CN111018176A - Demulsifier, preparation method and application thereof - Google Patents
Demulsifier, preparation method and application thereof Download PDFInfo
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- CN111018176A CN111018176A CN201911273141.XA CN201911273141A CN111018176A CN 111018176 A CN111018176 A CN 111018176A CN 201911273141 A CN201911273141 A CN 201911273141A CN 111018176 A CN111018176 A CN 111018176A
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- polyether
- demulsifier
- ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a demulsifier, a preparation method and application thereof. The material is prepared from the following raw materials in percentage by mass: 1-40% of dodecyl dimethyl benzyl ammonium chloride, 3-50% of dimethyl diallyl ammonium chloride, 0.3-5% of an initiator, 1-35% of polymeric aluminum ferric silicate, 1-20% of ferrous sulfate, 641-3% of polyether L, 78-5% of polyether F680.5 and 10-70% of water; the sum of the mass percentages of the components is 100 percent. The demulsifier can effectively demulsify emulsion wastewater and oily sewage to eliminate high-concentration COD in industrial wastewater, the COD content in the treated wastewater is below 500mg/L, the concentration of the COD in the wastewater is greatly reduced, the operation is very simple, only the pH range of the wastewater is required to be adjusted, and then the agent is added into the wastewater according to a proportion and stirred for several minutes, so that the cost is low, the safety is high, and the secondary pollution to a water body is extremely low.
Description
Technical Field
The invention relates to the technical field of sewage treatment in environmental treatment, in particular to a demulsifier for removing COD (chemical oxygen demand) in emulsion wastewater and oil field oily sewage, and a preparation method and application thereof.
Background
With the continuous acceleration of the industrialized pace of China, the living standard of people is gradually improved, and the consumption of water resources is increased day by day. The demand of industrial water and domestic water is increasing, the produced waste water and sewage are increasing, the components of water pollutants are more and more complex, the contents of organic matters, COD and the like in the water body are seriously exceeded, the eutrophication of the water body is caused, the phenomenon of milk river, ink river, orange juice river or toxic water river appears in part of river channels sometimes, and the serious harm is formed to the drinking water source, so the control of water pollution and eutrophication, and the improvement of water quality are important problems in the technical field of water treatment.
The treatment of oily wastewater, especially high-salinity high-concentration emulsion wastewater and oily sewage in oil fields, is always a problem concerned by a plurality of domestic environmental protection workers and management departments, along with the rapid development of chemical industry in China, various novel chemical products are applied to various industries, especially heavy pollution such as medicine, chemical industry, oil extraction in oil fields, electroplating, printing and dyeing, and the like, and the increasingly serious environmental pollution problem is brought while the product quality is improved, which is mainly shown in that: the organic pollutants in the wastewater have high concentration, stable structure and poor biodegradability, the conventional process is difficult to realize standard emission, the treatment cost is high, and great pressure is brought to energy conservation and emission reduction of enterprises.
The method for treating the emulsion wastewater and the oily sewage comprises the following steps: biological methods, oxidation methods, electrochemical methods, adsorption methods, and the like. The common process and the traditional water treatment chemicals are difficult to achieve the expected effect when solving the problems of high COD concentration, high toxicity and poor biodegradability in industrial wastewater (sewage). At present, most of COD removal of sewage in sewage treatment plants is carried out by a biological method, the designed COD content in inlet water is 500mg/L, the COD content in industrial wastewater is 10000-50000mg/L, and some wastewater is possibly higher, and the fundamental problem cannot be solved by the biological method.
Disclosure of Invention
The invention aims to provide a demulsifier, a preparation method and application thereof, so as to solve the technical problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
the demulsifier is prepared from the following raw materials in percentage by mass: 1-40% of dodecyl dimethyl benzyl ammonium chloride, 3-50% of dimethyl diallyl ammonium chloride, 0.3-5% of an initiator, 1-35% of polymeric aluminum ferric silicate, 1-20% of ferrous sulfate, 641-3% of polyether L, 78-5% of polyether F680.5 and 10-70% of water; the sum of the mass percentages of the raw material components is 100%.
As a further scheme of the invention, the demulsifier is prepared from the following raw materials in percentage by mass: 5-30% of dodecyl dimethyl benzyl ammonium chloride, 10-50% of dimethyl diallyl ammonium chloride, 1-5% of an initiator, 5-30% of polymeric ferric aluminum silicate, 2-15% of ferrous sulfate, 641-3% of polyether, F680.5-5% of polyether and 10-70% of water; the sum of the mass percentages of the raw material components is 100%.
