CN115895712A - Fine desulfurization auxiliary agent for oilfield produced liquid and preparation method thereof - Google Patents
Fine desulfurization auxiliary agent for oilfield produced liquid and preparation method thereof Download PDFInfo
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 61
- 230000023556 desulfurization Effects 0.000 title claims abstract description 61
- 239000007788 liquid Substances 0.000 title claims abstract description 39
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- -1 aldehyde compound Chemical class 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 150000001412 amines Chemical class 0.000 claims abstract description 11
- 239000008139 complexing agent Substances 0.000 claims abstract description 10
- 150000002505 iron Chemical class 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 12
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 8
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 7
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 7
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229920002866 paraformaldehyde Polymers 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 5
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 4
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 claims description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 4
- 229940090960 diethylenetriamine pentamethylene phosphonic acid Drugs 0.000 claims description 4
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 claims description 4
- 229960002089 ferrous chloride Drugs 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 3
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 3
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 claims description 2
- KIDJHPQACZGFTI-UHFFFAOYSA-N [6-[bis(phosphonomethyl)amino]hexyl-(phosphonomethyl)amino]methylphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCCCCCN(CP(O)(O)=O)CP(O)(O)=O KIDJHPQACZGFTI-UHFFFAOYSA-N 0.000 claims description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 19
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 8
- 230000003009 desulfurizing effect Effects 0.000 abstract description 7
- 238000011049 filling Methods 0.000 abstract description 7
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000011282 treatment Methods 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000008098 formaldehyde solution Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical compound C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011221 initial treatment Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- GGHDAUPFEBTORZ-UHFFFAOYSA-N propane-1,1-diamine Chemical compound CCC(N)N GGHDAUPFEBTORZ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a fine desulfurization auxiliary agent for oilfield produced liquid and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, the molar ratio is (0.8-1.5): 1, taking organic amine and an aldehyde compound as raw materials, taking an alcohol compound as a solvent, and synthesizing a desulfurization main agent by adopting an aldehyde-amine condensation method; secondly, adding an organic complexing agent into the soluble iron salt solution, wherein the molar ratio of the organic complexing agent to the soluble iron salt is (1-1.5): 1; finally, dropwise adding a main agent of a desulfurizing agent for reaction, and adjusting the pH value to 7-8 to obtain a liquid fine desulfurization product. The liquid fine desulfurization auxiliary agent has excellent fine desulfurization capability for low-concentration hydrogen sulfide, has the filling concentration far lower than that of the conventional liquid triazine desulfurizer, has the advantages of small filling amount and good desulfurization effect, and is particularly suitable for hydrogen sulfide removal treatment of offshore oil field produced liquid. In addition, the preparation method is simple, has low process requirements, is easy for batch production, and has good popularization and application values.
Description
Technical Field
The invention relates to the technical field of oilfield chemical desulphurization, in particular to a liquid fine desulphurization auxiliary agent for offshore oilfield produced liquid and a preparation method thereof.
Background
In the process of treating the produced liquid of the offshore oilfield, the existence of the hydrogen sulfide not only seriously threatens the life safety of field personnel, but also damages corrosive equipment. The offshore platform oil field mainly adopts a mode of filling a liquid desulfurizer in produced liquid to remove hydrogen sulfide.
At present, the liquid desulfurizer commonly used for offshore platforms is mainly organic amine desulfurizer and triazine desulfurizer. The action mechanism of the two types of desulfurizing agents is as follows: h in the same system 2 S reacts, thereby reducing the plateau hydrogen sulfide concentration. However, through on-site practical application, the inventor finds that the two types of liquid desulfurizing agents have better primary treatment effect on high-concentration hydrogen sulfide, and can achieve better coarse desulfurization effect by filling lower concentration. But the fine desulfurization effect is poor, when the concentration of the hydrogen sulfide on site is lower than 50ppm, the desulfurization effect is poor, and a large amount of filling is needed to meet the requirement that the concentration of the hydrogen sulfide required by site safety is lower than 10ppm.
Disclosure of Invention
The invention aims to solve the technical problems and provides a fine desulfurization auxiliary agent for oilfield produced liquid and a preparation method thereof.
