CN105540738A - Efficient demulsifier and preparation method and application thereof - Google Patents
Efficient demulsifier and preparation method and application thereof Download PDFInfo
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- CN105540738A CN105540738A CN201510957508.5A CN201510957508A CN105540738A CN 105540738 A CN105540738 A CN 105540738A CN 201510957508 A CN201510957508 A CN 201510957508A CN 105540738 A CN105540738 A CN 105540738A
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- emulsion splitter
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- polygala root
- extracting solution
- formalin
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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
Abstract
The present invention discloses an efficient demulsifier and a preparation method and application thereof, the demulsifier comprises the following components in parts by weight: 44-51 parts of poly diallyl terephthalate, 30-37 parts of polyvinyl alcohol, 5-13 parts of formalin, 100-108 parts of ethylene glycol monobutyl ether and 15-22 parts of a polygala tenuifolia extract liquid. The polygala tenuifolia extract liquid is obtained by crushing polygala tenuifolia, extracting with water and precipitating with an alcohol, eluting with a macroporous resin column and concentrating; the ethylene glycol monobutyl ether is heated, the polyvinyl alcohol is added, then the poly diallyl terephthalate is added, after heating treatment, cooling treatment is performed, the polygala tenuifolia extract liquid and the formalin are added for treatment, then cooling treatment is performed; and the mixture is cooled to room temperature to obtain the demulsifier. The the demulsifier has the advantages of easily obtained raw materials, low cost, good demulsification effect, simple preparation method, easy operation, less dosage, high temperature resistance, low temperature resistance, large dehydration amount, high dehydration speed, and the like, and is suitable for the field of industrial waste water, especially for wastewater containing waste oil in steel industry, coking industry, oil exploitation, machinery processing manufacturing and the like.
Description
Technical field
The present invention relates to emulsion splitter field, specifically a kind of emulsion splitter and its preparation method and application efficiently.
Background technology
Trade effluent refers to the waste water, sewage and the waste liquid that produce in Industrial processes, wherein containing the pollutent produced in the industrial production materials, intermediate product and the product that outflow with water and production process.Along with developing rapidly of industry, kind and the quantity of waste water rapidly increase, also increasingly extensive and serious to the pollution of water body, threaten the health and safety of the mankind.Therefore, for protection of the environment, the process of trade effluent is more even more important than the process of municipal effluent.The pollution that trade effluent causes mainly contains: organic aerobic Substances Pollution, and chemical toxicant pollutes, inoganic solids suspended solid pollutant, heavy metal contamination, acid pollution, alkali pollution, pollution of plant nutritions, thermal pollution, pathogen contamination etc.Many pollutents have color, stink or easily give birth to foam, and therefore trade effluent often presents unpleasant outward appearance, causes water body pollution in wide area, directly threatens the life and health of the people, therefore control trade effluent particularly important.Particularly steel industry, coking industry etc. can produce a large amount of materials containing waste oil class, this kind oil product oil is poor, water content is high, complicated component, containing mud, impurity such as lubrication lipid and moisture etc., most of smelter processing mode is landfill after outward transport, not only cannot directly utilize, and environmental pollution is very large.This processing mode is simply extensive, without economic benefit.
Summary of the invention
The object of the present invention is to provide that a kind of consumption is few, high temperature resistant, low temperature resistant, dehydrating amount is large, dewatering speed is fast, emulsion splitter and its preparation method and application efficiently, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
A kind of emulsion splitter efficiently, is made up of the following raw material according to weight part: poly terephthalic acid diallyl 44-51 part, polyvinyl alcohol 30-37 part, formalin 5-13 part, ethylene glycol monobutyl ether 100-108 part, polygala root extracting solution 15-22 part.
As the further scheme of the present invention: described efficient emulsion splitter, be made up of the following raw material according to weight part: poly terephthalic acid diallyl 46-49 part, polyvinyl alcohol 32-35 part, formalin 7-10 part, ethylene glycol monobutyl ether 104-106 part, polygala root extracting solution 17-20 part.
As the further scheme of the present invention: described efficient emulsion splitter, be made up of the following raw material according to weight part: poly terephthalic acid diallyl 48 parts, polyvinyl alcohol 33 parts, formalin 8 parts, ethylene glycol monobutyl ether 105 parts, polygala root extracting solution 18 parts.
