CN103665394B - A kind of Cyclohexanone Waste Water that utilizes is to prepare the method for Emulsion Resid - Google Patents

A kind of Cyclohexanone Waste Water that utilizes is to prepare the method for Emulsion Resid Download PDF

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CN103665394B
CN103665394B CN201210359054.8A CN201210359054A CN103665394B CN 103665394 B CN103665394 B CN 103665394B CN 201210359054 A CN201210359054 A CN 201210359054A CN 103665394 B CN103665394 B CN 103665394B
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waste water
residual oil
cyclohexanone
aqueous solution
emulsion resid
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CN103665394A (en
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李正琪
李昕阳
卢姝
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Abstract

A kind of Cyclohexanone Waste Water that utilizes is to prepare the method for Emulsion Resid, relate to the preparation method field of petroleum emulsification liquid, be specifically related to a kind of method preparing Emulsion Resid utilizing Cyclohexanone Waste Water, comprise the following steps: in Cyclohexanone Waste Water, add emulsifying agent and stablizer, the aqueous solution stirring and dissolving obtained is incubated; Residual oil is heated to fusing; The described aqueous solution is evenly joined in the residual oil of described fusing, stir and obtain Emulsion Resid.The advantage of the inventive method is to utilize waste water as the former water preparing Emulsion Resid, has both saved the use of clear water, simultaneously using waste water as raw material, play the effect of turning waste into wealth.

