A sewage degreasing agent and its preparation method and application

The polymer surfactant oil removal agent prepared by using functional monomers such as acryloyloxyethyldimethylbenzylammonium chloride has solved the problem of complex process, high cost or poor oil removal effect in the existing oil removal agent. , achieving efficient sewage oil removal and flocculation effects.

CN116948088BActive Publication Date: 2025-02-14SHENZHEN JIEWANG FINE CHEM TECH
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Patent Information

Application Number
CN202310979326.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-08-05
Publication Date
2025-02-14
Estimated Expiration
2043-08-05

AI Technical Summary

Technical Problem

The existing sewage oil dehydrating agents have problems such as complex preparation process, high cost or unsatisfactory oil removal effect, which is difficult to meet the high requirements for oil removal and flocculation rates in the return water of oil fields.

Method used

Functional monomers such as acryloyloxyethyldimethylbenzyl ammonium chloride, 2-(allyldimethylsilyl)pyridine, 1-vinyl-3-methylimidazole trifluoromethanesulfonate are used. , through high-position dropping reaction and drying granulation process, polymer surfactant oil removal agent was prepared.

Benefits of technology

The efficient oil removal effect is achieved with an oil removal rate of more than 98.5% and a flocculation rate of more than 96%. The process is simple, the raw materials are widely sourced, and the cost is relatively low.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of sewage treatment, and specifically relates to a sewage degreasing agent and its preparation method and application. The preparation method comprises adding acryloyloxyethyl dimethylbenzyl ammonium chloride, 2-(allyldimethylsilyl) pyridine, 1-vinyl-3-methylimidazole trifluoromethanesulfonate, emulsifier, buffer salt, distilled water, stirring evenly, and adjusting pH7-8; adding initiator solution to a high-position drop-adding tank, slowly dropping it into the reactor, and after the drop-adding is completed, continuing to heat up to 50-60°C, heat-keeping reaction, cooling to below 35°C, adjusting pH, and obtaining a viscous liquid; drying and granulating the above-mentioned viscous liquid to obtain a product degreasing agent. The degreasing agent of the present invention has the characteristics of wide source of raw materials, simple synthesis process, and high degreasing flocculation efficiency. When the concentration is 6mg / L, the degreasing rate reaches more than 98.5%, and the flocculation rate can reach more than 96%.
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Description

Technical Field

[0001] The invention belongs to the technical field of sewage treatment, and specifically relates to a sewage degreasing agent and a preparation method and application thereof. Background Art

[0002] Most of my country's oil fields have entered the middle and late stages of development, with secondary and tertiary oil recovery as the main methods of oil recovery. In order to stabilize and increase production, major oil fields have adopted various measures to increase produced fluids, resulting in a sharp increase in the water content of produced fluids, which has exceeded 90%, and a significant increase in sewage treatment volume.

[0003] The emulsification stability of oil droplets and suspended solids in this part of wastewater is strong. If these oily wastewaters are discharged at will, it will not only waste water and crude oil, but also seriously pollute the surrounding environment. Therefore, they must be treated and utilized reasonably to create good environmental and social and economic benefits. There are generally two final destinations for wastewater after treatment: (1) discharged after treatment to meet the discharge standards; (2) used as reinjection water for water injection mining or injected into waste formations after treatment to meet certain standards. As environmental pressures increase, the state has increasingly restricted the discharge of oilfield wastewater in compliance with standards. Shengli Oilfield has implemented zero discharge of produced water, which means that all water in the produced fluid needs to be injected back into the formation.

[0004] The oil content of oilfield reinjection water is strictly required, and wastewater needs to be treated for oil removal. Common physical methods include flotation, which is to introduce air into wastewater to generate tiny bubbles as carriers, so that pollutants such as emulsified oil and tiny suspended solids in the wastewater adhere to the bubbles to form a flotation body. The bubbles rise to the water surface by the buoyancy effect, and the purpose of separating impurities and purifying wastewater is achieved by collecting foam or scum on the water surface. The cost of flotation oil removal is low, but there are two problems: first, the introduction of oxygen in the flotation process will cause corrosion to oil well equipment, and second, the effect of pure flotation treatment is not ideal, and chemical agents are usually required to achieve a better oil removal effect.

