CN116785778A - Preparation method of modified biomass demulsifier, demulsifier and application - Google Patents
Preparation method of modified biomass demulsifier, demulsifier and application Download PDFInfo
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- CN116785778A CN116785778A CN202210269178.0A CN202210269178A CN116785778A CN 116785778 A CN116785778 A CN 116785778A CN 202210269178 A CN202210269178 A CN 202210269178A CN 116785778 A CN116785778 A CN 116785778A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002028 Biomass Substances 0.000 title claims abstract description 22
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 32
- 239000002351 wastewater Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229920000742 Cotton Polymers 0.000 claims description 26
- 239000000839 emulsion Substances 0.000 claims description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- 229920002678 cellulose Polymers 0.000 claims description 22
- 239000001913 cellulose Substances 0.000 claims description 22
- -1 amino compound Chemical class 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 238000010335 hydrothermal treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002834 transmittance Methods 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 34
- 238000002474 experimental method Methods 0.000 description 12
- 239000010779 crude oil Substances 0.000 description 7
- 230000005291 magnetic effect Effects 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 5
- 239000007764 o/w emulsion Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005553 drilling Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- FTQWRYSLUYAIRQ-UHFFFAOYSA-N n-[(octadecanoylamino)methyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCNC(=O)CCCCCCCCCCCCCCCCC FTQWRYSLUYAIRQ-UHFFFAOYSA-N 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229920005682 EO-PO block copolymer Polymers 0.000 description 1
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002332 oil field water Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920002755 poly(epichlorohydrin) Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/04—Breaking emulsions
- B01D17/047—Breaking emulsions with separation aids
Landscapes
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a preparation method of a modified biomass demulsifier, the demulsifier and application thereof. The application of the amino demulsifier in the oily wastewater can ensure that the water phase light transmittance reaches more than 86% after the oily wastewater is demulsified, and the oil removal rate is as high as 99%. The demulsifier provided by the invention has the characteristics of cheap and easily available raw materials, small dosage of the demulsifier, high demulsification efficiency, short time, recycling and reutilization of biomass waste, no pollution, easy degradation, simple preparation method and the like, has good adaptability, and has better application and popularization prospects.
Description
Technical Field
The invention relates to the technical field of demulsifiers in the petroleum and natural gas industry, in particular to a preparation method of an aminated biomass demulsifier, the demulsifier and application.
Background
In the petroleum and natural gas industry, the oil-water mixed water emulsion is a difficult problem to be solved in oil-gas exploration, oil extraction, oil field water transportation, treatment and refining. Firstly, in the drilling process, the additive added into the drilling fluid has an emulsifying effect on mixed diesel oil, grease and the like, so that the content of the drilling waste liquid oil is high, and the treatment, the reuse and the emission are affected; secondly, the crude oil emulsion is contacted with water to form emulsion due to the lipophilic characteristic of the natural surfactant in the crude oil; thirdly, the oil displacement agent which is used for emulsifying the active agent and the crude oil or chemically displacing the oil is emulsified with the crude oil, and the adsorption of an oil/water interface has a great influence on the delay of a sedimentation membrane or the inhibition of seepage. The active agent is adsorbed on the interface, so that precipitation of a film is often inhibited or delayed, oil-water separation is difficult, and links such as subsequent treatment, transportation and processing are affected. Thus, demulsification is of great importance in the oil and gas industry. Emulsion breaking methods can be divided into three categories, namely mechanical, electrical and chemical. In practice, a combination of mechanical and chemical, or electrical and chemical, is the best choice. The most widely used techniques include heating and adding demulsifiers.
