CN105540738B - A kind of efficient demulsifier and its preparation method and application - Google Patents
A kind of efficient demulsifier and its preparation method and application Download PDFInfo
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- CN105540738B CN105540738B CN201510957508.5A CN201510957508A CN105540738B CN 105540738 B CN105540738 B CN 105540738B CN 201510957508 A CN201510957508 A CN 201510957508A CN 105540738 B CN105540738 B CN 105540738B
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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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Abstract
The invention discloses a kind of efficient demulsifier and its preparation method and application, the demulsifier is made up of the raw material below according to parts by weight:44 51 parts of poly terephthalic acid diallyl, 30 37 parts of polyvinyl alcohol, 5 13 parts of formalin, 100 108 parts of ethylene glycol monobutyl ether, 15 22 parts of polygala extract solution.Polygala is crushed, the elution of water extract-alcohol precipitation, macroporous resin column, concentrates and produces polygala extract solution;Ethylene glycol monobutyl ether is heated, polyvinyl alcohol is added, cools after adding poly terephthalic acid diallyl and heating treatment, polygala extract solution is added and is handled with formalin, then the processing that cools;Room temperature is down to produce.The present invention is easy to get with raw material, cost is cheap, demulsification is good, preparation method is simple, simple operation, gained demulsifier has the advantages that few dosage, high temperature resistant, low temperature resistant, dehydrating amount is big and dewatering speed is fast, suitable for industrial wastewater field, especially suitable for that can produce the steel industry of the waste water containing waste oil class, coking industry, oilfield exploitation, machining manufacturing industry etc..
Description
Technical field
The present invention relates to demulsifier field, specifically a kind of efficient demulsifier and its preparation method and application.
Background technology
Industrial wastewater refers to caused waste water, sewage and waste liquid in industrial processes, wherein containing the work outflowed with water
Caused pollutant in industry production materials, intermediate product and product and production process.As industrial develops rapidly, waste water
Type and quantity rapidly increase, and the pollution to water body is also increasingly extensively and serious, threaten the health and safety of the mankind.Therefore, it is right
For environmental protection, the processing of industrial wastewater is more even more important than the processing of municipal sewage.Polluted caused by industrial wastewater main
Have:Organic aerobic Substances Pollution, chemical toxicant pollution, inoganic solids suspended solid pollutant, heavy metal pollution, acid pollution, alkali pollution,
Pollution of plant nutritions, thermal pollution, pathogen contamination etc..Many pollutants have color, stink or easily raw foam, therefore industry
Unpleasant outward appearance is often presented in waste water, causes water body pollution in wide area, directly threatens the life and health of the people, therefore
Control industrial wastewater particularly important.Particularly steel industry, coking industry etc. can produce the material largely containing waste oil class, should
Kind oil product oil is poor, water content is high, complicated component, containing sludge, the lubrication impurity such as lipid and moisture, most of smelters processing
Mode is filled after transporting outward, and does not simply fail to directly utilize, and environmental pollution is very big.This processing mode is simply extensive, nothing
Economic benefit.
The content of the invention
It is an object of the invention to provide a kind of dosage is few, high temperature resistant, low temperature resistant, dehydrating amount is big, dewatering speed is fast, efficiently
Demulsifier and its preparation method and application, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical scheme:
A kind of efficient demulsifier, is made up of the raw material below according to parts by weight:Poly terephthalic acid diallyl 44-51
Part, polyvinyl alcohol 30-37 parts, formalin 5-13 parts, ethylene glycol monobutyl ether 100-108 parts, polygala extract solution 15-22 parts.
As the further scheme of the present invention:The efficient demulsifier, is made up of the raw material below according to parts by weight:It is poly-
Diallyl p phthalate 46-49 parts, polyvinyl alcohol 32-35 parts, formalin 7-10 parts, ethylene glycol monobutyl ether 104-106
Part, polygala extract solution 17-20 parts.
As the further scheme of the present invention:The efficient demulsifier, is made up of the raw material below according to parts by weight:It is poly-
48 parts of diallyl p phthalate, 33 parts of polyvinyl alcohol, 8 parts of formalin, 105 parts of ethylene glycol monobutyl ether, polygala extract solution
18 parts.
