CN107126728A - The breaking method of waste emulsified mixture - Google Patents
The breaking method of waste emulsified mixture Download PDFInfo
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- CN107126728A CN107126728A CN201710430267.8A CN201710430267A CN107126728A CN 107126728 A CN107126728 A CN 107126728A CN 201710430267 A CN201710430267 A CN 201710430267A CN 107126728 A CN107126728 A CN 107126728A
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- Prior art keywords
- emulsified mixture
- waste emulsified
- breaking method
- demulsifier
- waste
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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
- B01D17/04—Breaking emulsions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/02—Preparation of ethers from oxiranes
- C07C41/03—Preparation of ethers from oxiranes by reaction of oxirane rings with hydroxy groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Lubricants (AREA)
Abstract
The step of being contacted the present invention relates to a kind of breaking method of waste emulsified mixture, including waste emulsified mixture with demulsifier；The demulsifier molecular structural formula is：Wherein, X is NH4+Or Na+Or K+, R is C2~C100Alkyl.
Description
Technical field
The present invention relates to a kind of breaking method of waste emulsified mixture.
Background technology
At present, environmental pollution, population expansion and inadequate resource turn into world's three major issues, therefore country's proposition is sustainable
Development strategy, i.e., while developing the economy, Saving energy and protecting environment sets up polynary energy supply system, reduces dirty
Dye discharge, realizes sustainable development, traditional economic model is progressively changed from " resource consumption-product industry-disposal of pollutants "
For " resource-product-regenerated resources ", accomplish production and consumption " disposal of pollutants minimum, changing waste into resources and harmless to environment ".
With the continuous aggravation of global energy crisis, reasonable utilize of energy resources seems even more important, and resources circulation regeneration is
The important method of energy sustainable development, recycling waste lubricating oil turns into the important channel of Resource Rationalization gradually.
During the cold rolling of stainless steel, cold rolling mill emulsion system is that cold rolling mill lubricates in the operation of rolling
With the critical system of cooling, to reduction roll-force, extension roll campaign, control all to have in terms of strip surface quality and template
Extremely important effect.With the increasingly increase of iron and steel output in recent years, the cold of lubrication and cooling effect is played in rolling process
Emulsion consumption is rolled also to increase year by year, but cold-rolling emulsion system is used for multiple times and how can handled as cold rolling waste emulsified mixture
Cold rolling waste emulsified mixture is the problem of each steel-making enterprise runs into.
The aqueous solution that cold-rolling emulsion is typically made into 3~5% when in use is used.Mainly pass through coagulation gas in current industry
The methods such as float glass process, ultrafiltration or electrocoagulation carry out waste emulsified mixture first treated.Two can be obtained after waste emulsified mixture first treated
Divide material：Most of water is separated recycling, or reaches and directly discharged after discharge standard；Another part is water content
In 30~80% water-in-oil type waste emulsified mixture concentrate, it is more itself to contain colloid state suspended impurity, mainly there is iron powder, drip
Blue or green matter oxide, additive oxide composition, content of impurities are high, and emulsification degree is serious, deals with complexity.At present for
Such waste emulsified mixture concentrate uses more method to be sour-clay-filtered：Essence is carried out to waste lubricating oil with sulfuric acid or other acid
System, acid sludge of then draining is refined to the oil after acid treatment with carclazyte, is recycled oil.But this method can form acid sludge, give up
Water and spent bleaching clay, it is big for environment pollution.
Document CN104447424A discloses a kind of sulfonic acid amine demulsifier and its synthetic method answering in cold rolling waste liquid
With.Document obtains cationic demulsifier demulsifier by two steps of etherification reaction and sulfating reaction.Demulsifier application
In Wuhan Iron and Steel Plant 1# cold rolling oil-containing waste waters and Wuhan Iron and Steel Plant 2# cold rolling oil-containing waste waters, after being demulsified by three-level, demulsification efficiency is close to 90%.But
The original state of waste emulsified mixture is not described for document, does not also indicate that the subsequent treatment of waste oil and waste water after demulsification is asked
Topic.Document CN101215578 discloses the synthesis and its application of a kind of lipopeptid biological demulsifying agent.It is characterized in that by tropical false silk ferment
Female LM bacterial strains are in using carbohydrate as the culture medium of primary raw material, in 20-35 DEG C, rotating speed 200-400r/min, air duct slats
26-48h is cultivated under part, that is, forms lipopeptid biological demulsifying agent-lipopeptid biological demulsifying agent containing lipopeptid surfactant and cultivates entirely
Liquid.By the full nutrient solution and oil-in-water emulsion with 1-2：8-10 volume ratio is mixed and mechanical agitation 5-8min, and demulsification efficiency reaches
To 95-96%.The demulsifier demulsification efficiency synthesized in document is higher, but the addition of demulsifier is larger, the waste oil waste water after demulsification
Emission problem is not also referred to.