In a first aspect, the invention provides a preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid, which is realized by adopting the following technical scheme.
A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid comprises the following steps:
s1, mixing an aldehyde compound and an alcohol compound, dripping organic amine into the mixture under the stirring state, and controlling the dripping speed to ensure that the reaction temperature does not exceed 60 ℃ and the dripping time is not less than 3 hours; after the dropwise addition is finished, stirring and reacting for 1-2h at 50-60 ℃, then heating to 70-80 ℃, and carrying out reduced pressure distillation for 1-2h at-0.09 to-0.1 MPa to obtain a main desulfurization agent; the molar ratio of the organic amine to the aldehyde compound is (0.8-1.5): 1, the mass of the alcohol compound accounts for 10-20% of the added materials;
s2, dissolving 0.008-0.05 mol of soluble iron salt in water, adding an organic complexing agent into the iron salt solution, stirring and reacting for 0.5-1h, wherein the molar ratio of the organic complexing agent to the soluble iron salt is (1-1.5): 1; and (3) dropwise adding the desulfurization main agent prepared in the step (S1) into the mixture, stirring and adjusting the pH value of the system to 7-8 to obtain the fine desulfurization auxiliary agent.
Further, the aldehyde compound is one or a mixture of two of formaldehyde, glutaraldehyde, trioxymethylene and paraformaldehyde.
Further, the alcohol compound is selected from methanol and/or ethanol.
Further, the organic amine is one or a mixture of two of ethanolamine, diethylamine, propylenediamine and diethylenetriamine.
Further, the soluble ferric salt is one of ferrous sulfate, ferrous chloride and ferrous nitrate.
Further, the organic complexing agent is a mixture of disodium ethylene diamine tetraacetate and organic acid, and the organic acid is selected from one of nitrilotriacetic acid, hydroxyethylidene diphosphonic acid, hexamethylenediamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene phosphonic acid and aminotrimethylene methylene phosphonic acid.
Furthermore, the molar quantity of the ethylene diamine tetraacetic acid disodium accounts for 80-90% of the total molar quantity of the organic complexing agent.
In a second aspect, the invention provides a fine desulfurization auxiliary agent for oilfield produced liquid, which is realized by adopting the following technical scheme.
A fine desulfurization auxiliary agent for oilfield produced liquid prepared by the preparation method.
The present application has the following advantageous effects.
The fine desulfurization auxiliary agent has excellent removal of H 2 The ability of S, especially for the fine desulfurization treatment of low-concentration hydrogen sulfide, has obvious effect, and overcomes the defects that the fine desulfurization performance of the existing liquid triazine desulfurizer and organic amine desulfurizer is poor and the safe production of a platform can be met only by adding a large amount of S. The preparation method of the fine desulfurization auxiliary agent is simple, has low process requirement, is easy for batch production, and has good popularization and application values.
Detailed Description
The present invention will be further described with reference to the following examples.
The information on the reagents used in the examples of the present invention is as follows:
the manufacturer of formaldehyde solution, glutaraldehyde solution, trioxymethylene, paraformaldehyde, methanol, ethanol, ethanolamine, diethylamine, propylenediamine, diethylenetriamine, ferrous sulfate, ferrous chloride, ferrous nitrate, disodium ethylenediamine tetraacetate, nitrilotriacetic acid, hydroxyethylidene diphosphonic acid, hexamethylenediamine tetramethylidene phosphonic acid, aminotrimethylene methylene phosphonic acid, and diethylenetriamine pentamethylene phosphonic acid is a Maya reagent.
