CN107652408A - A kind of conversed phase micro emulsion copolymerization interlayer modification clay alteration AM MAH pour point depressant for crude oil and preparation method thereof - Google Patents
A kind of conversed phase micro emulsion copolymerization interlayer modification clay alteration AM MAH pour point depressant for crude oil and preparation method thereof Download PDFInfo
- Publication number
- CN107652408A CN107652408A CN201710960900.4A CN201710960900A CN107652408A CN 107652408 A CN107652408 A CN 107652408A CN 201710960900 A CN201710960900 A CN 201710960900A CN 107652408 A CN107652408 A CN 107652408A
- Authority
- CN
- China
- Prior art keywords
- interlayer
- clay
- crude oil
- mah
- point depressant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Lubricants (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention provides a kind of conversed phase micro emulsion copolymerization interlayer modification clay alteration AM MAH pour point depressant for crude oil and its preparation.Preparation method includes：Interlayer dressing agent and clay is soluble in water, mix；AM and MAH monomers are added into the mixed solution of interlayer dressing agent and clay, mixes, obtains the aqueous phase solution containing monomer；Hexamethylene, emulsifying agent and initiator are added, and is stirred to mixing, obtains Microemulsion；The lower heating response of stirring, is produced.The present invention polymerize to form organic inorganic composite hydrophilic nano micro-sphere material with inorganic clay using water-soluble monomer AM and MAH in inverse emulsion system.Simple process, easily operated, production cost is low.Hydrophilic nano micro-sphere material provided by the invention, its interlayer size is 50 500nm, performance with good reduction condensation point of crude oil, there is acid and alkali-resistance simultaneously, with preferable broad spectrum activity, the pour-point depressant of land oil field high wax content oil is can not only be used for, is also used as the pour-point depressant of offshore oilfield high wax content oil.
Description
Technical field
The present invention relates to pour point depressant for crude oil, particularly a kind of conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH is former
Oily pour-point depressant and preparation method thereof.
Background technology
Crude oil is a kind of multi-component complex hydrocarbon mixture containing paraffin, and contains a certain amount of colloid and pitch
Matter paraffin is dissolved in crude oil, can be separated out when temperature reduces from crude oil, and it is brilliant to form wax；And as temperature declines, wax is brilliant to be increased
It is more, tridimensional network is formed, crude oil is lost flowability, the exploitation and conveyer belt to oil carry out very big difficulty.Waxy crude oil
Rheological characteristic and the defeated technique of pipe be always that high wax is former both at home and abroad at present by one of the main bugbear of China's Oil ＆ Gas Storage circle scientific research
The conveying of oil mainly uses physical method and chemical method.Physical method is mainly the mode of done site by site heated transportation, and is produced from China
Part crude oil particularly northeast and North China crude oil belong to high glutinous, Gao Ning high-wax oil, the low temperature rheological behavior of this quasi-oil
It is poor, heated transportation technique is mostly used at present.Heated transportation technique will not only consume substantial amounts of fuel oil and power, Er Qiejia
For hot pipeline after stopping transportation, there is larger insecurity in restarting for pipeline.At present at some crude oil pipeline of China
In running with low flux, pipeline heating facility scarce capacity, conduit running energy consumption rises and security declines, and section of tubing must not
Do not take it is positive and negative transport line mode, waste substantial amounts of human and material resources, considerably increase conveying cost.Chemical method has emulsification to drop
Solidifying method, suspension conveying pour point depression method and pour-point depressant pour point depression method.Emulsifying pour point depression and suspension conveying pour point depression method needs substantial amounts of water, anhydrous
Or water-deficient area can not use, and exist and post-process the problem of difficult (being such as dehydrated), thus have very big office in applying at the scene
It is sex-limited.Pour-point depressant pour point depression method changes the form that wax is brilliant in crude oil, makes wax be not easy to be formed at normal temperatures by adding chemical treatments
Three-dimensional space network structure, with the purpose for reaching pour point depression, improving crude oil low temperature flow.Addition pour-point depressant is simple to operate, equipment
Small investment, and need not post-process, it is easy to carry out automatic management to oil transportation process, also allows at sea recovering the oil and collecting defeated mistake
Used in journey.Therefore, into crude oil add chemical pour-point depression agent be realize crude oil normal temperature so that low temperature conveying it is most easy and most have
The method of effect.Pour-point depressant pour point depression technology starts from Davis in 1931 and contracted with chlorinated paraffin and naphthalene by Friedel-crafts earliest
Reaction is closed, has synthesized the pour-point depressant that the mankind apply earliest, i.e. paraflow, this pour-point depressant is used primarily in lubricating oil, so far
Still in extensive use.At present, a lot, the conventional crude oil of the type and quantity of the pour point depressant for crude oil of domestic and foreign literature and patent report
Pour-point depressant mainly has following several types：Ethylene maleic acid anhydride copolymer and its derivative, (methyl) Long Chain Alkyl Acrylate class
Polymer and its derivative, phenylethylene-maleic anhydride-Long Chain Alkyl Acrylate copolymer and its derivative, acrylic acid higher alcohols
Ester-maleic anhydride-copolymer-maleic anhydride and its derivative.These pour-point depressants have the preferable glutinous effect of pour point depression drop to waxy crude oil
Fruit, played an important role in China's waxy crude oil conveys technique.But the technology still has the problem of certain:(1)
Pour-point depressant has specific aim, and different crude oils are applicable different types of pour-point depressant；(2) under the conditions of integrated treatment, crude oil temperature returns
Rise and low temperature rheological behaviour is had a great influence, temperature recovery be present and deteriorate area；(3) dynamic after waxy crude oil integrated treatment and static state are steady
It is fixed ageing to be not met by pipe safety service condition；(4) addition of pour-point depressant causes the deposition of wax in pipeline to increase.