The preparation method of the efficient demulsifier, is comprised the steps of:
1) preparation process of polygala extract solution:After polygala is crushed, using water extraction and alcohol precipitation method, condensed cream is made, to concentration
The purified water of 6 times of volumes is added in cream, it is stirring while adding, 1.2-1.5h is stood, filtering, filtrate is flowed with 0.7-0.8BV/h
Speed cross macroporous resin column elution, be made the first eluent it is standby, then by the volumetric concentration of 6 times of volumes be 20% ethanol with
0.7-0.8BV/h flow velocitys cross macroporous resin column elution, and eluent discards, then the second for being 85% with the volumetric concentration of 6 times of volumes
Alcohol crosses macroporous resin column elution, elution flow rate 0.7-0.8BV/h, merges with first time eluent, and recovery merges in eluent
Ethanol and the 10-15% for being concentrated into original volume, produce polygala extract solution;
2) ethylene glycol monobutyl ether is heated to 90-95 DEG C, under conditions of low whipping speed is 100-125r/min, added poly-
Vinyl alcohol, continuation stir 15-20min, add poly terephthalic acid diallyl and be warming up to 120-125 at such a temperature
DEG C, 30-35min is stirred at such a temperature, is then cooled to 73-78 DEG C, is added polygala extract solution and formalin, is continued to stir
2-2.5h, then 55-58 DEG C is cooled to, 20-30min is stirred at such a temperature;Room temperature is down to produce.
The efficient demulsifier is preparing the application of industrial wastewater demulsifier.
As the further scheme of the present invention:Industrial wastewater is the industrial wastewater containing waste oil.
As the further scheme of the present invention:The adding consistency of demulsifier is 6-16ppm.
As the further scheme of the present invention:The adding consistency of demulsifier is 8-12ppm.
As the further scheme of the present invention:The adding consistency of demulsifier is 8ppm.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention is easy to get with raw material, and cost is cheap, and demulsification is good, and preparation method is simple, simple operation, gained demulsification
Agent has the advantages that few dosage, high temperature resistant, low temperature resistant, dehydrating amount is big and dewatering speed is fast, suitable for industrial wastewater field, especially
Suitable for the steel industry of the waste water that can produce the waste water largely containing waste oil class, coking industry, oilfield exploitation, machining
Manufacturing industry etc..
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of efficient demulsifier, it is made up of the raw material below according to parts by weight:Poly- terephthaldehyde
44 parts of diallyl phthalate, 30 parts of polyvinyl alcohol, 5 parts of formalin, 100 parts of ethylene glycol monobutyl ether, 15 parts of polygala extract solution.
The preparation process of polygala extract solution:After polygala is crushed, using water extraction and alcohol precipitation method, condensed cream is made, to condensed cream
The middle purified water for adding 6 times of volumes, it is stirring while adding, 1.2h is stood, filtering, filtrate is crossed into macropore tree with 0.7BV/h flow velocitys
Fat post elute, be made the first eluent it is standby, then by the volumetric concentration of 6 times of volumes be 20% ethanol with 0.7BV/h flow velocitys
Macroporous resin column elution is crossed, eluent discards, then the ethanol for being 85% with the volumetric concentration of 6 times of volumes is crossed macroporous resin column and washed
It is de-, elution flow rate 0.7BV/h, merge with first time eluent, recovery merges ethanol in eluent and is concentrated into original volume
10%, produce polygala extract solution.Ethylene glycol monobutyl ether is heated to 90 DEG C, under conditions of low whipping speed is 100r/min, added
Entering polyvinyl alcohol, 15min is stirred in continuation at such a temperature, is added poly terephthalic acid diallyl and is warming up to 120 DEG C,
30min is stirred at this temperature, is then cooled to 73 DEG C, adds polygala extract solution and formalin, continues to stir 2h, then be cooled to
55 DEG C, 20min is stirred at such a temperature;Room temperature is down to produce.
Embodiment 2
In the embodiment of the present invention, a kind of efficient demulsifier, it is made up of the raw material below according to parts by weight:Poly- terephthaldehyde
51 parts of diallyl phthalate, 37 parts of polyvinyl alcohol, 13 parts of formalin, 108 parts of ethylene glycol monobutyl ether, 22 parts of polygala extract solution.
