CN115193239A - Preparation method of composite liquid desulfurizer - Google Patents
Preparation method of composite liquid desulfurizer Download PDFInfo
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- CN115193239A CN115193239A CN202210787672.6A CN202210787672A CN115193239A CN 115193239 A CN115193239 A CN 115193239A CN 202210787672 A CN202210787672 A CN 202210787672A CN 115193239 A CN115193239 A CN 115193239A
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- 239000007788 liquid Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 238000003756 stirring Methods 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 150000001412 amines Chemical class 0.000 claims abstract description 13
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000000176 sodium gluconate Substances 0.000 claims abstract description 12
- 235000012207 sodium gluconate Nutrition 0.000 claims abstract description 12
- 229940005574 sodium gluconate Drugs 0.000 claims abstract description 12
- 239000003607 modifier Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 17
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 15
- 230000003009 desulfurizing effect Effects 0.000 claims description 12
- -1 polyethylene Polymers 0.000 claims description 9
- FAXDZWQIWUSWJH-UHFFFAOYSA-N 3-methoxypropan-1-amine Chemical compound COCCCN FAXDZWQIWUSWJH-UHFFFAOYSA-N 0.000 claims description 8
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 8
- 229920000768 polyamine Polymers 0.000 claims description 8
- 229920000573 polyethylene Polymers 0.000 claims description 8
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006477 desulfuration reaction Methods 0.000 abstract description 19
- 230000023556 desulfurization Effects 0.000 abstract description 19
- 230000005764 inhibitory process Effects 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000011368 organic material Substances 0.000 abstract description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- TXNXVKSSXJDGIR-UHFFFAOYSA-N OC(C)N1CN(CN(C1)O)O Chemical compound OC(C)N1CN(CN(C1)O)O TXNXVKSSXJDGIR-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000003546 flue gas Substances 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
- 239000002244 precipitate Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002973 irritant agent Substances 0.000 description 1
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- 239000003345 natural gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002455 scale inhibitor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a preparation method of a composite liquid desulfurizer, which comprises the following steps: s1: adding liquid alkali as a solvent into a reaction kettle; s2: adding aluminum hydroxide and sodium gluconate into the solvent in the S1, and stirring and mixing; s3: adding an organic amine solution into the mixture in the S2, stirring, heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing for temperature-controlled reaction for 0.2-0.3 hour; s4: stirring and heating, and controlling the reaction temperature to be constant for a certain time to obtain a main agent; s5: continuously adding the modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour; is formed by combining a plurality of organic and inorganic materials. Effectively makes up the limitation of the efficacy of the traditional single desulfurizer. The desulfurization and scale inhibition integrated device has the using effect of integrating desulfurization, scale inhibition and water purification, can effectively achieve the desulfurization using rate of over 99 percent, has the phenomena of obviously delaying scale inhibition, difficult formation of pipe scale and the like, and has obvious comprehensive cost performance advantage.
Description
Technical Field
The invention relates to the technical field of liquid desulfurizer preparation, in particular to a preparation method of a composite liquid desulfurizer.
Background
At present, the industry uses flake caustic soda or liquid caustic soda as a single raw material to carry out desulfurization treatment on flue gas. The method is applied to industries needing desulfurization treatment, such as ceramics, cement, glass, power plants, metallurgy, oil gas development and the like. In industrial production, large quantities of hydrogen sulfide are fed into the gas phase processing system along with natural gas. Hydrogen sulfide is a highly toxic and irritating gas that is not only harmful to humans, pollutes the environment, but also can cause severe corrosion to pipes and related equipment.
The prior industry takes caustic soda flakes or liquid caustic soda as a single raw material to perform the desulfurization treatment of flue gas, and has the following defects: only has the function of desulfurization, has single function, is easy to form the phenomenon of scaling and has overhigh use cost.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a composite liquid desulfurizer.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding liquid alkali as a solvent into a reaction kettle;
s2: adding aluminum hydroxide and sodium gluconate into the solvent in the S1, and stirring and mixing;
s3: adding an organic amine solution into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, and controlling the reaction temperature to be a specified reaction temperature for a certain time to obtain a main agent;
s5: continuously adding the modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and (4) adding a synergist and a dispersant into the product obtained in the step (S5), stirring until the mixture is uniformly mixed, and cooling to obtain the desulfurizer.
