CN109607901B - Waste emulsion freezing and demulsifying method - Google Patents
Waste emulsion freezing and demulsifying method Download PDFInfo
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- CN109607901B CN109607901B CN201811616114.3A CN201811616114A CN109607901B CN 109607901 B CN109607901 B CN 109607901B CN 201811616114 A CN201811616114 A CN 201811616114A CN 109607901 B CN109607901 B CN 109607901B
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- waste emulsion
- freezing
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- 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
- B01D17/0208—Separation of non-miscible liquids by sedimentation
- B01D17/0214—Separation of non-miscible liquids by sedimentation with removal of one of the phases
-
- 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
- B01D17/042—Breaking emulsions by changing the temperature
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/22—Treatment of water, waste water, or sewage by freezing
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (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)
- Processing Of Solid Wastes (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a waste emulsion freezing and demulsifying method, which comprises the following steps: (1) filtering the waste emulsion by using a bag filter; (2) adding a hydrophilic material bag into the waste emulsion filtered by the bag filter, and standing for a period of time to reduce the moisture content in the waste emulsion; (3) filtering the waste emulsion added with the hydrophilic material by using a screen to remove a hydrophilic material bag; (4) adjusting the pH value of the waste emulsion from which the hydrophilic material bag is removed to 6-8, and filtering the waste emulsion by using a tubular membrane filter; (5) adding sodium chloride into the waste emulsion filtered by the tubular membrane filter, and freezing the waste emulsion at a certain temperature for a period of time to completely freeze the waste emulsion; (6) taking out the frozen waste emulsion, standing and thawing at room temperature until oil and water are layered. The waste emulsion freezing and demulsifying method combines the adsorption of the hydrophilic material with the freezing and demulsifying, and can reduce the volume of the refrigerating fluid and reduce the energy consumption.
Description
Technical Field
The invention belongs to the field of emulsion wastewater treatment, and particularly relates to a waste emulsion freezing demulsification method.
Background
In the daily production, manufacturing, machining, grinding and the like, the surfaces of metals and machine parts are often lubricated and cooled by using cooling lubricating liquid. In the using process, the performance of the cooling and lubricating liquid is gradually reduced due to oxidation and rancidity, and the cooling and lubricating effect is finally lost to form waste emulsion. If the waste emulsified oil generated in the process is directly taken to be used for wastewater treatment, the cost is very high, the cost can reach about 4000 yuan/ton in Tianjin area, and the cost is very high for wastewater treatment every year in individual areas of China even up to 8000 yuan/ton.
The waste emulsion is waste liquid generated in the machining process, and has high pollutant concentration, high treatment difficulty and high treatment cost. The method of adding medicines to demulsify is generally adopted, so that a large amount of medicines are consumed, and a large amount of solid waste is generated. The demulsification mechanism of freezing and thawing is that because the freezing point of water is higher, freezing crystallization firstly occurs, so that emulsifier molecules are adsorbed on the surface of ice crystals and are melted in oil, and the concentration of a surfactant on an oil-water interface film is reduced, thereby achieving the purpose of demulsification. By adopting a freezing demulsification method, the emulsion or the concentrated solution of the emulsion after membrane filtration can realize oil-water separation without adding any demulsifier, the treatment cost is low, and the separated oil can be recycled.
Disclosure of Invention
In view of the above, the present invention aims to provide a waste emulsion freezing and demulsifying method, which overcomes the defects of the prior art, and combines the adsorption of hydrophilic materials with freezing and demulsifying to reduce the volume of freezing liquid and reduce energy consumption.
A waste emulsion freezing demulsification method comprises the following steps:
(1) filtering the waste emulsion by using a bag filter to remove hard solid impurities;
(2) adding a hydrophilic material bag into the waste emulsion filtered by the bag filter, standing for a period of time, and reducing the water content in the waste emulsion by adsorbing water by the hydrophilic material;
(3) filtering the waste emulsion added with the hydrophilic material by using a screen to remove a hydrophilic material bag;
(4) adjusting the pH value of the waste emulsion from which the hydrophilic material bag is removed to 6-8, and filtering the waste emulsion by using a tubular membrane filter;
(5) adding sodium chloride into the waste emulsion filtered by the tubular membrane filter, and freezing the waste emulsion at a certain temperature for a period of time to completely freeze the waste emulsion;
(6) taking out the frozen waste emulsion, standing and thawing at room temperature until oil and water are layered.