Example 1
A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid comprises the following steps:
(1) Firstly, adding 30g of paraformaldehyde (1 mol) and 20.6g of ethanol into a reaction kettle, stirring at normal temperature, dropwise adding 30.5g (0.5 mol) of ethanolamine and 21.9g (0.3 mol) of diethylamine into an overhead dropwise adding tank for 3h, and controlling the temperature to be 55 ℃; after the dropwise addition is finished, controlling the temperature to be 50 ℃, stirring and reacting for 2h, then heating to 70 ℃, carrying out reduced pressure distillation for 1h under-0.09 MPa, and cooling to normal temperature to obtain a desulfurization main agent (6.1 g);
(2) Adding 7.6g of ferrous sulfate (0.05 mol) into 100g of water, and stirring at normal temperature to dissolve uniformly; 22.69g (0.0675 mol) of disodium ethylenediamine tetraacetic acid and 1.43g (0.0075 mol) of nitrilotriacetic acid were added thereto, and the reaction was stirred for 0.5 hour. 6.1g of desulfurization main agent is dripped, stirred at normal temperature for reaction, and the pH value of the system is adjusted to 7.5, so that a fine desulfurization auxiliary agent product is obtained.
Example 2
A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid comprises the following steps:
(1) Firstly, adding 73g of formaldehyde solution (37 percent of effective content, 0.9 mol), 9g of trioxymethylene (0.1 mol) and 16.1g of methanol into a reaction kettle, stirring at normal temperature, dropwise adding 74.13g (1 mol) of propane diamine through an overhead dropwise adding groove for 4h, and controlling the temperature to be 60 ℃; after the dropwise addition is finished, controlling the temperature at 60 ℃, stirring and reacting for 1.5h, then heating to 80 ℃, carrying out reduced pressure distillation for 2h under-0.1 MPa, and cooling to normal temperature to obtain a main desulfurization agent (3.5 g);
(2) Adding 1.0g of ferrous chloride (0.008 mol) into 100g of water, and stirring at normal temperature to dissolve uniformly; then adding 2.69g (0.008 mol) of disodium ethylene diamine tetraacetate and 0.69g (60% of effective content, 0.002 mol) of hydroxyethylidene diphosphonic acid, and stirring for reaction for 0.5h. 3.5g of desulfurization main agent is dripped, the mixture is stirred at normal temperature to react, and the pH value of the system is adjusted to 8, so that a fine desulfurization auxiliary agent product is obtained.
Example 3
A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid comprises the following steps:
(1) 160.2g of glutaraldehyde solution (with 50% effective content, 0.8 mol), 6g of paraformaldehyde (0.2 mol), 20.5g of ethanol and 25g of methanol are added into a reaction kettle, stirred at normal temperature, and 91.6g of ethanolamine is dropwise added through a high-position dropwise adding groove
(1.5 mol), the dripping time is 3h, and the temperature is controlled to be 50 ℃; after the dropwise addition is finished, controlling the temperature to be 55 ℃, stirring and reacting for 1h, then heating to 75 ℃, carrying out reduced pressure distillation for 1.5h under the pressure of-0.095 MPa, and cooling to normal temperature to obtain a main desulfurization agent (2.8 g);
(2) Adding 3.6g of ferrous nitrate (0.02 mol) into 100g of water, and stirring at normal temperature to dissolve uniformly; 6.72g (0.02 mol) of disodium ethylenediamine tetraacetate and 3.34g (97% effective content, 0.004 mol) of hexamethylenediamine tetramethylidene phosphonic acid were added, and the reaction was stirred for 1 hour. 2.8g of desulfurization main agent is dripped, the mixture is stirred at normal temperature to react, and the pH value of the system is adjusted to 7, so that a fine desulfurization auxiliary agent product is obtained.
Example 4
A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid comprises the following steps:
(1) Firstly, adding 30g of paraformaldehyde (1 mol), 3.3g of ethanol and 30g of methanol into a reaction kettle, stirring at normal temperature, dropwise adding 103.17g (1 mol) of diethylenetriamine into an overhead dropwise adding groove for 4h, and controlling the temperature to be 60 ℃; after the dropwise addition is finished, controlling the temperature to be 55 ℃, stirring and reacting for 1h, then heating to 80 ℃, carrying out reduced pressure distillation for 2h under-0.1 MPa, and cooling to normal temperature to obtain a main desulfurization agent (3.2 g);
(2) Adding 4.56g of ferrous sulfate (0.03 mol) into 100g of water, and stirring at normal temperature to dissolve uniformly; then, 10.1g (0.03 mol) of disodium ethylenediaminetetraacetate and 3.0g (50% active content, 0.005 mol) of aminotrimethylenephosphonic acid were added, and the reaction was stirred for 1 hour. 3.2g of desulfurization main agent is dripped, stirred at normal temperature for reaction, and the pH value of the system is adjusted to 7.8, so that a fine desulfurization auxiliary agent product is obtained.