The preparation method of described efficient emulsion splitter, is made up of following steps:
1) preparation process of polygala root extracting solution: after polygala root is pulverized, adopt water extraction and alcohol precipitation method, obtained condensed cream, the purified water of 6 times of volumes is added in condensed cream, limit edged stirs, leave standstill 1.2-1.5h, filter, filtrate is crossed macroporous resin column wash-out with 0.7-0.8BV/h flow velocity, obtained first elutriant is for subsequent use, by the volumetric concentration of 6 times of volumes be again 20% ethanol cross macroporous resin column wash-out with 0.7-0.8BV/h flow velocity, elutriant discards, macroporous resin column wash-out is crossed again with the ethanol that the volumetric concentration of 6 times of volumes is 85%, elution flow rate is 0.7-0.8BV/h, merge with first time elutriant, reclaim and merge ethanol in elutriant and the 10-15% being concentrated into original volume, obtain polygala root extracting solution,
2) ethylene glycol monobutyl ether is heated to 90-95 DEG C, low whipping speed is under the condition of 100-125r/min, add polyvinyl alcohol, continue to stir 15-20min at such a temperature, then add poly terephthalic acid diallyl and be warming up to 120-125 DEG C, stir 30-35min at such a temperature, then be cooled to 73-78 DEG C, add polygala root extracting solution and formalin, continue to stir 2-2.5h, be cooled to 55-58 DEG C again, stir 20-30min at such a temperature; Be down to room temperature and get final product.
Described efficient emulsion splitter is in the application preparing trade effluent emulsion splitter.
As the further scheme of the present invention: trade effluent is the trade effluent containing waste oil.
As the further scheme of the present invention: the adding consistency of emulsion splitter is 6-16ppm.
As the further scheme of the present invention: the adding consistency of emulsion splitter is 8-12ppm.
As the further scheme of the present invention: the adding consistency of emulsion splitter is 8ppm.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention has raw material and is easy to get, with low cost, demulsification is good, preparation method is simple, simple operation, gained emulsion splitter has that consumption is few, high temperature resistant, low temperature resistant, dehydrating amount is large and the advantage such as dewatering speed is fast, is applicable to trade effluent field, is specially adapted to the steel industry, coking industry, oilfield exploitation, mechanical workout production etc. of the waste water that can produce a large amount of waste water containing waste oil class.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of emulsion splitter efficiently, is made up of the following raw material according to weight part: poly terephthalic acid diallyl 44 parts, polyvinyl alcohol 30 parts, formalin 5 parts, ethylene glycol monobutyl ether 100 parts, polygala root extracting solution 15 parts.
The preparation process of polygala root extracting solution: after polygala root is pulverized, adopt water extraction and alcohol precipitation method, obtained condensed cream, the purified water of 6 times of volumes is added in condensed cream, limit edged stirs, leave standstill 1.2h, filter, filtrate is crossed macroporous resin column wash-out with 0.7BV/h flow velocity, obtained first elutriant is for subsequent use, by the volumetric concentration of 6 times of volumes be again 20% ethanol cross macroporous resin column wash-out with 0.7BV/h flow velocity, elutriant discards, macroporous resin column wash-out is crossed again with the ethanol that the volumetric concentration of 6 times of volumes is 85%, elution flow rate is 0.7BV/h, merge with first time elutriant, reclaim and merge ethanol in elutriant and be concentrated into 10% of original volume, obtain polygala root extracting solution.Ethylene glycol monobutyl ether is heated to 90 DEG C, low whipping speed is under the condition of 100r/min, add polyvinyl alcohol, continue to stir 15min at such a temperature, then add poly terephthalic acid diallyl and be warming up to 120 DEG C, stir 30min at such a temperature, then be cooled to 73 DEG C, add polygala root extracting solution and formalin, continue to stir 2h, be cooled to 55 DEG C again, stir 20min at such a temperature; Be down to room temperature and get final product.
Embodiment 2
In the embodiment of the present invention, a kind of emulsion splitter efficiently, is made up of the following raw material according to weight part: poly terephthalic acid diallyl 51 parts, polyvinyl alcohol 37 parts, formalin 13 parts, ethylene glycol monobutyl ether 108 parts, polygala root extracting solution 22 parts.