In summary, the useless breast of water-in-oil type stainless-steel cold-rolling of above-mentioned document patent not for water content 30~80%
Change the demulsifier application of liquid.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of new waste emulsified mixture for the demulsification problem of cold rolling waste emulsified mixture
Breaking method, this method substitute acid stainless-steel cold-rolling waste emulsified mixture demulsification during use, or reduction at present with
The consumption of demulsifier, reduces the after-treatment expense of cold rolling waste liquid.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：A kind of breaking method of waste emulsified mixture, bag
Include the step of waste emulsified mixture is contacted with demulsifier；The demulsifier molecular structural formula is：
Wherein, X is NH4+Or Na+Or K+, R is C2~C100Alkyl.
In above-mentioned technical proposal, it is preferable that X is NH4+Or Na+。
In above-mentioned technical proposal, it is preferable that R is C2~C80Alkyl；It is highly preferred that R is C2~C50Alkyl；Most preferably
Ground, R is C2~C20Alkyl.
In above-mentioned technical proposal, the waste emulsified mixture is cold rolling waste emulsified mixture.Preferably, the waste emulsified mixture is water content
For 30~80 weight % water-in-oil type stainless-steel cold-rolling waste emulsified mixture.
In above-mentioned technical proposal, the consumption of the demulsifier for waste emulsified mixture weight 0.2~5.0%, preferably 0.5~
2.0%.
In above-mentioned technical proposal, Contact Temperature is 50~95 DEG C.
In above-mentioned technical proposal, time of contact is 0.5~12 hour.
Demulsifier in the present invention is prepared by following chemical reaction：
The preparation method of the demulsifier, comprises the following steps：
A) in the mixed system of BFEE and sodium hydroxide, etherificate occurs for glycerine and epoxychloropropane instead
Should, generation intermediate product I.BFEE, sodium hydroxide and C2H5OH mol ratio is 1：(1~1.2)：(0.003~
0.005).The mol ratio of glycerine and epichlorohydrin reaction is 1:(3~3.5), reaction condition is：20~30 DEG C of temperature, when
Between 7~8 hours.
B) ring-opening reaction occurs for intermediate product I and fatty alcohol, and intermediate product I epoxy bond disconnects, the hydroxyl of fatty alcohol with
Intermediate product I end is connected, the raw intermediate product II of reaction.The mol ratio of intermediate product I and long-chain fatty alcohol is 1:(3~
3.5), reaction condition is：80~85 DEG C of temperature, 12~13 hours time.Ring-opening reaction process needs catalyst, and catalyst is gold
The mol ratio of category potassium, catalyst and fatty alcohol is 1：(5~6).
C) with sulfamic acid sulfating reaction occurs for intermediate product II, and sulfamic acid occurs with the hydroxyl on intermediate product II
Addition reaction, ultimately generates purpose product, and final products are brown waxy solid.Reaction condition is：110~120 DEG C of temperature, when
Between 3~4 hours.
Demulsifier in the present invention can be by infrared analysis spectral characterization, and scanning range is 4000~500cm-1.In wave number
For 1200.5cm-1Locate as RO-SO2- O- absworption peak, is 1422.6cm in wave number-1Locate the absworption peak for C-O-C, be in wave number
2950~2890cm-1Locate the C-H absworption peaks for fatty alkyl, be 3205cm in wave number-1For N-H stretching vibration peak, 1565cm-1For N-H flexural vibrations peak.
