CN106833587A - A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease - Google Patents
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease Download PDFInfo
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- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
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Abstract
The present invention relates to a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, it is raw material using kitchen waste grease, bio oil hydroxy sulfonate is obtained by processing the series reaction such as purification, sulfonating reaction, hydrolysis neutralization, point liquid and vacuum distillation, the kitchen waste grease that the present invention is used, it is the mixture of various triglycerides after processing purification, the oil resource enriches, low production cost；Described bio oil hydroxy sulfonate is a kind of surfactant, is applied to field of petroleum exploitation.The bio oil hydroxyl sulfoacid salt surfactant of present invention synthesis has preferable surface-active, interfacial activity, and biological degradability is good, environmental toxicity is small, alternative traditional petroleum sulfonate surfactant.
Description
Technical field
The invention belongs to organic compound synthesis field, in particular it relates to a kind of there is preferable surface-active, interface to live
Property, the bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease that biological degradability is good, environmental toxicity is small, and apply
In oil exploitation.
Background technology
Kitchen waste grease refers to that the mankind produce in edible natural vegetable oil and animal tallow, and grease deep-processing process
A series of raw fatty wastes for losing edibility, are commonly called as waste oil, hogwash fat, swill oil etc..It was found that waste grease
Amount account for the 20~30% of edible oil total quantity consumed.A large amount of accumulations of kitchen waste grease are gone back except triggering food security accident
Huge risk of environmental pollution can be brought.It is in particular in several aspects：1) food-safety problem is caused.Due to kitchen abandoned oil
The easy oxidative rancidity of fat goes bad, and produces aflatoxins with strong carcinogenesis etc., once dealing with improperly, reenters food
Chain, it will have a strong impact on human health, in some instances it may even be possible to cause great food security accident.2) polluted-water.Kitchen waste grease
It is one of important trophism water pollutant, water quality deterioration and eutrophication can be caused into water body, and make sewage treatment plant
Biological processing unit treatment effeciency is significantly reduced.3) emitting offensive odor.Exposure time is long in atmosphere for kitchen waste grease, and oxygen occurs
Change is become sour, and distributes volatile fat acids foul gas, has a strong impact on environment, be trigger public's kickback main cause it
One.
With the fast development of China's economy, China is in rising trend always to the demand of oil and oil product, stone
The demand of oil and exploitation contradiction.How to effectively improve oil recovery factor, find Development of Novel oil recovery technique into
It is the key subjects of China Petroleum, wherein surfactant flooding has become one of key means of this kind of new technology.
The main large-medium-sized oilfield of China is already in the latter stage in waterflooding development stage, enters the new technology that tertiary oil recovery is representative
Phase of development, surfactant flooding agent is widely used in each elephant.At present, domestic surface used for tertiary oil recovery is lived
Property agent mainly has petroleum carboxylate, petroleum sulfonate, heavy alkylbenzene sulfonate etc..The raw material for synthesizing these surfactants is available for
The scope of selection is not extensive enough, mainly refining oil byproduct petroleum distillate (mainly heavy aromatics, aromatic hydrocarbons), heavy alkyl benzene and SO3
Based on produce, produced using autoclave or falling film sulfonation units, the technique such as auxiliary neutralization, compounding obtains can be used for the displacement of reservoir oil
Alkylaryl sulfonates.Due to oil product as raw material, these sulfosalt surfactants are substantially all containing aromatic ring, especially
It is that aromatic ring structure is also contained in part, biological decomposition ability, environmental improvement difficulty are big, have pollution to environment.And pass through in recent years
Often there is the nervous situation of raw material supply, cause cost of material to go up year by year, need the available sources for expanding raw material badly.
Using the active ingredient in kitchen waste grease as the raw material of tertiary oil recovery surfactant, meal can be effectively solved
Kitchen waste grease is directly discharged into sewer or is filled or burned by Domestic Waste Collection processing system and causes resource
Waste and problem of environmental pollution.Kitchen waste grease recycling is promoted, is turned waste into wealth, turned harm into good, be not only development and follow
The important content of ring economy, is also the fundamental measure for solving the food-safety problem that kitchen waste grease triggers.Or stone
Bulk petroleum resource is saved in the production of oil exploitation surfactant.