The preparation process of polygala root extracting solution: after polygala root is pulverized, adopt water extraction and alcohol precipitation method, obtained condensed cream, the purified water of 6 times of volumes is added in condensed cream, limit edged stirs, leave standstill 1.5h, filter, filtrate is crossed macroporous resin column wash-out with 0.8BV/h flow velocity, obtained first elutriant is for subsequent use, by the volumetric concentration of 6 times of volumes be again 20% ethanol cross macroporous resin column wash-out with 0.8BV/h flow velocity, elutriant discards, macroporous resin column wash-out is crossed again with the ethanol that the volumetric concentration of 6 times of volumes is 85%, elution flow rate is 0.8BV/h, merge with first time elutriant, reclaim and merge ethanol in elutriant and be concentrated into 15% of original volume, obtain polygala root extracting solution.Ethylene glycol monobutyl ether is heated to 95 DEG C, low whipping speed is under the condition of 125r/min, add polyvinyl alcohol, continue to stir 20min at such a temperature, then add poly terephthalic acid diallyl and be warming up to 125 DEG C, stir 35min at such a temperature, then be cooled to 78 DEG C, add polygala root extracting solution and formalin, continue to stir 2.5h, be cooled to 58 DEG C again, stir 30min at such a temperature; Be down to room temperature and get final product.
Embodiment 3
In the embodiment of the present invention, a kind of emulsion splitter efficiently, is made up of the following raw material according to weight part: poly terephthalic acid diallyl 46 parts, polyvinyl alcohol 32 parts, formalin 7 parts, ethylene glycol monobutyl ether 104 parts, polygala root extracting solution 17 parts.
The preparation process of polygala root extracting solution: after polygala root is pulverized, adopt water extraction and alcohol precipitation method, obtained condensed cream, the purified water of 6 times of volumes is added in condensed cream, limit edged stirs, leave standstill 1.4h, filter, filtrate is crossed macroporous resin column wash-out with 0.7BV/h flow velocity, obtained first elutriant is for subsequent use, by the volumetric concentration of 6 times of volumes be again 20% ethanol cross macroporous resin column wash-out with 0.7BV/h flow velocity, elutriant discards, macroporous resin column wash-out is crossed again with the ethanol that the volumetric concentration of 6 times of volumes is 85%, elution flow rate is 0.7BV/h, merge with first time elutriant, reclaim and merge ethanol in elutriant and be concentrated into 12% of original volume, obtain polygala root extracting solution.Ethylene glycol monobutyl ether is heated to 92 DEG C, low whipping speed is under the condition of 110r/min, add polyvinyl alcohol, continue to stir 17min at such a temperature, then add poly terephthalic acid diallyl and be warming up to 122 DEG C, stir 32min at such a temperature, then be cooled to 75 DEG C, add polygala root extracting solution and formalin, continue to stir 2.2h, be cooled to 57 DEG C again, stir 25min at such a temperature; Be down to room temperature and get final product.
Embodiment 4
In the embodiment of the present invention, a kind of emulsion splitter efficiently, is made up of the following raw material according to weight part: poly terephthalic acid diallyl 49 parts, polyvinyl alcohol 35 parts, formalin 10 parts, ethylene glycol monobutyl ether 106 parts, polygala root extracting solution 20 parts.
Preparation process is consistent with embodiment 3.
Embodiment 5
In the embodiment of the present invention, a kind of emulsion splitter efficiently, is made up of the following raw material according to weight part: poly terephthalic acid diallyl 48 parts, polyvinyl alcohol 33 parts, formalin 8 parts, ethylene glycol monobutyl ether 105 parts, polygala root extracting solution 18 parts.
Preparation process is consistent with embodiment 3.
Embodiment 6
The dehydrating effect producing a large amount of waste water containing waste oil class and carry out smelted by the emulsion splitter obtained by embodiment of the present invention 1-5 in experiment for certain Steel Plant.
Experimental temperature is 70 DEG C, and Water in oil 60.4%, experimental result is as shown in table 1.Simultaneously, also be provided with 3 groups of comparative examples, except not containing except polygala root extracting solution in comparative example 1, all the other proportionings are consistent with preparation process and embodiment 5, only containing polygala root extracting solution in comparative example 2, its preparation process is consistent with embodiment 5, and comparative example 3 is not except containing except formalin, and all the other proportionings are consistent with preparation process and embodiment 5.
The demulsification of the different emulsion splitter of table 1
As can be seen from Table 1, embodiment of the present invention 1-5 treatment effect is better than comparative example 1-3, illustrates that the present invention is worked under each component acting in conjunction.