Description

A kind of Cyclohexanone Waste Water that utilizes is to prepare the method for Emulsion Resid
Technical field:
The present invention relates to the preparation method field of petroleum emulsification liquid, be specifically related to a kind of method preparing Emulsion Resid utilizing Cyclohexanone Waste Water.
Background technology:
Chemical industry is the conventional column industry of China, and industrial chemicals and the product of production are widely used in every field.Chemical industry is again the industry of high pollution, and the organic pollutant of the waste water produced usually containing high density, be difficult to by common method of wastewater treatment as biochemical treatment, film process etc. reaches qualified discharge.
The waste water that pimelinketone device produces is the organic pollutant of difficult degradation mostly, and it is large that this waste water has the water yield, and the features such as organic pollutant colourity is dark, complicated component, degradability difference, belong to unmanageable trade effluent.For the trade effluent that this device of certain chemical company produces, the pH of waste water is about 11, COD crbe 1000 ~ 20000mg/L, colourity is up to more than 2000 times, and the organism contained in waste water is difficult to degraded.
Petrochemical industry generally can obtain the residual oil of about 40% in the process of processing crude oil, and the overwhelming majority is used as fuel to use.But because residual oil viscosity is large, asphalt content is high, causes incomplete combustion, and the by product that burning generates also pollutes the environment.Residual oil is made Emulsion Resid and can effectively improve oil gasification rate, make it burn completely.Patent " emulsification method of vacuum residuum " (application number 98125094.7) describes a kind of emulsification method of residual oil, by vacuum residuum, water and the emulsifying agent containing sulfonated petro-leum formaldehyde condensation products are mixed and made into Emulsion Resid, the method cost is low, and stability also meets service requirements.Above-mentioned patent utilizes clear water to prepare Emulsion Resid, but utilize wastewater from chemical industry also not meet report to prepare Emulsion Resid.
" a kind of preparation research of residual oil emulsified fuel oil " (Li Shanjian, Li Qianding, Li Tiansheng, Chemical Engineering Technology and exploitation, 2008,37,18-21) report a kind of preparation method of Emulsion Resid, this research is mainly optimized the formula of emulsifying agent and technique, and water used is ortho-water.
Summary of the invention:
For the shortcoming that prior art exists, the object of the present invention is to provide a kind of Cyclohexanone Waste Water that utilizes to prepare the method for Emulsion Resid, discharge the environment produced pollution to avoid Cyclohexanone Waste Water.
For realizing above target, the technical scheme that the present invention takes, is characterized in that comprising the steps:
1) in Cyclohexanone Waste Water, add emulsifying agent and stablizer, by the aqueous solution stirring and dissolving obtained, and be heated to 70 ~ 80 oc is incubated, described Cyclohexanone Waste Water, emulsifying agent, and the mass ratio of stablizer is 10 ~ 30:0.1 ~ 5:0.003 ~ 0.05;
2) taking with the mass ratio of above-mentioned Cyclohexanone Waste Water is the residual oil of 70 ~ 90, is heated to 120 ~ 150 oc, makes residual oil melt, and is incubated under being then placed in the temperature identical with the holding temperature of the described aqueous solution;
3) under described holding temperature and high-speed stirring condition, the described aqueous solution is evenly joined in the residual oil of described fusing, stir 5 ~ 15min and can obtain Emulsion Resid.
Wherein, the pH of described Cyclohexanone Waste Water is 9 ~ 13, COD is 1000 ~ 20000mg/L, and main organic composition is pimelinketone, organic acid.
On the basis of technique scheme, emulsifying agent is the mixture of alkylphenol polyoxyethylene (OP-10) or alkylphenol polyoxyethylene (OP-10) and one or more emulsifying agents following: sodium lauryl sulphate, sodium polystyrene sulfonate, tween 80;
On the basis of technique scheme, stablizer is one or more mixture of polyacrylamide (1630s) or Walocel MT 20.000PV, polyvinyl alcohol and water glass.
The advantage of the inventive method is to utilize waste water as the former water preparing Emulsion Resid, has both saved the use of clear water, simultaneously using waste water as raw material, play the effect of turning waste into wealth.
The present invention efficiently solves the discharge of this type of wastewater from chemical industry and administers a difficult problem, decreases the pollution of organic waste water to environment, has obvious economic and social benefit.
Accompanying drawing illustrates:
Fig. 1 is the schema utilizing Cyclohexanone Waste Water to prepare Emulsion Resid.
Specific implementation method:
Containing a large amount of organism in Cyclohexanone Waste Water, its feature is as shown in the table:
Wastewater source Cyclohexanone Waste Water
pH 9~13
COD(mg/L) 1000~20000
Main organic composition Pimelinketone, organic acid
Compared with patent " emulsification method of vacuum residuum " (application number 98125094.7), the present invention utilizes Cyclohexanone Waste Water as aqueous phase, emulsifying agent alkylphenol polyoxyethylene (OP-10) and stablizer polyacrylamide (1630s) is adopted to prepare Emulsion Resid, and preparation condition is optimized, accomplish utilization of waste material.