The preparation process of polygala extract solution:After polygala is crushed, using water extraction and alcohol precipitation method, condensed cream is made, to condensed cream
The middle purified water for adding 6 times of volumes, it is stirring while adding, 1.5h is stood, filtering, filtrate is crossed into macropore tree with 0.8BV/h flow velocitys
Fat post elute, be made the first eluent it is standby, then by the volumetric concentration of 6 times of volumes be 20% ethanol with 0.8BV/h flow velocitys
Macroporous resin column elution is crossed, eluent discards, then the ethanol for being 85% with the volumetric concentration of 6 times of volumes is crossed macroporous resin column and washed
It is de-, elution flow rate 0.8BV/h, merge with first time eluent, recovery merges ethanol in eluent and is concentrated into original volume
15%, produce polygala extract solution.Ethylene glycol monobutyl ether is heated to 95 DEG C, under conditions of low whipping speed is 125r/min, added
Entering polyvinyl alcohol, 20min is stirred in continuation at such a temperature, is added poly terephthalic acid diallyl and is warming up to 125 DEG C,
35min is stirred at this temperature, is then cooled to 78 DEG C, adds polygala extract solution and formalin, continues to stir 2.5h, then cool
To 58 DEG C, 30min is stirred at such a temperature;Room temperature is down to produce.
Embodiment 3
In the embodiment of the present invention, a kind of efficient demulsifier, it is made up of the raw material below according to parts by weight:Poly- terephthaldehyde
46 parts of diallyl phthalate, 32 parts of polyvinyl alcohol, 7 parts of formalin, 104 parts of ethylene glycol monobutyl ether, 17 parts of polygala extract solution.
The preparation process of polygala extract solution:After polygala is crushed, using water extraction and alcohol precipitation method, condensed cream is made, to condensed cream
The middle purified water for adding 6 times of volumes, it is stirring while adding, 1.4h is stood, filtering, filtrate is crossed into macropore tree with 0.7BV/h flow velocitys
Fat post elute, be made the first eluent it is standby, then by the volumetric concentration of 6 times of volumes be 20% ethanol with 0.7BV/h flow velocitys
Macroporous resin column elution is crossed, eluent discards, then the ethanol for being 85% with the volumetric concentration of 6 times of volumes is crossed macroporous resin column and washed
It is de-, elution flow rate 0.7BV/h, merge with first time eluent, recovery merges ethanol in eluent and is concentrated into original volume
12%, produce polygala extract solution.Ethylene glycol monobutyl ether is heated to 92 DEG C, under conditions of low whipping speed is 110r/min, added
Entering polyvinyl alcohol, 17min is stirred in continuation at such a temperature, is added poly terephthalic acid diallyl and is warming up to 122 DEG C,
32min is stirred at this temperature, is then cooled to 75 DEG C, adds polygala extract solution and formalin, continues to stir 2.2h, then cool
To 57 DEG C, 25min is stirred at such a temperature;Room temperature is down to produce.
Embodiment 4
In the embodiment of the present invention, a kind of efficient demulsifier, it is made up of the raw material below according to parts by weight:Poly- terephthaldehyde
49 parts of diallyl phthalate, 35 parts of polyvinyl alcohol, 10 parts of formalin, 106 parts of ethylene glycol monobutyl ether, 20 parts of polygala extract solution.
Preparation process is consistent with embodiment 3.
Embodiment 5
In the embodiment of the present invention, a kind of efficient demulsifier, it is made up of the raw material below according to parts by weight:Poly- terephthaldehyde
48 parts of diallyl phthalate, 33 parts of polyvinyl alcohol, 8 parts of formalin, 105 parts of ethylene glycol monobutyl ether, 18 parts of polygala extract solution.
Preparation process is consistent with embodiment 3.
Embodiment 6
Demulsifier made from 1-5 of the embodiment of the present invention is smelted for certain steel plant in experiment and produced largely containing useless
The dehydrating effect that the waste water of oils is carried out.
Experimental temperature is 70 DEG C, and Water in oil 60.4%, experimental result is as shown in table 1.Meanwhile it is also provided with 3 groups of contrasts
, in comparative example 1 in addition to polygala extract solution is not contained, remaining proportioning is consistent with embodiment 5 with preparation process, in comparative example 2 only
Containing polygala extract solution, its preparation process is consistent with embodiment 5, and comparative example 3 is not in addition to formalin is contained, remaining proportioning and system
Standby process is consistent with embodiment 5.
The demulsification of 1 different demulsifiers of table
From table 1 it follows that 1-5 treatment effects of the embodiment of the present invention are better than comparative example 1-3, illustrate the present invention be
Worked under each component collective effect.
Embodiment 7
In experiment, demulsifier obtained by the embodiment of different adding consistencies is smelted into generation for certain steel plant and largely contained
The dehydrating effect that the waste water for having waste oil class is carried out.By taking the gained demulsifier of embodiment 5 as an example.
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, preferably 8-12ppm, most preferably 8ppm.