The chemical demulsifier is an amphiphilic compound with hydrophilicity and hydrophobicity and can be adsorbed on an oil-water interface. Demulsifiers generally exhibit similar behavior to emulsifiers, but it is possible to replace stabilizers in the aqueous and oil phases, allowing the droplets to combine. In order to break up the stable oil/water interface around the emulsified water droplets, chemical demulsifiers typically need to have a stronger surface activity than natural emulsion stabilizers. Chemical demulsifiers of note are classified as polymeric surfactants, nanoparticles, and ionic liquids. For example, ethylene oxide-propylene oxide (EO-PO) block copolymers, silicone polyethers, dendrimers, biodegradable polymeric surfactants, ionic liquids and nanoparticle-based demulsifiers have attracted increasing attention in the industry. However, these demulsifiers have some inherent problems such as complex and dangerous preparation process, high cost of raw materials, certain pollution to the environment, serious resource waste and the like.
Chinese patent publication No. CN105384927a, publication No. 2016, 3 and 9 discloses an oil-in-water emulsion breaker and a preparation method thereof, wherein bisamide is prepared sequentially, chlorinated polyether is prepared, and finally cationic polyether is prepared, namely the oil-in-water emulsion breaker; the preparation method comprises the following steps: 1) Under stirring, the organic amine and fatty acid were mixed according to 1: 2-1: 4 (molar ratio), controlling the temperature of the reaction system at 50-170 ℃ and the reaction time at 3-18 h to obtain bisamide; 2) Sequentially adding an organic solvent ethanol and bisamide into a four-mouth bottle with a thermometer, a stirrer and a condenser tube, beginning to drop the polyepichlorohydrin at 20-120 ℃, stirring for 5 hours, and cooling to obtain chlorinated polyether which is a brownish red viscous liquid; 3) Placing the synthesized chlorinated polyether and dimethylamine aqueous solution into a clean reaction kettle, introducing nitrogen to remove air, controlling the temperature to be 50-80 ℃, reacting for 5 hours, continuously heating to 120 ℃, and reacting for 6 hours to obtain the tan water-soluble cationic polyether which is the oil-in-water emulsion demulsifier. The organic demulsifier prepared by the method has higher efficiency, but the demulsifier can be left in an oil phase or a water phase after demulsification, so that corresponding environmental problems are generated.
The Chinese patent document with publication number of CN106219669A and publication date of 2016, 12 and 14 discloses a preparation method of a magnetic graphene oxide demulsifier, which is prepared by taking magnetic iron powder as a carrier and loading graphene oxide on the surface of the magnetic iron powder, wherein the dosage ratio of the ferromagnetic powder, ethanol, water, a silane coupling agent and the graphene oxide is 1-5g, 70-95mL, 5-30mL, 0.2-1g and 1-5g. The method is characterized in that the demulsifier is prepared by taking magnetic iron powder as a carrier and loading graphene oxide on the surface of the magnetic iron powder, and the demulsifier can be reused. The magnetic iron powder modified graphene oxide demulsifier has the advantages of recycling and the like, but has the problems of complex process, high raw material cost and the like. Thus, there remains a major challenge to find a new demulsifier that is widely available, low cost and excellent in performance.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention provides a preparation method of a modified biomass demulsifier, which can effectively solve the technical problems of high raw material cost, narrow source selection range and poor performance of the demulsifier in the prior art.
The invention also aims at providing the demulsifier prepared by the preparation method.
It is a further object of the present invention to provide the use of the demulsifier prepared.
The invention is realized by adopting the following technical scheme:
a preparation method of a modified biomass demulsifier is characterized by comprising the following steps: the cotton is regenerated by phosphoric acid hydrolysis to obtain cellulose oligomer, and then the cellulose oligomer and amino compound are directly prepared by hydrothermal method to obtain the amino demulsifier.
The preparation method specifically comprises the following steps: adding cotton into phosphoric acid, fully dissolving, heating to 40-70 ℃, stirring for 1-3h, adding ethanol to regenerate dissolved cellulose and obtain cellulose oligomer, adding the cellulose oligomer into an amino compound aqueous solution, stirring uniformly, transferring to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal treatment to obtain the amino demulsifier.