For Cyclohexanone Waste Water, it can be used as raw material to prepare Emulsion Resid.Described Emulsion Resid, its raw material in mass, is filled a prescription as follows:
1. the Cyclohexanone Waste Water 10 ~ 30 parts containing following 2nd, 3 class components;
2. alkylphenol polyoxyethylene (OP-10) 0.1 ~ 5 part;
3. polyacrylamide (1630s) 0.003 ~ 0.05 part;
4. 70 ~ 90 parts, residual oil
According to formula feature, emulsifying agent, except for except alkylphenol polyoxyethylene (OP-10), can also be the mixture of alkylphenol polyoxyethylene (OP-10) and one or more emulsifying agents following: as sodium lauryl sulphate, sodium polystyrene sulfonate, tween 80;
Stablizer except for except polyacrylamide (1630s), can also be following one or more: Walocel MT 20.000PV, polyvinyl alcohol, water glass.
The concrete technical scheme of the method for the invention is:
Step 1: take the Cyclohexanone Waste Water 10 ~ 30 parts (mass ratio) that pH is 9 ~ 13, add the emulsifying agent alkylphenol polyoxyethylene (OP-10) of 0.1 ~ 5 part, the aqueous solution that the stablizer polyacrylamide (1630s) of 0.003 ~ 0.05 part obtains emulsifying agent, stirring and dissolving, and be heated to 70 ~ 80 oc is incubated;
Step 2: take 70 ~ 90 parts, residual oil, be heated to 120 ~ 150 oc makes it melt, then with above-mentioned solution uniform temp under be incubated;
Step 3: under said temperature and high-speed stirring condition, evenly joined in residual oil by the aqueous solution of emulsifying agent, stirs 5 ~ 15min and can obtain Emulsion Resid.
On the basis of technique scheme, emulsifying agent, except for except alkylphenol polyoxyethylene (OP-10), can also be the mixture of alkylphenol polyoxyethylene (OP-10) and one or more emulsifying agents following: as sodium lauryl sulphate, sodium polystyrene sulfonate, tween 80;
On the basis of technique scheme, stablizer except for except polyacrylamide (1630s), can also be following one or more: Walocel MT 20.000PV, polyvinyl alcohol, water glass.
The preferred embodiments of the present invention are as follows:
Embodiment 1: (pH is 9 to get Cyclohexanone Waste Water, COD is 5000 mg/L) 20g is in there-necked flask, the polyacrylamide (1630s) of the alkylphenol polyoxyethylene (OP-10) and 0.005g that add 0.3g obtains the aqueous solution of emulsifying agent, and stirring and dissolving, is heated to 80 oc is incubated.Take residual oil 80g, be heated to 120 oc makes it melt, then 80 obe incubated under C.Under high-speed stirring condition, the aqueous solution of emulsifying agent is evenly joined in residual oil, stir 15min and can obtain Emulsion Resid.Obtained Emulsion Resid viscosity is 600mPaS, and under normal temperature, Absorbable organic halogens deposits more than 3 days.Preparation flow is see Fig. 1.
Embodiment 2: (pH is 10 to get Cyclohexanone Waste Water, COD is 8000 mg/L) 30g is in there-necked flask, the Walocel MT 20.000PV adding the alkylphenol polyoxyethylene (OP-10) of 0.1g, 0.2g sodium lauryl sulphate and 0.05g obtains the aqueous solution of emulsifying agent, and stirring and dissolving, is heated to 75 oc is incubated.Take residual oil 70g, be heated to 120 oc makes it melt, then 75 obe incubated under C.Under high-speed stirring condition, the aqueous solution of emulsifying agent is evenly joined in residual oil, stir 5min and can obtain Emulsion Resid.Obtained Emulsion Resid viscosity is 800mPaS, and under normal temperature, Absorbable organic halogens deposits more than 3 days.
Embodiment 3: get Cyclohexanone Waste Water (pH is 11, COD is 20000 mg/L) 10g in there-necked flask, the poly-polyvinyl alcohol of the alkylphenol polyoxyethylene (OP-10) and 0.05g that add 5g obtains the aqueous solution of emulsifying agent, and stirring and dissolving, is heated to 70 oc is incubated.Take residual oil 90g, be heated to 130 oc makes it melt, then 70 obe incubated under C.Under high-speed stirring condition, the aqueous solution of emulsifying agent is evenly joined in residual oil, stir 10min and can obtain Emulsion Resid.Obtained Emulsion Resid viscosity is 700mPaS, and under normal temperature, Absorbable organic halogens deposits more than 3 days.
Embodiment 4: (pH is 12 to get Cyclohexanone Waste Water, COD is 10000 mg/L) 15g is in there-necked flask, add the alkylphenol polyoxyethylene (OP-10) of 0.8g, 0.6g sodium polystyrene sulfonate, 0.2g tween 80 and the water glass of 0.003g, the aqueous solution that the polyvinyl alcohol of 0.01g obtains emulsifying agent, stirring and dissolving, is heated to 70 oc is incubated.Take residual oil 85g, be heated to 150 oc makes it melt, then 70 obe incubated under C.Under high-speed stirring condition, the aqueous solution of emulsifying agent is evenly joined in residual oil, stir 15min and can obtain Emulsion Resid.Obtained Emulsion Resid viscosity is 500mPaS, and under normal temperature, Absorbable organic halogens deposits more than 3 days.
Embodiment 5: (pH is 13 to get Cyclohexanone Waste Water, COD is 1000 mg/L) 12g is in there-necked flask, add the polyacrylamide (1630s) of the alkylphenol polyoxyethylene (OP-10) of 2g, 1g sodium polystyrene sulfonate and 0.004g, the polyvinyl alcohol of 0.02g obtains the aqueous solution of emulsifying agent, stirring and dissolving, is heated to 70 oc is incubated.Take residual oil 85g, be heated to 150 oc makes it melt, then 70 obe incubated under C.Under high-speed stirring condition, the aqueous solution of emulsifying agent is evenly joined in residual oil, stir 15min and can obtain Emulsion Resid.Obtained Emulsion Resid viscosity is 550mPaS, and under normal temperature, Absorbable organic halogens deposits more than 3 days.