The content of the invention
It is an object of the invention to provide a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, profit
The bio oil hydroxyl sulfoacid salt surfactant prepared with the method has preferable surface-active, interfacial activity, biodegradable
The good, environmental toxicity of property is small, alternative traditional petroleum sulfonate surfactant.
To achieve these goals, the present invention uses following technical scheme：
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, comprises the following steps：
A, the processed purification of kitchen waste grease, obtain treatment grease, and the treatment grease is the mixing of several triglycerides
Thing；
B, kitchen waste grease and the solvent that will process purification are mixed in and are burnt equipped with magnetic rotor, condenser pipe, three mouthfuls of thermometer
In bottle, there-necked flask is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, quickly stirs 10-20min, makes kitchen waste grease complete
CL, obtains the mixed solution of light brown；
C, at room temperature toward oleum is slowly dropped into the mixed solution of there-necked flask, while quickly being stirred, timing is opened
After beginning to instill oleum 10-15min, heat up and be incubated；
D, reach the reaction time after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until reaction solution is in acidity
When, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 2-5min is sufficiently mixed, product is poured into separatory funnel, use distilled water diluting
Solution, vibrates and stirs, and stands 10-15min, the crude product of isolated bio oil hydroxy sulfonate, by the crude product
In the thermostat water bath using after simulating vacuum distillation apparatus vacuum distillation 1.5-2h, obtain bio oil hydroxy sulfonate into
Product.
Preferably, the kitchen waste grease is selected from any one in frying oil, swill oil, waste oil.
Preferably, the solvent is selected from any one in carbon tetrachloride, 1,2- dichloroethanes, hexamethylene.
Preferably, the volume ratio of described kitchen waste grease and solvent is 1:1-1:4.
Preferably, described kitchen waste grease is 9 with the volume ratio of oleum:1-3:1.
Preferably, described reaction temperature is 40-80 DEG C
Preferably, the described reaction time is 2-6h.
Preferably, the application of described bio oil hydroxyl sulfoacid salt surfactant, is applied to field of petroleum exploitation.
Beneficial effects of the present invention：
1st, it is of the invention with kitchen waste grease as raw material, for kitchen waste grease resource higher value application provides new thinking,
Also for the synthesis of Surfactants Used for Oil field class provides raw material new way.
2nd, production low cost, process is simple, the environment-protecting asepsis of present invention synthesis, can rely on the existing surface-active in oil field
Agent production equipment device, is capable of achieving industrialized production.
3rd, the bio oil hydroxy sulfonate of present invention synthesis has preferable surface-active, and mass fraction is at 45 DEG C
The surface tension of 0.5% solution is 29.44mN/m.
4th, the bio oil hydroxy sulfonate of present invention synthesis has preferable interfacial activity, in 45 DEG C, 5000mg/L mineralisings
Under the conditions of degree, mass fraction is 0.5% solution and the interfacial tension of Daqing crude oil is 1.97 × 10-3mN/m。
5th, the bio oil hydroxy sulfonate with present invention synthesis is oil displacement agent, because without aromatic rings, phase in the raw material of synthesis
Sulfonate surfactant more very widely used today than oil field, with biological degradability it is good, environmental toxicity is small the characteristics of, to open
Hair is efficient, environment-friendly type oil displacement agent provides new method.
6th, bio oil hydroxyl sulfoacid salt surfactant of the invention is used for the oil displacement system of chemical flooding, energy and Daqing crude oil
Form 10-3The ultralow interfacial tension of mN/m number of levelss, realizes the purpose of optimal oil displacement efficiency.In 45 DEG C, 5000mg/L mineralisings
10 can be formed under the reservoir condition of degree with Daqing crude oil-3The ultralow interfacial tension of the mN/m orders of magnitude, improves oil recovery factor
12.52%, achieve and preferably improve oil recovery factor effect.
Specific embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, raw material and equipment for being used etc. is commercially available or commonly used in the art.
Method in following embodiments, unless otherwise instructed, is the conventional method of this area.