Further, the cotton is natural cotton.
Further, the cotton is a product taking cotton as a raw material.
Further, the mass ratio of the cotton to the phosphoric acid is 1-5:100.
further, the mass ratio of the cellulose oligomer to the amino compound aqueous solution is 2:40-50.
Further, the amino compound is at least one of ammonia water, urea, ammonium bicarbonate and ethylenediamine.
The amino demulsifier prepared by the preparation method of the modified biomass demulsifier.
The amino demulsifier is applied to oil-containing wastewater emulsion.
Further, the application comprises the following steps: dispersing the amino demulsifier in water to obtain a suspension, and then mixing the suspension and the oily wastewater emulsion at room temperature and standing for 10-30 min.
After demulsification is finished, most of the amino demulsifier adsorbs oil and floats on water together with the separated oil phase, and a small part of the oil phase is settled in the water, so that the oil phase can be separated easily through long-time settlement or centrifugal separation.
Further, the addition amount of the amino demulsifier in the oily wastewater is 25-150mg/L.
Further, the adding amount of the amino demulsifier in the oily wastewater is 75-100mg/L.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method takes cotton as a precursor, and the prepared amino demulsifier has a large amount of active amino groups on the surface, shows high interfacial activity, can quickly reduce interfacial tension and induces demulsification.
2. The raw materials of the preparation method can be directly obtained from natural cotton or obtained from waste cotton fabrics, can interact with asphaltene after modification, and can carry out electrostatic neutralization between positively charged oil drops and negatively charged oil drops in emulsion after modification to promote demulsification. The invention fully utilizes natural biomass, reduces the use of fossil raw materials, can be degraded in natural environment, and has better application prospect.
3. The amino demulsifier provided by the invention can realize normal-temperature demulsification of oil-containing emulsion, realizes effective separation of oil and water, has the characteristics of small dosage and high demulsification efficiency, and the oil removal rate of 75mg/L demulsifier under normal-temperature conditions for 30min can reach 99.20%.
Drawings
FIG. 1 is a scanning electron microscope image of an aminated demulsifier described in example 4.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The cotton used in the examples is natural cotton. The crude oil used in the examples was derived from a Tarim field.
Example 1
As a preferred embodiment of the invention, a preparation method of a modified biomass demulsifier is disclosed, cotton is regenerated by phosphoric acid hydrolysis to obtain a cellulose oligomer, and then the cellulose oligomer and an amino compound are directly subjected to hydrothermal preparation to obtain an amino demulsifier.
Example 2
As another preferred embodiment of the invention, a preparation method of a modified biomass demulsifier is disclosed, which specifically comprises the following steps: adding cotton into phosphoric acid, fully dissolving, heating to 50 ℃, stirring for 2 hours, adding ethanol to regenerate dissolved cellulose and obtain cellulose oligomer, adding the cellulose oligomer into an amino compound aqueous solution, uniformly stirring, transferring to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal treatment to obtain the amino demulsifier. The cotton is natural cotton. The mass ratio of cotton to phosphoric acid is 3:100; the mass ratio of the cellulose oligomer to the amino compound aqueous solution is 2:45. The amino compound is at least one of ammonia water, urea, ammonium bicarbonate and ethylenediamine.
Example 3
The amino demulsifier prepared in the example 1 or 2 is applied to the oil-containing wastewater emulsion, and comprises the following steps: dispersing the amino demulsifier in water to obtain a suspension, and then mixing the suspension and the oily wastewater emulsion at room temperature and standing for 10-30 min.
After demulsification is finished, most of the amino demulsifier adsorbs oil and floats on water together with the separated oil phase, and a small part of the oil phase is settled in the water, so that the oil phase can be separated easily through long-time settlement or centrifugal separation. Further, the addition amount of the amino demulsifier in the oily wastewater is 75mg/L.