As a further scheme of the invention, the demulsifier is prepared from the following raw materials in percentage by mass: 10-20% of dodecyl dimethyl benzyl ammonium chloride, 20-45% of dimethyl diallyl ammonium chloride, 1-4% of an initiator, 10-20% of polymeric ferric aluminum silicate, 5-10% of ferrous sulfate, 641-3% of polyether, F682-5% of polyether and 20-50% of water; the sum of the mass percentages of the raw material components is 100%.
As a further scheme of the invention, the demulsifier is prepared from the following raw materials in percentage by mass: 15% of dodecyl dimethyl benzyl ammonium chloride, 30% of dimethyl diallyl ammonium chloride, 2% of initiator, 15% of polymeric aluminum ferric silicate, 7% of ferrous sulfate, 642% of polyether L, 683.5% of polyether F and 25.5% of water.
As a further aspect of the invention, the initiator is sodium peroxide.
The preparation method of the demulsifier comprises the following steps: mixing dimethyl diallyl ammonium chloride and an initiator according to the formula amount, adding the mixture into water according to the formula amount, heating to 65 ℃, and stirring for reacting for 180 minutes; and sequentially adding dodecyl dimethyl benzyl ammonium chloride, polymeric aluminum ferric silicate and ferrous sulfate according to the formula amount, uniformly stirring, simultaneously heating to 100 ℃, adding polyether L64 and polyether F68 according to the formula amount, stirring for reacting for 120 minutes, and finally cooling to room temperature to obtain the demulsifier product.
The demulsifier is applied to the treatment of high-concentration emulsion wastewater and high-oil-content industrial sewage.
The invention has the beneficial effects that: the demulsifier can effectively demulsify emulsion wastewater and oily sewage to eliminate high-concentration COD in industrial wastewater, the COD content in the treated wastewater is below 500mg/L, the concentration of the COD in the wastewater is greatly reduced, the operation is very simple, only the pH range of the wastewater is required to be adjusted, and then the agent is added into the wastewater according to a proportion and stirred for several minutes, so that the cost is low, the safety is high, and the secondary pollution to a water body is extremely low.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The demulsifier is prepared by the following steps: mixing 30% of dimethyl diallyl ammonium chloride and 2% of initiator, adding the mixture into 25.5% of water, heating to 65 ℃, stirring for reaction for 180 minutes, sequentially adding 15% of dodecyl dimethyl benzyl ammonium chloride, 15% of polymeric aluminum ferric silicate and 7% of ferrous sulfate, uniformly stirring, simultaneously heating to 100 ℃, adding 2% of polyether L64 and 3.5% of polyether F68, stirring for reaction for 120 minutes, and finally cooling to room temperature to obtain the demulsifier product.
Adding 1% of the demulsifier product into the emulsion wastewater with the measured COD concentration of 35700mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the water layer is 2050 mg/L; and adding 1% of the demulsifier product into the oil field oil-containing wastewater with the measured COD concentration of 10500mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the obtained water layer is 2583 mg/L.
Example 2
The demulsifier is prepared by the following steps: mixing 30% of dimethyl diallyl ammonium chloride and 2% of initiator, adding the mixture into 25.5% of water, heating to 80 ℃, stirring for reaction for 120 minutes, sequentially adding 15% of dodecyl dimethyl benzyl ammonium chloride, 15% of polymeric aluminum ferric silicate and 7% of ferrous sulfate, uniformly stirring, simultaneously heating to 100 ℃, adding 2% of polyether L64 and 3.5% of polyether F68, stirring for reaction for 120 minutes, and finally cooling to room temperature to obtain the demulsifier product.
Adding 1% of the demulsifier product into the emulsion wastewater with the measured COD concentration of 35700mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the water layer is 3730 mg/L; and adding 1% of the demulsifier product into the oil field oil-containing wastewater with the measured COD concentration of 10500mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the water layer is 2396 mg/L.