Preferably, the organic amine solution added in S3 is 2 to 7 parts by mass, and the organic amine is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine.
Preferably, the mass part of the synergist added in the S5 is 1-3 parts, and the synergist is one of piperazine, N-methyldiethanolamine and sulfolane.
Preferably, the mass part of the dispersant added in S5 is 0.5-3 parts, and the dispersant is one of methanol, ethanol and glycol.
Preferably, the liquid alkali solution added in S1 is 60-80 parts by mass of sodium hydroxide solution.
Preferably, the mass parts of the aluminum hydroxide and the sodium gluconate in the S2 are respectively 1-5 parts and 0.5-5 parts.
Preferably, the modifier added in S5 is a phosphoric acid solution with the mass fraction of 5-10 parts.
Preferably, in the S4, the reaction temperature is 40-60 ℃, and the reaction time is 0.5 hour.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of a composite liquid desulfurizer, which has the following beneficial effects:
1. the preparation method of the compound liquid desulfurizer is formed by combining various organic and inorganic materials. Effectively makes up the limitation of the efficacy of the traditional single desulfurizer. The desulfurization and scale inhibition integrated device has the using effect of integrating desulfurization, scale inhibition and water purification, can effectively achieve the desulfurization using rate of over 99 percent, and has the phenomena of obviously delaying scale inhibition, difficult formation of pipe scale and the like. The comprehensive cost performance advantage of the product is obvious.
2. According to the preparation method of the compound liquid desulfurizer, liquid alkali is introduced to generate a desulfurization function, aluminum hydroxide generates a water purification function, and sodium gluconate generates a function of obviously delaying scale inhibition. Effectively overcomes the limitation that the traditional single desulfurizer only has the single function of desulfurization. The product has obvious advantages of comprehensive cost performance, and the cost is lower by more than 5% compared with the traditional method of using single raw material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Shown in the described embodiments, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The following examples, which are set forth to illustrate, are intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used for convenience in describing and simplifying the description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be construed as limiting the invention.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
The first embodiment is as follows:
a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding 60 parts by mass of sodium hydroxide solution serving as a solvent into a reaction kettle;
s2: adding 1 part by mass of aluminum hydroxide and 0.5 part by mass of sodium gluconate into the solvent in the S1, and stirring and mixing;
s3: adding 2 parts by mass of organic amine which is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, controlling the reaction temperature at a specified reaction temperature (40-60 ℃), and continuously reacting for 0.5 hour to obtain a main agent;
s5: continuously adding 5 parts by mass of phosphoric acid solution serving as a modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and (3) adding 1 part by mass of a synergist into the product obtained in the step (S5), wherein the synergist is one of piperazine, N-methyldiethanolamine and sulfolane, and 0.5 part by mass of a dispersant which is one of methanol, ethanol and ethylene glycol, stirring until the materials are uniformly mixed, and cooling to obtain the desulfurizer.
Example two:
a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding 64 parts by mass of sodium hydroxide solution serving as a solvent into a reaction kettle;
s2: adding 1.5 parts by mass of aluminum hydroxide and 1 part by mass of sodium gluconate to the solvent in the step S1, and stirring and mixing;
s3: adding 3 parts by mass of organic amine which is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, controlling the reaction temperature at a specified reaction temperature (the reaction temperature is 40-60 ℃), and continuously reacting for 0.5 hour to obtain a main agent;
s5: continuously adding 6 parts by mass of phosphoric acid solution serving as a modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and adding 1.5 parts by mass of a synergist which is one of piperazine, N-methyldiethanolamine and sulfolane and 1 part by mass of a dispersant which is one of methanol, ethanol and glycol into the product obtained in the step S5, stirring until the mixture is uniformly mixed, and cooling to obtain the desulfurizer.
Example three:
a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding 68 parts by mass of sodium hydroxide solution serving as a solvent into a reaction kettle;
s2: adding 2.2 parts by mass of aluminum hydroxide and 1.5 parts by mass of sodium gluconate into the solvent in the S1, and stirring and mixing;
s3: adding 4 parts by mass of organic amine which is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, controlling the reaction temperature at a specified reaction temperature (the reaction temperature is 40-60 ℃), and continuously reacting for 0.5 hour to obtain a main agent;
s5: continuously adding 6.5 parts by mass of phosphoric acid solution serving as a modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and (3) adding 2 parts by mass of a synergist into the product obtained in the step (S5), wherein the synergist is one of piperazine, N-methyldiethanolamine and sulfolane and 2 parts by mass of a dispersant, and the dispersant is one of methanol, ethanol and ethylene glycol, stirring until the materials are uniformly mixed, and cooling to obtain the desulfurizer.