Embodiment 1
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, comprises the following steps：A, frying oil are through adding
Work is purified, and obtains treatment grease, and the treatment grease is the mixture of various triglycerides；B, will process purification frying oil with
1,2- dichloroethanes is by volume 1:2 are mixed in equipped with magnetic rotor, condenser pipe, the there-necked flask of thermometer, and three mouthfuls are burnt
Bottle is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, quickly stirs 10min, is completely dissolved kitchen waste grease, obtains shallow
The mixed solution of brown；C, it is 3 according to kitchen waste grease and oleum volume ratio:1, at room temperature toward the mixing of there-necked flask
Oleum is slowly dropped into solution, while quickly being stirred, after timing starts to instill oleum 10min, is warming up to anti-
40 DEG C of temperature is answered, and keeps reacting 6h；D, reach 6h after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until
When reaction solution is not in acidity, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 2min is sufficiently mixed, product poured into separatory funnel,
Use distilled water diluting solution, vibrate and stir, by 10min standing after, isolated bio oil hydroxy sulfonate it is thick
Product, the crude product is utilized in thermostat water bath after simulating vacuum distillation apparatus vacuum distillation 1.5h, obtains bio oil hydroxyl
The finished product of base sulfonate.Yield is 60.15%.
The bio oil hydroxy sulfonate that the present embodiment is obtained mass fraction at 45 DEG C is the surface tension of 0.5% solution
It is 30.12mN/m, under the conditions of 45 DEG C, 5000mg/L salinities, mass fraction is 0.5% solution and the interface of Daqing crude oil
Tension force is 2.16 × 10-3mN/m。
It is 5.26cm in length, a diameter of 2.54cm, permeability is 0.136 μm2Grand celebration natural core on be simulated
Oil displacement experiment.Step is：Water drive to aqueous 98% first is injected with Daqing oil field, metaideophone 0.4PV (rock pore volume) concentration is
Bio oil hydroxy sulfonate surfactant solution prepared by 0.5% the present embodiment, then sequent water flooding to the port of export loses
Oil, can improve oil recovery factor 12.52% on the basis of water drive.
Embodiment 2
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, comprises the following steps：A, frying oil are through adding
Work is purified, and obtains treatment grease, and the treatment grease is the mixture of various triglycerides；B, will process purification frying oil with
1,2- dichloroethanes is by volume 1:1 is mixed in equipped with magnetic rotor, condenser pipe, the there-necked flask of thermometer, and three mouthfuls are burnt
Bottle is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, quickly stirs 16min, is completely dissolved kitchen waste grease, obtains shallow
The mixed solution of brown；C, it is 8 according to kitchen waste grease and oleum volume ratio:1, at room temperature toward the mixing of there-necked flask
Oleum is slowly dropped into solution, while quickly being stirred, after timing starts to instill oleum 13min, is warming up to anti-
Temperature 50 C is answered, and keeps reacting 4h；D, reach 4h after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until
When reaction solution is not in acidity, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 3min is sufficiently mixed, product poured into separatory funnel,
Use distilled water diluting solution, vibrate and stir, by 12min standing after, isolated bio oil hydroxy sulfonate it is thick
Product, the crude product is utilized in thermostat water bath after simulating vacuum distillation apparatus vacuum distillation 1.8h, obtains bio oil hydroxyl
The finished product of base sulfonate.Yield is 54.82%.
The bio oil hydroxy sulfonate that the present embodiment is obtained mass fraction at 45 DEG C is the surface tension of 0.5% solution
It is 32.68mN/m, under the conditions of 45 DEG C, 5000mg/L salinities, mass fraction is 0.5% solution and the interface of Daqing crude oil
Tension force is 2.39 × 10-3mN/m。
It is 5.52cm in length, a diameter of 2.56cm, permeability is 0.147 μm2Grand celebration natural core on be simulated
Oil displacement experiment.Step is：Water drive to aqueous 98% first is injected with Daqing oil field, metaideophone 0.4PV (rock pore volume) concentration is
Bio oil hydroxy sulfonate surfactant solution prepared by 0.5% the present embodiment, then sequent water flooding to the port of export loses
Oil, can improve oil recovery factor 10.92% on the basis of water drive.