Example 3
The demulsifier is prepared by the following steps: mixing 25% of dimethyl diallyl ammonium chloride and 2% of initiator, adding the mixture into 20% of water, heating to 65 ℃, stirring for reaction for 180 minutes, sequentially adding 20% of dodecyl dimethyl benzyl ammonium chloride, 15% of polymeric aluminum ferric silicate and 7% of ferrous sulfate, uniformly stirring, simultaneously heating to 100 ℃, adding 5% of polyether L64 and 6% of polyether F68, stirring for reaction for 120 minutes, and finally cooling to room temperature to obtain the demulsifier product.
Adding 1% of the demulsifier product into the emulsion wastewater with the measured COD concentration of 35700mg, stirring for 5-10min, standing for 10min, and detecting the COD of the obtained water layer to be 1760 mg/L; and adding 1% of the demulsifier product into the oil field oil-containing wastewater with the COD concentration of 10500mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the water layer is 1570 mg/L.
Example 4
The demulsifier is prepared by the following steps: mixing 40% of dimethyl diallyl ammonium chloride and 1.5% of initiator, adding the mixture into 25.5% of water, heating to 65 ℃, stirring for reaction for 180 minutes, sequentially adding 10% of dodecyl dimethyl benzyl ammonium chloride, 8% of polymeric aluminum ferric silicate and 5% of ferrous sulfate, stirring uniformly, simultaneously heating to 100 ℃, adding 5% of polyether L64 and 5% of polyether F68, stirring for reaction for 120 minutes, and finally cooling to room temperature to obtain the demulsifier product.
Adding 1% of the demulsifier product into the emulsion wastewater with the measured COD concentration of 35700mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the water layer is 3281 mg/L; and adding 1% of the demulsifier product into the oil field oil-containing wastewater with the measured COD concentration of 10500mg, stirring for 5-10min, standing for 10min, and detecting that the COD of the obtained water layer is 2860 mg/L.
The demulsifier disclosed by the invention is mainly prepared by compounding dodecyl dimethyl benzyl ammonium chloride and dimethyl diallyl ammonium chloride and modifying by polyether L64 and polyether F68, so that the demulsifier can better demulsify W/O type and O/W type emulsions in high-concentration emulsion wastewater and industrial oil-containing wastewater, and organic matter particles after demulsification are rapidly flocculated and precipitated under the action of polymeric ferric aluminum silicate and ferrous sulfate. Thereby achieving the purpose of sewage purification. The demulsifier provided by the invention can effectively solve the problems of high COD content and difficult removal in emulsion wastewater and industrial oily wastewater.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The demulsifier is characterized by being prepared from the following raw materials in percentage by mass: 1-40% of dodecyl dimethyl benzyl ammonium chloride, 3-50% of dimethyl diallyl ammonium chloride, 0.3-5% of an initiator, 1-35% of polymeric aluminum ferric silicate, 1-20% of ferrous sulfate, 641-3% of polyether L, 78-5% of polyether F680.5 and 10-70% of water; the sum of the mass percentages of the raw material components is 100%.
2. The demulsifier of claim 1, which is prepared from the following raw materials in percentage by mass: 5-30% of dodecyl dimethyl benzyl ammonium chloride, 10-50% of dimethyl diallyl ammonium chloride, 1-5% of an initiator, 5-30% of polymeric ferric aluminum silicate, 2-15% of ferrous sulfate, 641-3% of polyether, F680.5-5% of polyether and 10-70% of water; the sum of the mass percentages of the raw material components is 100%.
3. The demulsifier of claim 1, which is prepared from the following raw materials in percentage by mass: 10-20% of dodecyl dimethyl benzyl ammonium chloride, 20-45% of dimethyl diallyl ammonium chloride, 1-4% of an initiator, 10-20% of polymeric ferric aluminum silicate, 5-10% of ferrous sulfate, 641-3% of polyether, F682-5% of polyether and 20-50% of water; the sum of the mass percentages of the raw material components is 100%.
4. The demulsifier of claim 1, which is prepared from the following raw materials in percentage by mass: 15% of dodecyl dimethyl benzyl ammonium chloride, 30% of dimethyl diallyl ammonium chloride, 2% of initiator, 15% of polymeric aluminum ferric silicate, 7% of ferrous sulfate, 642% of polyether L, 683.5% of polyether F and 25.5% of water.