Example four:
a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding 72 parts by mass of sodium hydroxide solution serving as a solvent into a reaction kettle;
s2: adding 3 parts by mass of aluminum hydroxide and 2 parts by mass of sodium gluconate into the solvent in the step S1, and stirring and mixing;
s3: adding 5 parts by mass of organic amine which is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, controlling the reaction temperature at a specified reaction temperature (the reaction temperature is 40-60 ℃), and continuously reacting for 0.5 hour to obtain a main agent;
s5: continuously adding 7 parts by mass of phosphoric acid solution serving as a modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and adding 2.2 parts by mass of a synergist into the product obtained in the step S5, wherein the synergist is one of piperazine, N-methyldiethanolamine and sulfolane and 2.2 parts by mass of a dispersant, and the dispersant is one of methanol, ethanol and glycol, stirring until the components are uniformly mixed, and cooling to obtain the desulfurizer.
Example five:
a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding 76 parts by mass of sodium hydroxide solution serving as a solvent into a reaction kettle;
s2: adding 4 parts by mass of aluminum hydroxide and 3 parts by mass of sodium gluconate into the solvent in the step S1, and stirring and mixing;
s3: adding 6 parts by mass of organic amine which is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, controlling the reaction temperature at a specified reaction temperature (the reaction temperature is 40-60 ℃), and continuously reacting for 0.5 hour to obtain a main agent;
s5: continuously adding 8 parts by mass of phosphoric acid solution serving as a modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and adding 2.5 parts by mass of a synergist into the product obtained in the step S5, wherein the synergist is one of piperazine, N-methyldiethanolamine and sulfolane and 2.5 parts by mass of a dispersant, and the dispersant is one of methanol, ethanol and ethylene glycol, stirring until the materials are uniformly mixed, and cooling to obtain the desulfurizer.
Example six:
a preparation method of a composite liquid desulfurizer comprises the following steps:
s1: adding 80 parts by mass of sodium hydroxide solution serving as a solvent into a reaction kettle;
s2: adding 5 parts by mass of aluminum hydroxide and 5 parts by mass of sodium gluconate into the solvent in the step S1, and stirring and mixing;
s3: adding 7 parts by mass of organic amine which is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine and polyethylene polyamine into the mixture in the S2, stirring and heating to 60 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing and controlling the temperature to react for 0.2-0.3 hours;
s4: stirring and heating, controlling the reaction temperature at a specified reaction temperature (40-60 ℃), and continuously reacting for 0.5 hour to obtain a main agent;
s5: continuously adding 10 parts by mass of phosphoric acid solution serving as a modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and (3) adding 3 parts by mass of a synergist into the product obtained in the step (S5), wherein the synergist is one of piperazine, N-methyldiethanolamine and sulfolane, and the dispersant is 3 parts by mass of one of methanol, ethanol and ethylene glycol, stirring until the materials are uniformly mixed, and cooling to obtain the desulfurizer.
Comparative example 1:
5ml of the liquid desulfurizing agent prepared in examples 1 to 6 and 5ml of 1,3, 5-trihydroxyethylhexahydro-s-triazine desulfurizing agent commonly used in the prior art are taken as a control group respectively, treated at 50 ℃, added into an absorption bottle filled with 95ml of clear water, stirred uniformly and then introduced with mixed gas of nitrogen and hydrogen sulfide containing 4000ppm of hydrogen sulfide concentration. Controlling the gas flow rate to be 20ml/min, and fully contacting the mixed gas with the desulfurizer diluent. And then, measuring the content of hydrogen sulfide in the desulfurized mixed gas by using a hydrogen sulfide detector at the outlet of the absorption bottle. The test results are shown in table 1 below:
as can be seen from Table 1, the liquid desulfurizing agent provided by the invention has better desulfurizing effect, the solution after desulfurization is uniform, no precipitate exists, while 1,3, 5-trihydroxyethylhexahydro-s-triazine in the prior art has precipitate after desulfurization, and therefore, after desulfurization by using the liquid desulfurizing agent provided by the invention, a long-chain monoethanolamine is not generated, but a long-chain divinylamino polyether substance with good water solubility is generated, so that the scaling tendency of an oil-gas well can be relieved. The liquid desulfurizer provided by the invention has stronger permeability due to existence of the divinylaminopolyether group, plays a better emulsification role, can obviously increase the dissolution speed of hydrogen sulfide and the mass transfer speed in a solution, promotes the desulfurization reaction, is more environment-friendly and reliable, obviously increases the desulfurization efficiency and improves the desulfurization rate. Among them, the liquid desulfurizing agent prepared in example 2 is better in desulfurization performance.