Example 4
The embodiment provides a preparation method of a modified biomass demulsifier, which is obtained through the following steps:
2g of cotton is added into 100ml of phosphoric acid, after being fully dissolved, the temperature is raised to 50 ℃ and the mixture is stirred for 2 hours, then 50ml of ethanol is added and the mixture is stirred for 20 minutes to regenerate cellulose oligomer, and then the product is freeze-dried by centrifugal washing to be neutral.
2g of cellulose oligomer is added into 50ml of amino compound aqueous solution, stirred uniformly and transferred into a polytetrafluoroethylene reaction kettle, and then subjected to hydrothermal reaction at 220 ℃ for 24 hours to obtain an amino demulsifier.
Example 5
The embodiment provides a preparation method of a modified biomass demulsifier, which is obtained through the following steps:
2g of cotton is added into 100ml of phosphoric acid, after being fully dissolved, the temperature is raised to 50 ℃ and the mixture is stirred for 2 hours, then 50ml of ethanol is added and the mixture is stirred for 20 minutes to regenerate cellulose oligomer, and then the product is freeze-dried by centrifugal washing to be neutral.
2g of cellulose oligomer is added into 50ml of amino compound aqueous solution, stirred uniformly and transferred into a polytetrafluoroethylene reaction kettle, and then subjected to hydrothermal reaction at 200 ℃ for 24 hours to obtain an amino demulsifier.
Example 6
Suspensions of different concentrations were formulated based on the aminated demulsifier prepared in example 4 to characterize the demulsification performance of the different concentrations of the aminated demulsifier in the oil-containing wastewater emulsion.
5 parts by weight of crude oil was added to 495 parts by weight of deionized water, stirred and mixed, heated to 60℃and then stirred at 11000r/min for 20 minutes, to obtain a stable oily wastewater emulsion (oil-in-water emulsion).
Adding different parts by weight of the amino demulsifier prepared in the example 4 into water to prepare amino demulsifier suspensions with mass fractions of 0.3%,0.25%,0.2%,0.15%,0.1% and 0.05%, and marking the obtained samples as experimental groups 1-6 respectively; the blank is water and the sample is designated as experimental group 7.
1 part by volume of the above experimental groups 1 to 6 was added to 20 parts by volume of the oily wastewater emulsion, and then mixed well by shaking, and then left at normal temperature for 30 minutes, and the light transmittance and oil removal rate thereof were measured, and the results are shown in Table 1.
Table 1 demulsification results for Experimental groups 1-7
| Group of | Demulsifier (mg/L) | Transmittance (%) | Oil removal Rate (%) |
| Experiment group 1 | 150 | 70.1 | 98.75 |
| Experiment group 2 | 125 | 74.4 | 98.82 |
| Experiment group 3 | 100 | 86.3 | 99.20 |
| Experiment group 4 | 75 | 86.6 | 99.20 |
| Experiment group 5 | 50 | 69.3 | 98.8 |
| Experiment group 6 | 25 | 36.1 | 97.5 |
| Experiment group 7 | 0 | 0 | 0 |
And (3) injection: the "amino demulsifier (mg/L)" in the table refers to the concentration of the amino demulsifier in the oil-containing wastewater emulsion.
As shown in Table 1, the amino demulsifier provided by the invention has good demulsification performance, the light transmittance of the oil-containing wastewater emulsion can reach 86.6% after sedimentation for 30min at normal temperature at the concentration of 75mg/L, and the oil removal rate is as high as 99.20%
Example 7
Based on the aminated demulsifier prepared in example 4, experimental groups 8-12 were set up in sequence for characterizing the demulsification performance of the aminated demulsifier at different pH values.
5 parts by weight of crude oil was added to 495 parts by weight of deionized water, stirred and mixed, the pH was adjusted by adding hydrochloric acid or sodium hydroxide, heated to 60℃and then stirred at 11000r/min for 20 minutes to obtain a stable oily wastewater emulsion (oil-in-water emulsion).