[0005] At present, chemical degreasing is attracting more and more attention. The commonly used chemical degreasing agent is degreasing agent, but the degreasing agents on the market generally have the following disadvantages: some have good degreasing effect, but have the disadvantages of complex preparation and use process and high cost; some have a single ingredient, simple preparation and use process, low cost, but have the disadvantage of poor degreasing effect.

[0006] ZL201410254042.8 discloses a composite flocculation deoiling agent for oily wastewater treatment, which is a composite of aluminum sulfate, magnesium chloride, magnesium hydroxide, bentonite and polyacrylamide. The deoiling agent has the characteristics of small dosage, high oil removal efficiency, simple preparation and low cost, but the deoiling agent needs to use corrosive magnesium hydroxide, which has a strong corrosive effect on equipment. At the same time, a large amount of magnesium ions and aluminum ions are used in the invention, which are easy to react with polymers or surfactants in binary composite flooding to produce precipitation, and it is difficult to apply it in the treatment of binary composite flooding produced water.

[0007] Soviet invention patent SU935481 discloses a technology for treating industrial wastewater using aluminum sulfate and cationic flocculants. The main disadvantages of this invention are that its preparation method is complicated, the price is expensive, and the effect on oily wastewater is not ideal. Summary of the invention

[0008] In view of the deficiencies in the current prior art, the present invention provides a wastewater oil removal agent and a preparation method and application thereof. The oil removal agent of the present invention has the characteristics of a wide source of raw materials, a simple synthesis process, and a high oil removal and flocculation efficiency. When the use concentration is 6 mg / L, the oil removal rate reaches more than 98.5%, and the flocculation rate can reach more than 96%.

[0009] One of the purposes of the present invention is to provide a wastewater degreasing agent, the degreasing agent having the following molecular formula:

[0010]

[0011] Wherein, x=10000-100000;

[0012] y = 2000-20000;

[0013] z=5000-50000.

[0014] The viscosity average molecular weight of the degreasing agent is 10,000,000-20,000,000.

[0015] Another object of the present invention is to provide a method for preparing a sewage degreasing agent, the preparation method comprising:

[0016] (1) purging the reactor and pipelines with nitrogen, adding acryloyloxyethyl dimethylbenzyl ammonium chloride, 2-(allyldimethylsilyl)pyridine, 1-vinyl-3-methylimidazole trifluoromethanesulfonate, emulsifier, buffer salt, and distilled water in sequence, stirring evenly, and adjusting the pH to 7-8 with sodium hydroxide solution;

[0017] (2) Add the initiator solution into the high-position dropping tank and slowly drip it into the reactor. The initiator dripping time is controlled at 60-120 min. After the dripping is completed, continue to heat to 50-60° C., keep the temperature for reaction, cool to below 35° C., adjust the pH to 7-8 with sodium hydroxide solution, and obtain a viscous liquid;

[0018] (3) drying and granulating the viscous liquid to obtain a degreasing agent product.

[0019] In the present invention, preferably, based on 1 mole of acryloyloxyethyl dimethylbenzyl ammonium chloride, the amounts of 2-(allyldimethylsilyl)pyridine and 1-vinyl-3-methylimidazole trifluoromethanesulfonate are 0.1-0.3 mole and 0.2-0.8 mole, respectively.

[0020] Preferably, in step (1), the emulsifier is one of TX-10 (nonylphenol polyoxyethylene ether) and SPAN-60 (sorbitan monostearate), and the weight ratio of the emulsifier to acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.02-0.04:1.