5. The demulsifier of any one of claims 1-4, wherein the initiator is sodium peroxide.
6. The method for preparing the demulsifier of any one of claims 1-4, comprising the steps of: mixing dimethyl diallyl ammonium chloride and an initiator according to the formula amount, adding the mixture into water according to the formula amount, heating to 65 ℃, and stirring for reacting for 180 minutes; and sequentially adding dodecyl dimethyl benzyl ammonium chloride, polymeric aluminum ferric silicate and ferrous sulfate according to the formula amount, uniformly stirring, simultaneously heating to 100 ℃, adding polyether L64 and polyether F68 according to the formula amount, stirring for reacting for 120 minutes, and finally cooling to room temperature to obtain the demulsifier product.
7. An application of demulsifier in treating the high-concentration emulsified liquid waste water and high-oil-content industrial sewage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911273141.XA CN111018176A (en) | 2019-12-12 | 2019-12-12 | Demulsifier, preparation method and application thereof |
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| CN201911273141.XA CN111018176A (en) | 2019-12-12 | 2019-12-12 | Demulsifier, preparation method and application thereof |
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| CN111018176A true CN111018176A (en) | 2020-04-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113651392A (en) * | 2021-08-23 | 2021-11-16 | 天津开放大学 | Preparation method of composite demulsifying bactericide for oily wastewater |
| CN114891156A (en) * | 2022-06-14 | 2022-08-12 | 南京理工大学 | Series methyl alkyl substituent diallyl ammonium chloride copolymer demulsifier and preparation method thereof |
Citations (7)
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| US5560832A (en) * | 1995-05-08 | 1996-10-01 | Nalco Chemical Company | Demulsification of oily waste waters using silicon containing polymers |
| US20060289359A1 (en) * | 2005-06-23 | 2006-12-28 | Manek Maria B | Method of clarifying oily waste water |
| CN102807890A (en) * | 2012-08-31 | 2012-12-05 | 句容宁武高新技术发展有限公司 | Method for preparing demulsifier |
| CN103484151A (en) * | 2013-10-14 | 2014-01-01 | 句容宁武高新技术发展有限公司 | Synthesis method of cationic-polymer-modified crude oil demulsifier |
| CN103525455A (en) * | 2013-10-14 | 2014-01-22 | 江苏大学 | Cationic polymer modified crude oil demulsifying agent |
| CN105253974A (en) * | 2015-10-30 | 2016-01-20 | 广州振清环保技术有限公司 | Invert-demulsion coagulating agent, preparation method of invert-demulsion coagulating agent and application of invert-demulsion coagulating agent |
| CN110041474A (en) * | 2019-04-15 | 2019-07-23 | 中国海洋石油集团有限公司 | A kind of hybrid cation reverse-phase emulsifier and the preparation method and application thereof |
-
2019
- 2019-12-12 CN CN201911273141.XA patent/CN111018176A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5560832A (en) * | 1995-05-08 | 1996-10-01 | Nalco Chemical Company | Demulsification of oily waste waters using silicon containing polymers |
| US20060289359A1 (en) * | 2005-06-23 | 2006-12-28 | Manek Maria B | Method of clarifying oily waste water |
| CN102807890A (en) * | 2012-08-31 | 2012-12-05 | 句容宁武高新技术发展有限公司 | Method for preparing demulsifier |
| CN103484151A (en) * | 2013-10-14 | 2014-01-01 | 句容宁武高新技术发展有限公司 | Synthesis method of cationic-polymer-modified crude oil demulsifier |
| CN103525455A (en) * | 2013-10-14 | 2014-01-22 | 江苏大学 | Cationic polymer modified crude oil demulsifying agent |
| CN105253974A (en) * | 2015-10-30 | 2016-01-20 | 广州振清环保技术有限公司 | Invert-demulsion coagulating agent, preparation method of invert-demulsion coagulating agent and application of invert-demulsion coagulating agent |
| CN110041474A (en) * | 2019-04-15 | 2019-07-23 | 中国海洋石油集团有限公司 | A kind of hybrid cation reverse-phase emulsifier and the preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113651392A (en) * | 2021-08-23 | 2021-11-16 | 天津开放大学 | Preparation method of composite demulsifying bactericide for oily wastewater |
| CN114891156A (en) * | 2022-06-14 | 2022-08-12 | 南京理工大学 | Series methyl alkyl substituent diallyl ammonium chloride copolymer demulsifier and preparation method thereof |
| CN114891156B (en) * | 2022-06-14 | 2022-12-06 | 南京理工大学 | Series methyl alkyl substituent diallyl ammonium chloride copolymer demulsifier and preparation method thereof |
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Application publication date: 20200417 |