Preferably, the waste emulsion freezing and demulsification method further comprises the step of centrifugally separating the water phase after oil-water separation.
Preferably, in step (1), the filtration pore size of the bag filter is 300 μm.
Preferably, in the step (2), the hydrophilic material bag is a high molecular water-absorbing resin wrapped with hydrophilic non-woven fabric.
Preferably, in step (3), the pH of the waste emulsion is adjusted with sodium hydroxide and sulfuric acid.
Preferably, in the step (5), the addition amount of sodium chloride is 1 mol/L.
Preferably, in the step (6), the freezing temperature is-30-5 ℃, the freezing time is 8-40h, and the time required for standing and unfreezing at room temperature until the delamination boundary is obvious is 48-60 h.
The waste emulsion is an emulsion in a full emulsion state.
Compared with the prior art, the waste emulsion freezing and demulsifying method has the following advantages:
the waste emulsion freezing and demulsifying method combines the adsorption of the hydrophilic material with the freezing and demulsifying, firstly utilizes the hydrophilic material to adsorb partial water in the waste emulsion before freezing, and then freezes after filtering, thereby reducing the volume of the freezing liquid and reducing the energy consumption.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
A waste emulsion freezing demulsification method comprises the following steps: filtering the waste emulsion by using a 300-micron precision bag filter to remove solid impurities such as hard iron and the like; adding the macromolecular water-absorbing resin wrapped by the hydrophilic non-woven fabric into the waste emulsion filtered by the bag filter, standing for 1h, and adsorbing water by the hydrophilic non-woven fabric and the macromolecular water-absorbing resin to reduce the water content in the waste emulsion; then, filtering the waste emulsion added with the hydrophilic material by using a screen to remove the macromolecular water-absorbing resin wrapped by the hydrophilic non-woven fabric, wherein the volume of the waste emulsion is greatly reduced; then, adjusting the pH value of the waste emulsion removed from the hydrophilic material bag to 7 by using sodium hydroxide and sulfuric acid, and filtering the waste emulsion by using a tubular membrane filter; then adding sodium chloride into the waste emulsion filtered by the tubular membrane filter to ensure that the concentration of the waste emulsion is 1mol/L, and freezing the waste emulsion at the temperature of minus 7 ℃ for 8 hours to completely freeze the waste emulsion; then taking out the frozen waste emulsion, standing at room temperature for 50h, and thawing until oil and water are layered; and finally, carrying out centrifugal separation on the water phase after oil-water separation.
In the above process, the search process of different freezing temperatures is: the water samples are respectively frozen for 8 hours at the temperature of-7-0 ℃, and the freezing effect of the water samples is shown in table 1. The wastewater sample was a white emulsion at room temperature. When the ambient temperature is lower than-5 ℃, the water sample can be completely frozen and turns into yellow opaque solid.
TABLE 1 freezing Effect at different temperatures
Therefore, the freezing temperature was selected to be-7 ℃.
In the process, the investigation on the unfreezing time of the frozen water sample at room temperature comprises the following steps:
after the frozen water sample is stood and thawed at room temperature, the water sample is divided into two layers, namely a lower white emulsion and an upper yellow liquid with a white turbid phase. The two-phase interface of a water sample which is just thawed is poor in scale division, the layering is more obvious after the water sample is stood for 24 hours at room temperature, the two-phase interface is very clear after the water sample is stood for 48 hours, and the upper layer of the water sample is reddish brown and the turbidity is reduced.
Therefore, it is preferable to select the freezing temperature for 48 hours or more.
Example 2
A method for freezing and demulsifying waste emulsion, which is basically the same as the embodiment 1, except that: the freezing temperature is-20 ℃, the freezing time is 10h, and the room temperature thawing time is 55 h.
Comparative example 1
A freezing demulsification method directly freezes waste emulsion at-7 deg.C for 8h, and then unfreezes at normal temperature for 48h until oil and water are layered.
Comparative example 2
A method of freeze demulsification substantially as described in example 1, except that: the step of filtering with a bag filter and the step of treating with a hydrophilic nonwoven cloth-wrapped high molecular water-absorbing resin are eliminated.
Comparative example 3
A method of demulsifying a frozen emulsion, substantially as described in example 1, except that: the step of centrifugation was eliminated.