The demulsifier that the present invention is used is because itself special structure, and the chemical bond of linker counteracts the electricity between group
Distance between lotus repulsion and hydration, the amphiphilic structure that furthered, the interfacial property of the former emulsion of destruction that can be more efficiently,
Therefore having compared with traditional demulsifier in high surface-active, the processing procedure applied to stainless-steel cold-rolling waste emulsified mixture has
More efficient demulsification ability, effectively substitutes use of the acid during demulsification, the demulsification of former method has not been only reached, obtain
The higher reclaimed oil of quality, can be used as fuel oil；The water quality of waste water and before processing emulsion after processing is more or less the same, and will not produce
Raw secondary pollution, will not bring additional contamination, achieve preferable effect.
Below by embodiment, the present invention is further elaborated.
Brief description of the drawings
Fig. 1 is the infrared analysis spectrum of demulsifier in the present invention.
Wherein, it is RO-SO at 1200.5cm-1 that wave number, which is,2- O- absworption peak, wave number is 1422.6cm-1Locate as C-O-C's
Absworption peak, wave number is 2950~2890cm-1Locate the C-H absworption peaks for fatty alkyl, wave number is 3205cm-1Flexible for N-H shakes
Dynamic peak, 1565cm-1For N-H flexural vibrations peak.
Embodiment
【Embodiment 1】
1 mole of glycerine and 3 moles of epichlorohydrin are added to the ethanol solution of BFEE and sodium hydroxide
(BFEE, sodium hydroxide and C are reacted in mixed system2H5OH mol ratio is 1：1：0.003) sticky shape, is obtained saturating
Prescribed liquid product I；1 mole of intermediate product I and 3 moles of lauryl alcohol reactions are generated into faint yellow liquid intermediate product II；By 1 mole
Intermediate product II reacts with 3 moles of sulfamic acids, obtains final product as follows：
Infrared spectrum analysis (4000~500cm of scanning range is carried out to the product of synthesis-1), with the feature shown in Fig. 1
Peak.
【Embodiment 2】
1 mole of glycerine and 3 moles of epichlorohydrin are added to the ethanol solution of BFEE and sodium hydroxide
(BFEE, sodium hydroxide and C are reacted in mixed system2H5OH mol ratio is 1：1：0.005) sticky shape, is obtained saturating
Prescribed liquid product I；1 mole of intermediate product I and 3 moles of lauryl alcohol reactions are generated into faint yellow liquid intermediate product II；By 1 mole
Intermediate product II reacts with 3 moles of sodium sulfonates, obtains final product as follows：
Infrared spectrum analysis (4000~500cm of scanning range is carried out to the product of synthesis-1), with the feature shown in Fig. 1
Peak.
【Embodiment 3】
1 mole of glycerine and 3 moles of epichlorohydrin are added to the ethanol solution of BFEE and sodium hydroxide
(BFEE, sodium hydroxide and C are reacted in mixed system2H5OH mol ratio is 1：1.2：0.003, obtain sticky shape saturating
Prescribed liquid product I；1 mole of intermediate product I and the reaction of 3 moles ethanols are generated into faint yellow liquid intermediate product II；By in 1 mole
Between product II reacted with 3 moles of sulfamic acids, obtain final product it is as follows：
Infrared spectrum analysis (4000~500cm of scanning range is carried out to the product of synthesis-1), with the feature shown in Fig. 1
Peak.
【Comparative example 1】
The cold rolling waste emulsified oil of certain factory is handled using the common lauryl sodium sulfate demulsifier of in the market.The cold rolling useless emulsification
Oily water content is 67 weight %.In 70 DEG C of settling temperature, demulsifier addition 10g/L is settled 4 hours, dehydration rate is 92%.
【Embodiment 4】
Using【Embodiment 1】The demulsifier processing of preparation【Comparative example 1】In the cold rolling waste emulsified oil of certain factory.In settling temperature
For 70 DEG C, demulsifier addition is 1g/L, and under the conditions of settling 2 hours, dehydration rate reaches 92%.
As can be seen here, using the method for the present invention, not only reduce demulsifier consumption but also shorten the sedimentation time.
【Comparative example 2】
Phosphoric acid is used to handle water content for 54 weight % cold rolling waste emulsified oil, 90 DEG C of temperature, phosphoric acid addition 1% is sunk
Drop 12 hours, dehydration rate 80%.
