneself water in tap water or oil field, it is being treated that well logging is injected, water sample is gathered by effect well every day subsequently possible, fluorometry is adopted to carry out quantitative analysis, until extraction water sample detection does not go out above-mentioned fluorescein derivative.
3. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 10 times of quality, and described solvent is tap water;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1, described alkali is the sodium hydroxide of technical grade;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:1 for 1:1, temperature rising reflux 4 hours, described containing benzaldehyde compound to be concentration be 35% technical grade formalin, sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 2 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the sodium-chlor of technical grade.
4. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 15 times of quality, and described solvent is technical grade anhydrous methanol;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1.5, described alkali is the potassium hydroxide of technical grade;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:1 for 1:1.2, temperature rising reflux 5 hours, described is technical grade paraformaldehyde containing benzaldehyde compound, and sulphite is technical grade potassium sulfite;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 5 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the Repone K of technical grade.
5. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 20 times of quality, and described solvent is technical grade dehydrated alcohol;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:2, described alkali is the lithium hydroxide of technical grade;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:1.5 for 1:1.5, temperature rising reflux 3 hours, described is chemical pure trioxymethylene containing benzaldehyde compound, and sulphite is technical grade ammonium sulphite;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 8 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the sodium-chlor of technical grade.
6. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 50 times of quality, and described solvent is technical grade 95# ethanol;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:2.1, described alkali is chemical pure triethylamine;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:2.1 for 1:2, temperature rising reflux 2 hours, described is technical grade vulkacit H containing benzaldehyde compound, and sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 10 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the sodium-chlor of technical grade.
7. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 80 times of quality, and described solvent is technical grade deionized water;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:2.5, described alkali is analytically pure pyridine;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:2.5 for 1:2.5, temperature rising reflux 4 hours, described is the technical grade formalin of mass concentration 30% containing benzaldehyde compound, and sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, add the salt of gained material 15 times of quality, more than mixed grinding to 40 order, namely obtain the fluorescein derivative of oil field tracer agent, described salt is mass ratio is the sodium-chlor of 1:1 technical grade and the mixture of Repone K.
8. the fluorescein derivative preparation method of oil field according to claim 1 tracer agent, is characterized in that, comprise the following steps:
The first step, adds fluorescein in reactor, adds the dissolution with solvents of fluorescein 100 times of quality, and described solvent is technical grade deionized water;
Second step, stir in downhill reaction still and add with fluorescein amount of substance than the alkali for 1:1.8, described alkali is mass ratio is the sodium hydroxide of the technical grade of 1:1 and the mixture of salt of wormwood;
3rd step, stir in downhill reaction still and add with fluorescein amount of substance than the sulphite containing benzaldehyde compound and 1:3 for 1:3.5, temperature rising reflux 6 hours, described is chemical pure trioxymethylene containing benzaldehyde compound, and sulphite is technical grade S-WAT;
4th step, is cooled to room temperature by reactor, boils off solvent, adds the salt of gained material 20 times of quality, more than mixed grinding to 40 order, namely obtains the fluorescein derivative of oil field tracer agent, and described salt is the Repone K of technical grade.
Priority Applications (1)
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| US20050214807A1 (en) * | 2003-11-19 | 2005-09-29 | Iain Johnson | Environmental sensitive fluorogenic compounds and their application for singlet oxygen and protein detection |
| CN102731457A (en) * | 2012-06-25 | 2012-10-17 | 西南石油大学 | Water-soluble fluorescent tracing polymer and its preparation method |
| CN102924468A (en) * | 2012-11-12 | 2013-02-13 | 天津市化学试剂研究所 | Preparing method of fluorescein complexing agents |
| CN103224483A (en) * | 2013-05-06 | 2013-07-31 | 西北工业大学 | Fluorescent compound used for labeling oligosaccharide, and preparation method thereof |
| CN103275698A (en) * | 2013-05-31 | 2013-09-04 | 太原理工大学 | Ratio-dependent bisulfite ion fluorescent probes and preparation method thereof |
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| US20050214807A1 (en) * | 2003-11-19 | 2005-09-29 | Iain Johnson | Environmental sensitive fluorogenic compounds and their application for singlet oxygen and protein detection |
| CN102731457A (en) * | 2012-06-25 | 2012-10-17 | 西南石油大学 | Water-soluble fluorescent tracing polymer and its preparation method |
| CN102924468A (en) * | 2012-11-12 | 2013-02-13 | 天津市化学试剂研究所 | Preparing method of fluorescein complexing agents |
| CN103224483A (en) * | 2013-05-06 | 2013-07-31 | 西北工业大学 | Fluorescent compound used for labeling oligosaccharide, and preparation method thereof |
| CN103275698A (en) * | 2013-05-31 | 2013-09-04 | 太原理工大学 | Ratio-dependent bisulfite ion fluorescent probes and preparation method thereof |
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