Embodiment 3
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, comprises the following steps：A, frying oil are through adding
Work is purified, and obtains treatment grease, and the treatment grease is the mixture of various triglycerides；B, will process purification frying oil with
Hexamethylene is by volume 1:During 2 are mixed in equipped with magnetic rotor, condenser pipe, the there-necked flask of thermometer, there-necked flask is placed in
In heat collecting type constant-temperature heating magnetic stirring apparatus, 20min is quickly stirred, be completely dissolved kitchen waste grease, obtain light brown
Mixed solution；C, it is 7 according to kitchen waste grease and oleum volume ratio:1, at room temperature toward in the mixed solution of there-necked flask
Oleum is slowly dropped into, while quickly being stirred, after timing starts to instill oleum 15min, reaction temperature is warming up to
80 DEG C, and keep reacting 2h；D, reach 2h after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until reaction solution
When not in acidity, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 5min is sufficiently mixed, product is poured into separatory funnel, with distillation
Water dilute solution, vibrates and stirs, by after 15min standings, the crude product of isolated bio oil hydroxy sulfonate will
The crude product, using after simulating vacuum distillation apparatus vacuum distillation 2h, obtains bio oil hydroxy sulfonate in thermostat water bath
Finished product.Yield is 65.78%.
The bio oil hydroxy sulfonate that the present embodiment is obtained mass fraction at 45 DEG C is the surface tension of 0.5% solution
It is 29.64mN/m, under the conditions of 45 DEG C, 5000mg/L salinities, mass fraction is 0.5% solution and the interface of Daqing crude oil
Tension force is 1.85 × 10-3mN/m。
It is 5.47cm in length, a diameter of 2.51cm, permeability is 0.143 μm2Grand celebration natural core on be simulated
Oil displacement experiment.Step is：Water drive to aqueous 98% first is injected with Daqing oil field, metaideophone 0.4PV (rock pore volume) concentration is
Bio oil hydroxy sulfonate surfactant solution prepared by 0.5% the present embodiment, then sequent water flooding to the port of export loses
Oil, can improve oil recovery factor 13.04% on the basis of water drive.
Embodiment 4
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, comprises the following steps：A, frying oil are through adding
Work is purified, and obtains treatment grease, and the treatment grease is the mixture of various triglycerides；B, will process purification frying oil with
Carbon tetrachloride is by volume 1:During 2 are mixed in equipped with magnetic rotor, condenser pipe, the there-necked flask of thermometer, there-necked flask is put
In heat collecting type constant-temperature heating magnetic stirring apparatus, 20min is quickly stirred, be completely dissolved kitchen waste grease, obtain light brown
Mixed solution；C, it is 7 according to kitchen waste grease and oleum volume ratio:1, at room temperature toward the mixed solution of there-necked flask
In be slowly dropped into oleum, while quickly stirred, after timing starts to instill oleum 10min, be warming up to reaction temperature
60 DEG C of degree, and keep reacting 4h；D, reach 4h after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until reaction
When liquid is not in acidity, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 2min is sufficiently mixed, product is poured into separatory funnel, with steaming
Distilled water dilute solution, vibrates and stirs, after 10min stands, the crude product of isolated bio oil hydroxy sulfonate,
The crude product is utilized in thermostat water bath after simulating vacuum distillation apparatus vacuum distillation 2h, obtain bio oil hydroxy sulfonate
Finished product.Yield is 71.69%.
The bio oil hydroxy sulfonate that the present embodiment is obtained mass fraction at 45 DEG C is the surface tension of 0.5% solution
It is 31.27mN/m, under the conditions of 45 DEG C, 5000mg/L salinities, mass fraction is 0.5% solution and the interface of Daqing crude oil
Tension force is 2.01 × 10-3mN/m。
It is 5.73cm in length, a diameter of 2.58cm, permeability is 0.151 μm2Grand celebration natural core on be simulated
Oil displacement experiment.Step is：Water drive to aqueous 98% first is injected with Daqing oil field, metaideophone 0.4PV (rock pore volume) concentration is
Bio oil hydroxy sulfonate surfactant solution prepared by 0.5% the present embodiment, then sequent water flooding to the port of export loses
Oil, can improve oil recovery factor 12.15% on the basis of water drive.
Embodiment 5
A kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, comprises the following steps：A, frying oil are through adding
Work is purified, and obtains treatment grease, and the treatment grease is the mixture of various triglycerides；B, will process purification frying oil with
1,2- dichloroethanes is by volume 1:4 are mixed in equipped with magnetic rotor, condenser pipe, the there-necked flask of thermometer, and three mouthfuls are burnt
Bottle is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, quickly stirs 10min, is completely dissolved kitchen waste grease, obtains shallow
The mixed solution of brown；C, it is 9 according to kitchen waste grease and oleum volume ratio:1, at room temperature toward the mixing of there-necked flask
Oleum is slowly dropped into solution, while quickly being stirred, after timing starts to instill oleum 15min, is warming up to anti-
Temperature 50 C is answered, and keeps reacting 3h；D, reach 3h after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until
When reaction solution is not in acidity, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 5min is sufficiently mixed, product poured into separatory funnel,
Use distilled water diluting solution, vibrate and stir, by 15min standing after, isolated bio oil hydroxy sulfonate it is thick
Product, the crude product is utilized in thermostat water bath after simulating vacuum distillation apparatus vacuum distillation 1.5h, obtains bio oil hydroxyl
The finished product of base sulfonate.Yield is 49.57%.