Comparative example 2:
and detecting the anti-scaling performance of the medicament aiming at the Bohai sea LD27-2 oilfield field water quality. The detection method refers to a SY/T5673-1993 method for evaluating the performance of the oilfield scale inhibitor. According to the experimental conditions, 100ml of corresponding test medium is added into a colorimetric tube with a plug, the adding concentration of the desulfurizer is 200mg/L, the temperature is heated to 55 ℃ of the test temperature, and the constant temperature is kept for 48 hours. And (3) when the temperature is cooled, observing the scaling condition of the medium in the colorimetric tube, shaking the medium uniformly if the medium is scaled, filtering, and carrying out a titration experiment, wherein the titration experiment refers to GB7476-87 EDTA titration method for measuring the calcium content of water quality.
The performance of the antiscaling agent is characterized by antiscaling rate, and the larger the percentage value is, the better the antiscaling performance is. The scale inhibition ratio E was calculated as follows:
in the formula:
M 2 -the concentration of calcium ions in the product fluid after the addition of the agent;
M 1 -calcium ion concentration in the production fluid without the addition of medicament;
M 0 -initial calcium ion concentration in the production fluid.
The test results are shown in table 2 below:
TABLE 2 evaluation of Scale inhibition Properties
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a reference structure" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Claims (8)
1. The preparation method of the compound liquid desulfurizer is characterized by comprising the following steps:
s1: adding liquid alkali as a solvent into a reaction kettle;
s2: adding aluminum hydroxide and sodium gluconate into the solvent in the S1, and stirring and mixing;
s3: adding an organic amine solution into the mixture in the S2, stirring, heating to 40 ℃, then dropwise adding an alkanolamine compound at the temperature of 60-75 ℃, and then standing for temperature-controlled reaction for 0.2-0.3 hour;
s4: stirring and heating, and controlling the reaction temperature to be a specified reaction temperature for a certain time to obtain a main agent;
s5: continuously adding the modifier into the main agent, controlling the reaction temperature to be 40-50 ℃, and continuously stirring for reaction for 0.1-0.3 hour;
s6: and (4) adding a synergist and a dispersant into the product obtained in the step (S5), stirring until the mixture is uniformly mixed, and cooling to obtain the desulfurizer.
2. The preparation method of the compound liquid desulfurizing agent according to claim 1, wherein the organic amine solution added in S3 is 2 to 7 parts by mass, and the organic amine is one of methylamine solution, ethanolamine, ethylenediamine, 3-methoxypropylamine, diethylenetriamine, and polyethylene polyamine.
3. The preparation method of the compound type liquid desulfurizing agent according to claim 1, wherein the mass part of the synergist added in S5 is 1-3 parts, and the synergist is one of piperazine, N-methyldiethanolamine and sulfolane.
4. The preparation method of the compound liquid desulfurizer according to claim 1, wherein the dispersant added in S5 is 0.5 to 3 parts by mass, and the dispersant is one of methanol, ethanol, and ethylene glycol.
5. The preparation method of the compound liquid desulfurizing agent according to claim 1, wherein the liquid alkali solution added in the S1 is 60-80 parts by mass of sodium hydroxide solution.
6. The preparation method of the compound liquid desulfurizing agent according to claim 1, wherein the mass parts of the aluminum hydroxide and the sodium gluconate in the step S2 are 1-5 parts and 0.5-5 parts respectively.
7. The preparation method of the compound liquid desulfurizing agent according to claim 1, wherein the modifier added in S5 is phosphoric acid solution with a mass fraction of 5-10 parts.
8. The preparation method of the compound liquid desulfurizing agent according to claim 1, wherein in the step S4, the reaction temperature is 40 ℃ to 60 ℃ and the reaction time is 0.5 hour.
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