[0021] Preferably, in step (1), the buffer salt is one of sodium dihydrogen phosphate, potassium dihydrogen phosphate, ammonium dihydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, and diammonium hydrogen phosphate, and the weight ratio of the buffer salt to acryloyloxyethyl dimethylbenzyl ammonium chloride is 0.01-0.05:1.

[0022] Preferably, in step (1), the weight ratio of distilled water to acryloyloxyethyl dimethyl benzyl ammonium chloride is 8-10:1.

[0023] In the present invention, preferably, in step (2), the initiator is one of peroxides, azo compounds, and redox initiators.

[0024] More preferably, the peroxide is one of hydrogen peroxide, sodium peroxide and peracetic acid.

[0025] More preferably, the azo compound is azobisisobutyronitrile methanol or azobisisoheptylnitrile methanol.

[0026] More preferably, the redox type is one of a mixture of potassium persulfate + sodium sulfite, a mixture of sodium persulfate + sodium sulfite, and a mixture of ammonium persulfate + sodium sulfite.

[0027] Preferably, the weight ratio of the initiator to acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.05-0.2:1.

[0028] Preferably, in step (2), the insulation reaction time is 1-4 hours.

[0029] The synthetic reaction equation of the sewage degreasing agent of the present invention is as follows:

[0030]

[0031] The third object of the present invention is to disclose the application of the above wastewater degreasing agent in degreasing oil from oilfield wastewater or industrial wastewater.

[0032] The sewage degreasing agent provided by the present invention is a high molecular surfactant, which is polymerized by three functional monomers. It contains non-polar groups such as phenyl, silane, fluoroalkyl and long-chain alkyl, which are lipophilic and can adsorb oil in sewage, so that one side of the molecule penetrates into the oily dirt, and the emulsified oil and dissolved oil in the sewage are extracted through penetration, emulsification and stripping to form relatively stable floccules, which are dispersed and floated on the surface of the solution, thereby achieving the degreasing effect. It contains amide quaternary ammonium salt, imidazoline quaternary ammonium salt and pyridinamine, which can capture a large number of negatively charged suspended solids, and the bridging effect connects these suspended solids, so that flocculation is easy to occur, and the degreasing effect is enhanced.

[0033] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0034] (1) The raw materials of the degreasing agent of the present invention are widely available and the synthesis process is simple;

[0035] (2) The present invention has a high oil removal rate. When the concentration is 6 mg / L, the oil removal rate reaches more than 98.5%. At the same time, it has a high flocculation rate: when the concentration is 6 mg / L, the flocculation rate can reach more than 96%. DETAILED DESCRIPTION

[0036] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0037] The present invention will be further described below with reference to specific embodiments.

[0038] Example 1

[0039] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.05 mol of 2-(allyldimethylsilyl)pyridine, 0.154 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 2.69 g of TX-10, 1.35 g of sodium dihydrogen phosphate, and 1076 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0040] (2) adding an initiator solution in a high-position dropping tank, wherein the initiator solution is 6.7 g of azobisisobutyronitrile dissolved in 80 g of methanol, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 60 min. After the dropping is completed, the temperature is continued to rise to 58° C., and the temperature is kept for reaction for 1 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0041] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H1.

[0042] Example 2

[0043] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.063 mol of 2-(allyldimethylsilyl)pyridine, 0.1 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 5.38 g of span-60, 6.73 g of potassium dihydrogen phosphate, and 1098 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0044] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 14.2 g of hydrogen peroxide dissolved in 60 g of distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 120 min. After the dropping is completed, the temperature is continuously raised to 52° C., and the reaction is kept at this temperature for 3.5 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0045] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H2.

[0046] Example 3

[0047] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.074 mol of 2-(allyldimethylsilyl)pyridine, 0.188 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 4.44 g of span-60, 1.88 g of ammonium dihydrogen phosphate, and 1345 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0048] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 19.8 g of sodium peroxide dissolved in 100 g of distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 90 min. After the dropping is completed, the temperature is continuously raised to 55° C., and the reaction is kept at this temperature for 4 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0049] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H3.