The bio oil hydroxy sulfonate that the present embodiment is obtained mass fraction at 45 DEG C is the surface tension of 0.5% solution
It is 32.83mN/m, under the conditions of 45 DEG C, 5000mg/L salinities, mass fraction is 0.5% solution and the interface of Daqing crude oil
Tension force is 2.48 × 10-3mN/m。
It is 5.19cm in length, a diameter of 2.52cm, permeability is 0.129 μm2Grand celebration natural core on be simulated
Oil displacement experiment.Step is：Water drive to aqueous 98% first is injected with Daqing oil field, metaideophone 0.4PV (rock pore volume) concentration is
Bio oil hydroxy sulfonate surfactant solution prepared by 0.5% the present embodiment, then sequent water flooding to the port of export loses
Oil, can improve oil recovery factor 11.68% on the basis of water drive.
Embodiment described above is a kind of preferably scheme of the invention, not makees any formal to the present invention
Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (8)
1. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease, it is characterised in that comprise the following steps：
A, the processed purification of kitchen waste grease, obtain treatment grease, and the treatment grease is the mixing of several triglycerides
Thing；
B, kitchen waste grease and the solvent that will process purification are mixed in and are burnt equipped with magnetic rotor, condenser pipe, three mouthfuls of thermometer
In bottle, there-necked flask is placed in heat collecting type constant-temperature heating magnetic stirring apparatus, quickly stirs 10-20min, makes kitchen waste grease complete
CL, obtains the mixed solution of light brown；
C, at room temperature toward oleum is slowly dropped into the mixed solution of there-necked flask, while quickly being stirred, timing is opened
After beginning to instill oleum 10-15min, heat up and be incubated；
D, reach the reaction time after, toward reaction solution instilling ammoniacal liquor is hydrolyzed neutralization reaction, until reaction solution is in acidity
When, stop that ammoniacal liquor is added dropwise, after reaction solution stirring 2-5min is sufficiently mixed, product is poured into separatory funnel, use distilled water diluting
Solution, vibrates and stirs, and stands 10-15min, the crude product of isolated bio oil hydroxy sulfonate, by the crude product
In the thermostat water bath using after simulating vacuum distillation apparatus vacuum distillation 1.5-2h, obtain bio oil hydroxy sulfonate into
Product.
2. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease according to claim 1, it is special
Levy and be, kitchen waste grease described in step a is selected from any one in frying oil, swill oil, waste oil.
3. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease according to claim 1, it is special
Levy and be, solvent described in step b is selected from any one in carbon tetrachloride, 1,2- dichloroethanes, hexamethylene.
4. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease according to claim 1, it is special
Levy and be, the volume ratio of kitchen waste grease and solvent described in step b is 1:1-1:4.
5. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease according to claim 1, it is special
Levy and be, the kitchen waste grease described in step c is 9 with the volume ratio of oleum:1-3:1.
6. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease according to claim 1, it is special
Levy and be, the reaction temperature described in step c is 40-80 DEG C.
7. a kind of bio oil hydroxyl sulfoacid salt production process based on kitchen waste grease according to claim 1, it is special
Levy and be, the reaction time described in step c is 2-6h.
8. a kind of bio oil hydroxyl sulfoacid salt surfactant based on kitchen waste grease according to claim 1 should
With, it is characterised in that it is applied to field of petroleum exploitation.
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| CN109762613A (en) * | 2019-02-26 | 2019-05-17 | 太原理工大学 | A kind of method that novel water-coal slurry dispersing agent is prepared by bio oil |
| CN113880510A (en) * | 2021-10-19 | 2022-01-04 | 山西省交通科技研发有限公司 | Stabilizer for road base mixture and construction method thereof |
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Application publication date: 20170613 |