Embodiment 7
In experiment, the embodiment gained emulsion splitter of different adding consistency is smelted the dehydrating effect producing a large amount of waste water containing waste oil class and carry out for certain Steel Plant.For embodiment 5 gained emulsion splitter.
Experimental temperature is 70 DEG C, and Water in oil 60.4%, experimental result is as shown in table 2.As known from Table 2, adding consistency is 6-16ppm, is preferably 8-12ppm, it is preferred that 8ppm.
The different adding consistency demulsification of table 2
Embodiment 8
In experiment, embodiment gained emulsion splitter is smelted the dehydrating effect producing a large amount of waste water containing waste oil class and carry out at different temperatures for certain Steel Plant, for embodiment 5 gained emulsion splitter.Adding consistency is 8ppm.
Experimental temperature is-5 DEG C ,-10 DEG C ,-20 DEG C, and Water in oil 60.4%, experimental result is as shown in table 1.
Table 3
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (9)
1. an efficient emulsion splitter, it is characterized in that, be made up of the following raw material according to weight part: poly terephthalic acid diallyl 44-51 part, polyvinyl alcohol 30-37 part, formalin 5-13 part, ethylene glycol monobutyl ether 100-108 part, polygala root extracting solution 15-22 part.
2. efficient emulsion splitter according to claim 1, it is characterized in that, be made up of the following raw material according to weight part: poly terephthalic acid diallyl 46-49 part, polyvinyl alcohol 32-35 part, formalin 7-10 part, ethylene glycol monobutyl ether 104-106 part, polygala root extracting solution 17-20 part.
3. efficient emulsion splitter according to claim 2, it is characterized in that, be made up of the following raw material according to weight part: poly terephthalic acid diallyl 48 parts, polyvinyl alcohol 33 parts, formalin 8 parts, ethylene glycol monobutyl ether 105 parts, polygala root extracting solution 18 parts.
4. a preparation method for the efficient emulsion splitter as described in as arbitrary in claim 1-3, is characterized in that, be made up of following steps:
1) preparation process of polygala root extracting solution: after polygala root is pulverized, adopt water extraction and alcohol precipitation method, obtained condensed cream, the purified water of 6 times of volumes is added in condensed cream, limit edged stirs, leave standstill 1.2-1.5h, filter, filtrate is crossed macroporous resin column wash-out with 0.7-0.8BV/h flow velocity, obtained first elutriant is for subsequent use, by the volumetric concentration of 6 times of volumes be again 20% ethanol cross macroporous resin column wash-out with 0.7-0.8BV/h flow velocity, elutriant discards, macroporous resin column wash-out is crossed again with the ethanol that the volumetric concentration of 6 times of volumes is 85%, elution flow rate is 0.7-0.8BV/h, merge with first time elutriant, reclaim and merge ethanol in elutriant and the 10-15% being concentrated into original volume, obtain polygala root extracting solution,
2) ethylene glycol monobutyl ether is heated to 90-95 DEG C, low whipping speed is under the condition of 100-125r/min, add polyvinyl alcohol, continue to stir 15-20min at such a temperature, then add poly terephthalic acid diallyl and be warming up to 120-125 DEG C, stir 30-35min at such a temperature, then be cooled to 73-78 DEG C, add polygala root extracting solution and formalin, continue to stir 2-2.5h, be cooled to 55-58 DEG C again, stir 20-30min at such a temperature; Be down to room temperature and get final product.
5. according to the arbitrary described efficient emulsion splitter of claim 1-3 in the application preparing trade effluent emulsion splitter.
6. efficient emulsion splitter according to claim 5 is in the application preparing trade effluent emulsion splitter, it is characterized in that, trade effluent is the trade effluent containing waste oil.
7. according to the arbitrary described efficient emulsion splitter of claim 5-6 in the application preparing trade effluent emulsion splitter, it is characterized in that, the adding consistency of emulsion splitter is 6-16ppm.
8. efficient emulsion splitter according to claim 7 is in the application preparing trade effluent emulsion splitter, it is characterized in that, the adding consistency of emulsion splitter is 8-12ppm.
9. efficient emulsion splitter according to claim 8 is in the application preparing trade effluent emulsion splitter, it is characterized in that, the adding consistency of emulsion splitter is 8ppm.
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CN109097094A (en) * | 2018-06-29 | 2018-12-28 | 长江大学 | A kind of preparation method of nanometer of copolymer crude oil demulsifier |
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