The different adding consistency demulsifications of table 2
Embodiment 8
In experiment, demulsifier obtained by embodiment is smelted into the waste water produced largely containing waste oil class for certain steel plant
The dehydrating effect carried out at different temperatures, by taking the gained demulsifier of embodiment 5 as an example.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
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (8)
1. a kind of efficient demulsifier, it is characterised in that be made up of the raw material below according to parts by weight:Poly terephthalic acid diene
Propyl ester 44-51 parts, polyvinyl alcohol 30-37 parts, formalin 5-13 parts, ethylene glycol monobutyl ether 100-108 parts, polygala extract solution
15-22 parts;
Its preparation method, is comprised the steps of:
1) preparation process of polygala extract solution:After polygala is crushed, using water extraction and alcohol precipitation method, condensed cream is made, into condensed cream
The purified water of 6 times of volumes is added, it is stirring while adding, stand 1.2-1.5h, filtering, by filtrate with 0.7-0.8BV/h flow velocity mistakes
Macroporous resin column elute, be made the first eluent it is standby, then by the volumetric concentration of 6 times of volumes be 20% ethanol with 0.7-
0.8BV/h flow velocitys cross macroporous resin column elution, and eluent discards, then the ethanol mistake for being 85% with the volumetric concentration of 6 times of volumes
Macroporous resin column elutes, and elution flow rate 0.7-0.8BV/h, merges with first time eluent, and recovery merges ethanol in eluent
And the 10-15% of original volume is concentrated into, produce polygala extract solution;
2) ethylene glycol monobutyl ether is heated to 90-95 DEG C, under conditions of low whipping speed is 100-125r/min, adds polyethylene
15-20min is stirred in alcohol, continuation at such a temperature, is added poly terephthalic acid diallyl and is warming up to 120-125 DEG C,
30-35min is stirred at this temperature, is then cooled to 73-78 DEG C, adds polygala extract solution and formalin, continues to stir 2-
2.5h, then 55-58 DEG C is cooled to, 20-30min is stirred at such a temperature;Room temperature is down to produce.
2. efficient demulsifier according to claim 1, it is characterised in that be made up of the raw material below according to parts by weight:
Poly terephthalic acid diallyl 46-49 parts, polyvinyl alcohol 32-35 parts, formalin 7-10 parts, ethylene glycol monobutyl ether 104-
106 parts, polygala extract solution 17-20 parts.
3. efficient demulsifier according to claim 2, it is characterised in that be made up of the raw material below according to parts by weight:
48 parts of poly terephthalic acid diallyl, 33 parts of polyvinyl alcohol, 8 parts of formalin, 105 parts of ethylene glycol monobutyl ether, polygala extraction
18 parts of liquid.
4. the application of industrial wastewater demulsifier is being prepared according to any described efficient demulsifiers of claim 1-3.
5. efficient demulsifier according to claim 4 is preparing the application of industrial wastewater demulsifier, it is characterised in that work
Industry waste water is the industrial wastewater containing waste oil.
6. the application of industrial wastewater demulsifier is being prepared according to any described efficient demulsifiers of claim 4-5, its feature
It is, the adding consistency of demulsifier is 6-16ppm.
7. efficient demulsifier according to claim 6 is preparing the application of industrial wastewater demulsifier, it is characterised in that broken
The adding consistency of emulsion is 8-12ppm.
8. efficient demulsifier according to claim 7 is preparing the application of industrial wastewater demulsifier, it is characterised in that broken
The adding consistency of emulsion is 8ppm.
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CN103803764A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Oily sludge demulsifier and preparation method thereof |
CN103951009A (en) * | 2014-02-17 | 2014-07-30 | 宜兴汉光高新石化有限公司 | Coking demulsifier and preparation method thereof |
CN104556297A (en) * | 2015-01-28 | 2015-04-29 | 桑达化工(南通)有限公司 | High-efficiency demulsifier |
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2015
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CN101112662A (en) * | 2007-06-28 | 2008-01-30 | 北京海恩润德化工科学技术有限公司 | Mixed demulsification agent of produced liquid during ASP flooding |
CN101555056A (en) * | 2009-05-05 | 2009-10-14 | 中国石油兰州石油化工公司 | High-efficiency emulsion splitter |
EP2377910A1 (en) * | 2010-04-14 | 2011-10-19 | General Electric Company | Compositions and method for breaking water in oil emulsions |
CN102765767A (en) * | 2012-07-12 | 2012-11-07 | 天津市瑞德赛恩新材料开发有限公司 | Delay coking coke cooling water demulsifier composition and preparation method and application thereof |
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