【Embodiment 5】
Using【Embodiment 2】The demulsifier processing of preparation【Comparative example 2】In cold rolling waste emulsified oil.It is 65 in settling temperature
DEG C, addition is 1g/L, and under the conditions of settling 12 hours, dehydration rate reaches 89%.
As can be seen here, compared with being demulsified with phosphoric acid, the use of acid is not only effectively instead of, and with higher compared with acid
Be demulsified efficiency.Upper strata oil recovery is handled through oil filter after cold rolling waste emulsified mixture demulsification has reached fuel oil products requirement, lower floor's water
Sample is as clear as crystal, pH value be 6-7 between, it is identical with the pH value of original emulsion.
【Comparative example 3】
Phosphoric acid is used to handle water content for 75 weight % cold rolling waste emulsified oil, 90 DEG C of temperature, phosphoric acid addition 1% is sunk
Drop 12 hours, dehydration rate 83%.
【Embodiment 6】
Using【Embodiment 3】The demulsifier processing of preparation【Comparative example 3】In cold rolling waste emulsified oil.It is 65 in settling temperature
DEG C, addition is 1g/L, and under the conditions of settling 12 hours, dehydration rate reaches 93%.
Claims (10)
1. a kind of breaking method of waste emulsified mixture, including waste emulsified mixture with demulsifier the step of contact；The demulsification agent molecule knot
Structure formula is：
Wherein, X is NH4+Or Na+Or K+, R is C2~C100Alkyl.
2. the breaking method of waste emulsified mixture according to claim 1, it is characterised in that X is NH4+Or Na+。
3. the breaking method of waste emulsified mixture according to claim 1, it is characterised in that R is C2~C80Alkyl.
4. the breaking method of waste emulsified mixture according to claim 3, it is characterised in that R is C2~C50Alkyl.
5. the breaking method of waste emulsified mixture according to claim 1, it is characterised in that the waste emulsified mixture is cold rolling useless emulsification
Liquid.
6. the breaking method of waste emulsified mixture according to claim 5, it is characterised in that the waste emulsified mixture is that water content is 30
~80 weight % water-in-oil type stainless-steel cold-rolling waste emulsified mixture.
7. the breaking method of waste emulsified mixture according to claim 1, it is characterised in that the consumption of the demulsifier is useless emulsification
The 0.2~5.0% of liquid weight.
8. the breaking method of waste emulsified mixture according to claim 7, it is characterised in that the consumption of the demulsifier is useless emulsification
The 0.5~2.0% of liquid weight.
9. the breaking method of waste emulsified mixture according to claim 1, it is characterised in that Contact Temperature is 50~95 DEG C.
10. the breaking method of waste emulsified mixture according to claim 1, it is characterised in that time of contact is 0.5~12 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710430267.8A CN107126728A (en) | 2017-06-09 | 2017-06-09 | The breaking method of waste emulsified mixture |
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| CN201710430267.8A CN107126728A (en) | 2017-06-09 | 2017-06-09 | The breaking method of waste emulsified mixture |
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| CN201710430267.8A Pending CN107126728A (en) | 2017-06-09 | 2017-06-09 | The breaking method of waste emulsified mixture |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421535A (en) * | 2013-09-02 | 2013-12-04 | 江苏大学 | Step-by-step etherification modified crude oil demulsifier and synthetic method thereof |
| CN104447424A (en) * | 2014-11-13 | 2015-03-25 | 武汉钢铁(集团)公司 | Ammonium sulfamate demulsifier, synthesis method thereof and application of ammonium sulfamate in cold rolling of waste emulsion |
-
2017
- 2017-06-09 CN CN201710430267.8A patent/CN107126728A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421535A (en) * | 2013-09-02 | 2013-12-04 | 江苏大学 | Step-by-step etherification modified crude oil demulsifier and synthetic method thereof |
| CN104447424A (en) * | 2014-11-13 | 2015-03-25 | 武汉钢铁(集团)公司 | Ammonium sulfamate demulsifier, synthesis method thereof and application of ammonium sulfamate in cold rolling of waste emulsion |
Non-Patent Citations (2)
| Title |
|---|
| 姚志钢: "氨基磺酸法合成AESA研究", 《邵阳高等专科学校学报》 * |
| 韩恒: "三联阴离子表面活性剂的合成及其表面化学性能", 《日用化学工业》 * |
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Application publication date: 20170905 |