Example 5
A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid comprises the following steps:
(1) Firstly, 40.5g of formaldehyde solution (with 37 percent of effective content, 0.5 mol), 15g of paraformaldehyde (0.5 mol) and 15.2g of methanol are added into a reaction kettle, stirred at normal temperature, and then 61.08g of ethanolamine (1 mol) and 20.6g of diethylenetriamine (0.2 mol) are dripped into an overhead dripping tank for 4 hours at the controlled temperature of 55 ℃; after the dropwise addition is finished, controlling the temperature at 60 ℃, stirring and reacting for 2h, then heating to 80 ℃, carrying out reduced pressure distillation for 2h under-0.1 MPa, and cooling to normal temperature to obtain a main desulfurization agent (5.8 g);
(2) Adding 6.08g of ferrous sulfate (0.04 mol) into 100g of water, and stirring at normal temperature to dissolve uniformly; 13.4g (0.04 mol) of disodium ethylene diamine tetraacetate and 9.7g (50% effective content, 0.005 mol) of diethylenetriamine pentamethylene phosphonic acid are added, and the mixture is stirred and reacted for 1 hour. 5.8g of desulfurization main agent is dripped, the mixture is stirred at normal temperature to react, and the pH value of the system is adjusted to 8, so that a fine desulfurization auxiliary agent product is obtained.
Performance test 1
The desulfurization performance contrast test for desulfurization of oil field produced liquid comprises the following steps: the 5 liquid desulfurizing agents prepared by the embodiments 1 to 5 of the invention are compared with the s-triazine desulfurizing agent and the organic amine desulfurizing agent widely applied in the oil field at present. The liquid desulfurizer samples used for comparison in the experiment are all products successfully applied to the offshore platform after being widely optimized and screened, and have certain representativeness.
The selected target oil fields are Bohai sea and south sea low-concentration hydrogen sulfide oil fields respectively. The desulfurization ability was measured by ASTM D4810-88 (1999) method Standard for measuring the content of hydrogen sulfide in Natural gas by colorimetric Detector tube method. Introducing 1L of oil field production fluid into a closed container, immediately sealing the container, placing the container into a vibration box to vibrate for 5 minutes, taking a gas sample from the top of the closed container to detect the concentration of hydrogen sulfide, and recording the gas sample as a blank concentration C of hydrogen sulfide 0 . Filling a certain amount of desulfurizer into a closed container, introducing 1L of oil field produced liquid, immediately sealing the container, placing the container into a shaking box to shake for 5 minutes, taking a gas sample from the top of the closed container to detect the concentration of hydrogen sulfide, and recording the concentration of hydrogen sulfide as the concentration C of hydrogen sulfide, wherein the concentration C of hydrogen sulfide required by a platform is less than 10ppm.
A test platform: bohai sea certain oil field
Experiment raw materials: oil field produced liquid
Evaluation method: in situ desulfurization testing experiment
The test results are shown in table 1 below:
TABLE 1 field screening data sheet
Performance test 2
A test platform: certain low hydrogen sulfide oil field in south China sea
Experiment raw materials: oil field produced liquid
Evaluation method: in situ desulfurization testing experiment
The test results are shown in table 2 below:
TABLE 2 field screening data sheet
The detection data show that the offshore oil field liquid fine desulfurization auxiliary agent can be used for treating low-concentration hydrogen sulfide in an offshore oil field, has the advantages of low filling concentration and better desulfurization effect compared with the existing s-triazine and organic amine liquid desulfurizing agents widely applied to oil fields, and has good popularization and application values.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: equivalent changes made according to the structure, shape and principle of the invention shall be covered by the protection scope of the invention.