[0050] Example 4

[0051] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.1 mol of 2-(allyldimethylsilyl)pyridine, 0.2 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 4.35 g of span-60, 2.44 g of disodium hydrogen phosphate, and 1187 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0052] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 26.9 g of peracetic acid dissolved in 110 g of distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 80 min. After the dropping is completed, the temperature is continuously raised to 57° C., and the reaction is kept at this temperature for 3 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0053] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H4.

[0054] Example 5

[0055] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.082 mol of 2-(allyldimethylsilyl)pyridine, 0.22 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 2.82 g of TX-10, 6.13 g of disodium hydrogen phosphate, and 1176 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0056] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 8 g of sodium persulfate and 3.13 g of sodium sulfite dissolved in 80 g of distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 110 min. After the dropping is completed, the temperature is continuously raised to 58° C., and the reaction is kept at this temperature for 1 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0057] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H5.

[0058] Example 6

[0059] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.119 mol of 2-(allyldimethylsilyl)pyridine, 0.284 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 3.13 g of TX-10, 5.28 g of dipotassium hydrogen phosphate, and 1104 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0060] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 6.14 g potassium persulfate and 2.13 g sodium sulfite dissolved in 83 g distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 90 min. After the dropping is completed, the temperature is continuously raised to 56° C., and the reaction is kept at this temperature for 2 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0061] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H6.

[0062] Example 7

[0063] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.123 mol of 2-(allyldimethylsilyl)pyridine, 0.313 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 5.25 g of TX-10, 5.18 g of diammonium hydrogen phosphate, and 1176 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0064] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 7.3 g of ammonium persulfate and 3.23 g of sodium sulfite dissolved in 94 g of distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 70 min. After the dropping is completed, the temperature is continuously raised to 53° C., and the reaction is kept at this temperature for 1 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0065] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H7.

[0066] Example 8

[0067] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.144 mol of 2-(allyldimethylsilyl)pyridine, 0.383 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 4.84 g of TX-10, 4.35 g of sodium dihydrogen phosphate, and 1258 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0068] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 10.2 g of ammonium persulfate and 2.41 g of sodium sulfite dissolved in 107 g of distilled water, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 80 min. After the dropping is completed, the temperature is continuously raised to 55° C., and the reaction is kept at this temperature for 1 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0069] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H8.

[0070] Example 9

[0071] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.15 mol of 2-(allyldimethylsilyl)pyridine, 0.4 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 4.66 g of TX-10, 3.33 g of sodium dihydrogen phosphate, and 1100 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0072] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 8.48 g of azobisisoheptanonitrile dissolved in 95 g of methanol, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 100 min. After the dropping is completed, the temperature is continuously raised to 52° C., and the reaction is kept at this temperature for 1 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0073] (3) Drying and granulating the viscous liquid to obtain the degreasing agent H9.

[0074] Example 10

[0075] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.12 mol of 2-(allyldimethylsilyl)pyridine, 0.4 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 3.15 g of TX-10, 4.1 g of sodium dihydrogen phosphate, and 1106 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0076] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 12.11 g of azobisisobutyronitrile dissolved in 96 g of methanol, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 120 min. After the dropping is completed, the temperature is continuously raised to 60° C., and the reaction is kept at this temperature for 1.5 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0077] (3) Drying and granulating the viscous liquid to obtain the product degreasing agent H 10 .

[0078] Embodiment 11

[0079] (1) Purge the reactor and pipeline with nitrogen, add 0.5 mol of acryloyloxyethyl dimethylbenzyl ammonium chloride, 0.133 mol of 2-(allyldimethylsilyl)pyridine, 0.22 mol of 1-vinyl-3-methylimidazole trifluoromethanesulfonate, 3.88 g of TX-10, 3.4 g of sodium dihydrogen phosphate, and 1112 g of distilled water in sequence, stir evenly, and adjust the pH to 7-8 with sodium hydroxide solution;

[0080] (2) adding an initiator solution into a high-position dropping tank, wherein the initiator solution is 10.22 g of azobisisobutyronitrile dissolved in 110 g of methanol, and slowly dropping the solution into the reactor. The initiator dropping time is controlled within 60 min. After the dropping is completed, the temperature is continuously raised to 50° C., and the temperature is kept for reaction for 1 h. The temperature is then lowered to below 35° C., and the pH is adjusted to 7-8 with a sodium hydroxide solution to obtain a viscous liquid.