Claims (2)

1. utilize Cyclohexanone Waste Water to prepare a method for Emulsion Resid, said method comprising the steps of:
1) in Cyclohexanone Waste Water, add emulsifying agent and stablizer, by the aqueous solution stirring and dissolving obtained, and be heated to 70 ~ 80 DEG C of insulations, described Cyclohexanone Waste Water, emulsifying agent, the mass ratio of stablizer three is 10 ~ 30:0.1 ~ 5:0.003 ~ 0.05;
Described emulsifying agent is one or more the mixture in alkylphenol polyoxyethylene or alkylphenol polyoxyethylene and sodium lauryl sulphate, sodium polystyrene sulfonate and tween 80;
Described stablizer is one or more the mixture in polyacrylamide or Walocel MT 20.000PV, polyvinyl alcohol and water glass;
2) taking with the mass ratio of above-mentioned Cyclohexanone Waste Water is the residual oil of 70 ~ 90, is heated to 120 ~ 150 DEG C, and residual oil is melted, and is incubated under being then placed in the temperature identical with the holding temperature of the described aqueous solution;
3) under described holding temperature and high-speed stirring condition, the described aqueous solution is evenly joined in the residual oil of described fusing, stir 5 ~ 15min and can obtain Emulsion Resid.
2. utilize Cyclohexanone Waste Water to prepare the method for Emulsion Resid as claimed in claim 1, it is characterized in that, the pH of described Cyclohexanone Waste Water is 9 ~ 13, COD is 1000 ~ 20000mg/L.
CN201210359054.8A 2012-09-24 2012-09-24 A kind of Cyclohexanone Waste Water that utilizes is to prepare the method for Emulsion Resid Active CN103665394B (en)

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CN105085936B (en) * 2014-04-25 2018-11-02 中国石油化工股份有限公司 A method of preparing Emulsion Resid using PVA device waste water
CN105967261A (en) * 2016-05-26 2016-09-28 许婷 Sewage treatment agent special for printing and dyeing wastewater and preparation method of sewage treatment agent

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101240186A (en) * 2007-02-06 2008-08-13 肇庆西江发电厂有限公司 Residual oil viscosity-reducing emulsification and technique for applying the same in large-scale diesel generator
CN101724276A (en) * 2008-10-29 2010-06-09 中国石油化工股份有限公司 Lignin modified asphalt composition with steady heat storage and preparation method thereof
CN101949282A (en) * 2010-07-22 2011-01-19 中国石油天然气股份有限公司 Oil displacement method for residual oil asphalt emulsion

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101240186A (en) * 2007-02-06 2008-08-13 肇庆西江发电厂有限公司 Residual oil viscosity-reducing emulsification and technique for applying the same in large-scale diesel generator
CN101724276A (en) * 2008-10-29 2010-06-09 中国石油化工股份有限公司 Lignin modified asphalt composition with steady heat storage and preparation method thereof
CN101949282A (en) * 2010-07-22 2011-01-19 中国石油天然气股份有限公司 Oil displacement method for residual oil asphalt emulsion

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