Claims (8)
1. A preparation method of a fine desulfurization auxiliary agent for oilfield produced liquid is characterized by comprising the following steps: the method comprises the following steps:
s1, mixing an aldehyde compound and an alcohol compound, dripping organic amine into the mixture under the stirring state, and controlling the dripping speed to ensure that the reaction temperature does not exceed 60 ℃ and the dripping time is not less than 3 hours; after the dropwise addition is finished, stirring and reacting for 1-2h at 50-60 ℃, then heating to 70-80 ℃, and carrying out reduced pressure distillation for 1-2h at-0.09 to-0.1 MPa to obtain a main desulfurization agent; the molar ratio of the organic amine to the aldehyde compound is (0.8-1.5): 1, the mass of the alcohol compound accounts for 10-20% of the added materials;
s2, dissolving 0.008-0.05 mol of soluble iron salt in water, adding an organic complexing agent into the iron salt solution, stirring and reacting for 0.5-1h, wherein the molar ratio of the organic complexing agent to the soluble iron salt is (1-1.5): 1; and (3) dropwise adding the desulfurization main agent prepared in the step (S1) into the mixture, stirring and adjusting the pH value of the system to 7-8 to obtain the fine desulfurization auxiliary agent.
2. The preparation method of the fine desulfurization auxiliary agent for the oilfield produced liquid according to claim 1, characterized by comprising the following steps: the aldehyde compound is one or a mixture of two of formaldehyde, glutaraldehyde, trioxymethylene and paraformaldehyde.
3. The preparation method of the fine desulfurization auxiliary agent for the oilfield produced liquid according to claim 1, characterized by comprising the following steps: the alcohol compound is selected from methanol and/or ethanol.
4. The preparation method of the fine desulfurization auxiliary agent for the oilfield produced liquid according to claim 1, characterized by comprising the following steps: the organic amine is one or a mixture of two of ethanolamine, diethylamine, propylenediamine and diethylenetriamine.
5. The preparation method of the fine desulfurization auxiliary agent for the oilfield produced liquid according to claim 1, characterized by comprising the following steps: the soluble ferric salt is one of ferrous sulfate, ferrous chloride and ferrous nitrate.
6. The preparation method of the fine desulfurization auxiliary agent for the oilfield produced fluid according to claim 1, characterized by comprising the following steps: the organic complexing agent is a mixture of disodium ethylene diamine tetraacetate and organic acid, and the organic acid is one of nitrilotriacetic acid, hydroxyethylidene diphosphonic acid, hexamethylene diamine tetramethylene phosphonic acid, diethylenetriamine pentamethylene phosphonic acid and amino trimethylene phosphonic acid.
7. The preparation method of the fine desulfurization auxiliary agent for the oilfield produced liquid according to claim 6, characterized by comprising the following steps: the molar weight of the ethylene diamine tetraacetic acid disodium accounts for 80-90% of the total molar weight of the organic complexing agent.
8. A fine desulfurization aid for oilfield produced fluid prepared by the preparation method of any one of claims 1 to 7.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2119526C1 (en) * | 1997-04-23 | 1998-09-27 | Ахматфаиль Магсумович Фахриев | Method of removing hydrogen sulfide from gas condensate, petroleum, and petroleum products |
| CN105056719A (en) * | 2015-07-30 | 2015-11-18 | 福州大学化肥催化剂国家工程研究中心 | Preparation method of FeOOH low-temperature desulfurizer and desulfurizer prepared through same |
| CN108676577A (en) * | 2018-03-26 | 2018-10-19 | 中国海洋石油集团有限公司 | A kind of oil field mining liquid liquid desulfurizing agent and preparation method thereof |
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2022
- 2022-12-19 CN CN202211632083.7A patent/CN115895712A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2119526C1 (en) * | 1997-04-23 | 1998-09-27 | Ахматфаиль Магсумович Фахриев | Method of removing hydrogen sulfide from gas condensate, petroleum, and petroleum products |
| CN105056719A (en) * | 2015-07-30 | 2015-11-18 | 福州大学化肥催化剂国家工程研究中心 | Preparation method of FeOOH low-temperature desulfurizer and desulfurizer prepared through same |
| CN108676577A (en) * | 2018-03-26 | 2018-10-19 | 中国海洋石油集团有限公司 | A kind of oil field mining liquid liquid desulfurizing agent and preparation method thereof |
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