[0081] (3) Drying and granulating the viscous liquid to obtain the product degreasing agent H 11 .

[0082] Example 12 Evaluation of oil removal effect

[0083] The present invention was diluted into a 100 mg / L solution, and the deoiling agent was added according to effective concentrations of 2, 4, and 6 mg / L. The evaluation method referred to Q / SH10201961-2018 "General Technical Conditions for Deoiling Agents for Oilfield Produced Water Treatment", and the evaluation index was oil content, and the oil removal rate was calculated.

[0084] The object of evaluation is the sewage from a joint station of Shengli Oilfield, which contains 185mg / L oil, 98mg / L suspended solids, 29000mg / L mineralization and 70℃ temperature.

[0085] The AN-249 degreasing agent produced by Hebei Annuo Environmental Protection Technology Co., Ltd. was used for comparative experiments. The experimental results are shown in Table 1.

[0086] Table 1 Degreasing agent oil removal rate test results

[0087]

[0088]

[0089] From Table 1 we can see that:

[0090] (1) Degreasing agent H of the present invention 1-11 The oil removal rate reached over 83% when the concentration was 2mg / L, and the highest reached 91.0%; while the oil removal rate of AN-249 was 65.9% when the concentration was 2mg / L;

[0091] (2) Degreasing agent H of the present invention 1-11The oil removal rate reached over 92% when the concentration was 4 mg / L, and the highest reached 95.7%; while the oil removal rate of AN-249 was 86% when the concentration was 4 mg / L;

[0092] (3) Degreasing agent H of the present invention 1-11 When the concentration was 6 mg / L, the oil removal rate reached over 98.5%, with the highest reaching 99.5%; while the oil removal rate of AN-249 was 90.8% when the concentration was 6 mg / L.

[0093] Test Example 2 Evaluation of Flocculation Effect

[0094] The present invention was diluted into a 100 mg / L solution, and the deoiling agent was added according to effective concentrations of 2, 4, and 6 mg / L. The evaluation method referred to Q / SH10201356-2016 "General Technical Conditions for Flocculants for Conventional Produced Water Treatment in Oilfields", and the evaluation index was suspended matter, and the flocculation rate was calculated.

[0095] The object of evaluation is the sewage from a joint station of Shengli Oilfield, which contains 185mg / L oil, 98mg / L suspended solids, 29000mg / L mineralization and 70℃ temperature.

[0096] The AN-249 degreasing agent produced by Hebei Annuo Environmental Protection Technology Co., Ltd. was used for comparative experiments. The experimental results are shown in Table 2.

[0097] Table 2 Degreasing agent flocculation rate test results

[0098] Degreaser 2mg / L,% 4mg / L,% 6mg / L,% <![CDATA[H1]]> 79 85.9 96.5 <![CDATA[H2]]> 81.1 86.8 96.5 <![CDATA[H3]]> 80 85.6 96.6 <![CDATA[H4]]> 81.3 86.7 96.8 <![CDATA[H5]]> 83.8 87.8 96.9 <![CDATA[H6]]> 85 88.1 97.3 <![CDATA[H7]]> 85.4 88.9 97.8 <![CDATA[H8]]> 85.7 90.8 97.7 <![CDATA[H9]]> 85.5 90.8 97.6 <![CDATA[H 10 ]]> 86 91.4 98.1 <![CDATA[H 11 ]]> 85.3 91.5 98.5 AN-249 44 63.1 71

[0099] From Table 2 we can see that:

[0100] (1) Degreasing agent H of the present invention 1-11 The flocculation rate reached more than 78% when the concentration was 2 mg / L, and the highest reached 86%; while the flocculation rate of AN-249 was 44% when the concentration was 2 mg / L;

[0101] (2) Degreasing agent H of the present invention 1-11 The flocculation rate reached over 85% when the concentration was 4 mg / L, and the highest reached 91.5%; while the flocculation rate of AN-249 was 63.1% when the concentration was 4 mg / L;

[0102] (3) Degreasing agent H of the present invention 1-11 When the concentration was 6 mg / L, the flocculation rate was over 96%, with the highest reaching 98.5%; while the flocculation rate of AN-249 was 71.0% when the concentration was 6 mg / L.

[0103] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A method for preparing a sewage degreasing agent, characterized in that: The preparation method comprises: (1) purging the reactor and pipelines with nitrogen, adding acryloyloxyethyl dimethylbenzyl ammonium chloride, 2-(allyldimethylsilyl)pyridine, 1-vinyl-3-methylimidazole trifluoromethanesulfonate, emulsifier, buffer salt, and distilled water in sequence, stirring evenly, and adjusting the pH to 7-8 with sodium hydroxide solution; (2) Add the initiator solution into the high-position dropping tank and slowly drip it into the reactor. The initiator dripping time is controlled at 60-120 min. After the dripping is completed, continue to heat to 50-60° C., keep the temperature for reaction, cool to below 35° C., adjust the pH to 7-8 with sodium hydroxide solution, and obtain a viscous liquid; (3) drying and granulating the viscous liquid to obtain a degreasing agent; Based on 1 mole part of acryloyloxyethyl dimethylbenzyl ammonium chloride, the amounts of 2-(allyldimethylsilyl)pyridine and 1-vinyl-3-methylimidazole trifluoromethanesulfonate are 0.1-0.3 mole parts and 0.2-0.8 mole parts respectively.

2. The method for preparing a sewage degreasing agent according to claim 1, characterized in that: In step (1), the emulsifier is one of TX-10 (nonylphenol polyoxyethylene ether) and SPAN-60 (sorbitan monostearate), and the weight ratio of the emulsifier to acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.02-0.04:

1.

3. The method for preparing a sewage degreasing agent according to claim 1, characterized in that: In step (1), the buffer salt is one of sodium dihydrogen phosphate, potassium dihydrogen phosphate, ammonium dihydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, and diammonium hydrogen phosphate, and the weight ratio of the buffer salt to acryloyloxyethyl dimethylbenzyl ammonium chloride is 0.01-0.05:

1.

4. The method for preparing a sewage degreasing agent according to claim 1, characterized in that: In step (2), the initiator is one of peroxides, azo compounds, and redox initiators, and the weight ratio of the initiator to acryloyloxyethyl dimethylbenzyl ammonium chloride is 0.05-0.2:

1.

5. The method for preparing a sewage degreasing agent according to claim 4, characterized in that: The peroxide is one of hydrogen peroxide, sodium peroxide and peracetic acid.

6. The method for preparing a sewage degreasing agent according to claim 4, characterized in that: The azo compounds are azobisisobutyronitrile or azobisisoheptanenitrile.

7. The method for preparing a sewage degreasing agent according to claim 4, characterized in that: The redox type is one of a mixture of potassium persulfate + sodium sulfite, a mixture of sodium persulfate + sodium sulfite, and a mixture of ammonium persulfate + sodium sulfite.

8. The method for preparing a sewage degreasing agent according to claim 1, characterized in that: In step (2), the insulation reaction time is 1-4h.

9. The degreasing agent prepared by the preparation method according to any one of claims 1 to 8, characterized in that: The degreasing agent molecular formula is as follows: Wherein, x=10000-100000; y=2000-20000; z=5000-50000。 10. The degreasing agent according to claim 9, characterized in that The viscosity average molecular weight of the degreasing agent is 10,000,000-20,000,000.

Citation Information

Patent Citations

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