Adding the amino demulsifier prepared in the example 4 into water to prepare amino demulsifier suspensions with mass fractions of 0.05%, 0.1% and 0.15%, and respectively marking the samples as experimental groups 8-12;
1 part by volume of the above-mentioned aminated demulsifier suspension was added to 20 parts by volume of oil-containing wastewater emulsions having different pH values, and then mixed by sufficient shaking, and left at normal temperature for 30 minutes, and the light transmittance and oil removal rate thereof were measured, and the results are shown in Table 2.
Table 2 demulsification results for Experimental groups 8-12
| Group of | pH | Transmittance% | Oil removal rate% |
| Experiment group 8 | 4 | 0.9 | 91.68 |
| Experiment group 9 | 6 | 66.1 | 99.18 |
| Experiment group 10 | 7 | 86.6 | 99.16 |
| Experiment group 11 | 8 | 71.4 | 98.47 |
| Experiment group 12 | 10 | 3.4 | 93.8 |
As can be seen from table 2: the amino demulsifier provided by the invention can obtain higher demulsification efficiency near neutrality.
The demulsifier provided by the invention is suitable for demulsification of oil-containing wastewater emulsion, and has the characteristics of simple preparation method, wide raw material sources, no pollution, easiness in degradation, excellent demulsification performance and the like.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (12)
1. A preparation method of a modified biomass demulsifier is characterized by comprising the following steps: the cotton is regenerated by phosphoric acid hydrolysis to obtain cellulose oligomer, and then the cellulose oligomer and amino compound are directly prepared by hydrothermal method to obtain the amino demulsifier.
2. The method for preparing the modified biomass demulsifier according to claim 1, wherein the method comprises the following steps: the preparation method specifically comprises the following steps: adding cotton into phosphoric acid, fully dissolving, heating to 40-70 ℃, stirring for 1-3h, adding ethanol to regenerate dissolved cellulose and obtain cellulose oligomer, adding the cellulose oligomer into an amino compound aqueous solution, stirring uniformly, transferring to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal treatment to obtain the amino demulsifier.
3. The method for preparing the modified biomass demulsifier as claimed in claim 1 or 2, wherein the method comprises the following steps: the cotton is natural cotton.
4. The method for preparing the modified biomass demulsifier as claimed in claim 1 or 2, wherein the method comprises the following steps: the cotton is a product taking cotton as a raw material.
5. The method for preparing the modified biomass demulsifier as claimed in claim 1 or 2, wherein the method comprises the following steps: the mass ratio of the cotton to the phosphoric acid is 1-5:100.
6. the method for preparing the modified biomass demulsifier as claimed in claim 1 or 2, wherein the method comprises the following steps: the mass ratio of the cellulose oligomer to the amino compound aqueous solution is 2:40-50.
7. The method for preparing the modified biomass demulsifier as claimed in claim 1 or 2, wherein the method comprises the following steps: the amino compound is at least one of ammonia water, urea, ammonium bicarbonate and ethylenediamine.
8. An aminated demulsifier prepared by the method for preparing a modified biomass demulsifier according to claims 1-2.
9. Use of an aminated demulsifier prepared by the preparation method of the modified biomass demulsifier according to claims 1-2 in oil-containing wastewater emulsion.
10. Use of an aminated demulsifier as claimed in claim 9 in an oil-containing wastewater emulsion, comprising the steps of: dispersing the amino demulsifier in water to obtain a suspension, and then mixing the suspension and the oily wastewater emulsion at room temperature and standing for 10-30 min.
11. Use of an aminated demulsifier as claimed in claim 10 in an oil-containing wastewater emulsion, characterised in that: the addition amount of the amino demulsifier in the oily wastewater is 25-150mg/L.
12. Use of an aminated demulsifier as claimed in claim 11 in an oil-containing wastewater emulsion, characterised in that: the addition amount of the amino demulsifier in the oily wastewater is 75-100mg/L.
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