The oil content in the final aqueous phase of examples 1 and 2, comparative examples 1-3 was measured and found to be 88%, 86%, 71%, 80% and 82%, respectively.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A waste emulsion freezing demulsification method is characterized by comprising the following steps: the method comprises the following steps:
(1) filtering the waste emulsion by using a bag filter to remove hard solid impurities;
(2) adding a hydrophilic material bag into the waste emulsion filtered by the bag filter, standing for a period of time, and reducing the water content in the waste emulsion by adsorbing water by the hydrophilic material;
(3) filtering the waste emulsion added with the hydrophilic material by using a screen to remove a hydrophilic material bag;
(4) adjusting the pH value of the waste emulsion from which the hydrophilic material bag is removed to 6-8, and filtering the waste emulsion by using a tubular membrane filter;
(5) adding sodium chloride into the waste emulsion filtered by the tubular membrane filter, and freezing the waste emulsion at a certain temperature for a period of time to completely freeze the waste emulsion;
(6) taking out the frozen waste emulsion, standing and thawing at room temperature until oil and water are layered.
2. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: also comprises a step of separating the water phase after oil-water separation by centrifugation.
3. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: in the step (1), the filtering pore size of the bag filter is 300 microns.
4. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: in the step (2), the hydrophilic material bag is made of high molecular water-absorbing resin wrapped by hydrophilic non-woven fabric.
5. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: in the step (3), the pH of the waste emulsion is adjusted by using sodium hydroxide and sulfuric acid.
6. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: in the step (5), the addition amount of sodium chloride is 1 mol/L.
7. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: in the step (6), the freezing temperature is-30 to-5 ℃, the freezing time is 8 to 40 hours, and the time required for standing and unfreezing at room temperature until the layering limit is obvious is 48 to 60 hours.
8. The method for freezing and demulsifying waste emulsion as claimed in claim 1, wherein: the waste emulsion is an emulsion in a full emulsion state.
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| CN201811616114.3A CN109607901B (en) | 2018-12-27 | 2018-12-27 | Waste emulsion freezing and demulsifying method |
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| CN201811616114.3A CN109607901B (en) | 2018-12-27 | 2018-12-27 | Waste emulsion freezing and demulsifying method |
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| CN109607901B true CN109607901B (en) | 2021-05-04 |
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| CN110028201A (en) * | 2019-05-08 | 2019-07-19 | 杭州齐创环境工程有限公司 | A kind of waste emulsified mixture resource utilization processing system and technique |
| CN112305176A (en) * | 2020-12-04 | 2021-02-02 | 中铝东南材料院（福建）科技有限公司 | Method for detecting concentration of emulsion for hot aluminum rolling |
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| CN205133521U (en) * | 2015-11-27 | 2016-04-06 | 广州中万环保科技有限公司 | Useless emulsion purification unit |
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| CN106902551A (en) * | 2017-03-31 | 2017-06-30 | 昆明理工大学 | A kind of breaking method of emulsion |
| CN108689529A (en) * | 2017-04-06 | 2018-10-23 | 华东理工大学 | A kind of method of suspension crystallization and freeze-thaw Combined Treatment used cutting liquid |
| CN109607919A (en) * | 2018-12-27 | 2019-04-12 | 天津海普尔膜科技有限公司 | A kind of waste emulsified mixture high temperature breaking method |
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- 2018-12-27 CN CN201811616114.3A patent/CN109607901B/en active Active
Patent Citations (6)
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| CN103043838A (en) * | 2012-12-26 | 2013-04-17 | 大连春兴科技股份有限公司 | Freezing and thawing treatment method for suspended wastewater |
| CN205133521U (en) * | 2015-11-27 | 2016-04-06 | 广州中万环保科技有限公司 | Useless emulsion purification unit |
| CN106495362A (en) * | 2016-12-07 | 2017-03-15 | 云南大地绿坤环保科技有限公司 | A kind of breaking method of waste emulsified mixture |
| CN106902551A (en) * | 2017-03-31 | 2017-06-30 | 昆明理工大学 | A kind of breaking method of emulsion |
| CN108689529A (en) * | 2017-04-06 | 2018-10-23 | 华东理工大学 | A kind of method of suspension crystallization and freeze-thaw Combined Treatment used cutting liquid |
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