Nano material is because of its distinctive small-size effect, skin effect and quantum tunneling effect, in all fields of national economy
There is extremely wide application prospect.Polymer microsphere refers to that diameter in nanoscale to micron, is shaped as spherical or other geometry
The high polymer material or polymer composite of body.The research and application of polymeric microball material develop very fast in recent years
Speed, due to special pattern and size, polymer microsphere possesses the specific function not available for other materials.Polymer microsphere
Using each corner for having penetrated into our lives, from bulk products such as coating, paper surface coating, cosmetics, to use
Micro-capsule, Separation of Proteins in medicament slow release control have been applied to polymeric microball material with the high added value of chromatography media.
There is not been reported for conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil at present.
The content of the invention
It is an object of the invention to provide a kind of conversed phase micro emulsion copolymerization interlayer to modify clay alteration AM-MAH pour point depressant for crude oil
And preparation method thereof.
Conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil provided by the present invention is according to bag
The method for including following step is prepared：
1) it is interlayer dressing agent and clay is soluble in water, mix, obtain the mixed solution of interlayer dressing agent and clay；
2) acrylamide (AM) is added into the mixed solution of above-mentioned interlayer dressing agent and clay and maleic anhydride (MAH) is single
Body, and stir to mixing, obtain the aqueous phase solution containing monomer；
3) hexamethylene, emulsifying agent and initiator are added into the above-mentioned aqueous phase solution containing monomer, and is stirred to mixing,
Obtain Microemulsion；
4) above-mentioned Microemulsion is reacted in a heated condition, obtains conversed phase micro emulsion copolymerization interlayer and repair
Adorn clay alteration AM-MAH pour point depressant for crude oil.
In above method step 1), the interlayer dressing agent is multiple quaternary ammonium salts clay interlaminar modifier.
The multiple quaternary ammonium salts clay interlaminar modifier is according to patent《A kind of multiple quaternary ammonium salts clay interlaminar modifier and its
Preparation method》(application number：200810102231.8) disclosed in method be prepared.
The preparation method of the multiple quaternary ammonium salts clay interlaminar modifier, comprises the following steps：
1) unrighted acid is dissolved in dimethylbenzene, and mixed with catalyst, be heated to 180-220 DEG C, added
Diethylenetriamine is reacted, and obtains bisamide；
2) bisamide is mixed with ethanol, is heated to 30-40 DEG C, add polyethylene polyamine, carried out at 70-80 DEG C anti-
Should, obtain multiple quaternary ammonium salts clay interlaminar modifier；
Wherein, unrighted acid used is one in nutmeg oleic acid, palmitoleic acid, oleic acid, castor oil acid or erucic acid
The mixture of kind or its any combination；Polyethylene polyamine used is ethylenediamine, triethylene tetramine, TEPA or the chloro- 2- of 3-
The mixture of one kind or its any combination in hydroxypropyl-trimethyl ammonium chloride；Used catalyst be alundum (Al2O3), phosphoric acid or
Any one in boric acid.
In above-mentioned preparation method, the mol ratio of unrighted acid, diethylenetriamine and polyethylene polyamine is 1.5-2：
0.8-1：The mol ratio of 0.8-1, catalyst and unrighted acid is 0.05-0.1：0.08-1.2.
In step 1), when diethylenetriamine is reacted with unrighted acid, dimethylbenzene and catalyst, reaction temperature must
It must control between 180-220 DEG C, other types of reaction can occur less than 180-220 DEG C, higher than this temperature raw material medicine
It can decompose；The reaction time of the step is 1.5-2.5h；In step 2), reaction time 2-4h.
The clay is unselected clay, and wherein the weight/mass percentage composition of montmorillonite is 80%-98%.
The mass fraction of interlayer dressing agent, clay and water can be 0.3-0.5,4-6 and 80-100 successively.
Described mix is realized by stirring.
The rotating speed of the stirring can be 10000-15000r/min, and mixing time can be 20-40min.
In step 2), the mass fraction of acrylamide can be 9-11；MAH mass fraction can be 9-11；Speed of agitator can
For 10000-15000r/min, mixing time can be 20-40min.
In step 3), the mass fraction of hexamethylene can be 110-120.
Concretely azobisisobutyronitrile AIBN, its mass fraction can be 0.01-0.03 to the initiator.
Concretely mass ratio is 1 to the emulsifying agent：1 Span80 and Tweeen60 mixture, the quality of emulsifying agent
Number can be 0.2-0.4.
The rotating speed of the stirring can be 10000-15000r/min, and mixing time can be 20-40min.
In step 4), the reaction is carried out under agitation.
The rotating speed of the stirring can be 500-1000r/min.
The temperature of reaction can be 50-70 DEG C, and preferably 55-65 DEG C, the reaction time can be 120-150min.
Reaction, which finishes, obtains conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depression of crude oil agent materials, is not required to
The last handling process such as it is incubated.
The conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil is a kind of nanospheres,
Its interlayer size is 1-15.0um, concretely 1-2.5um, 1.5-3.5um, 1.5-3.5um, 5.0-10.0um, 5.0-
7.5um、10.0-15.0um、2.5-5.0um。
The conversed phase micro emulsion copolymerization interlayer being prepared by the above method modifies clay alteration AM-MAH pour point depressant for crude oil
Fall within protection scope of the present invention.
It is prepared by above-mentioned conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil nanospheres
Application in the pour-point depressant of waxy crude oil falls within protection scope of the present invention.
Conversed phase micro emulsion copolymerization interlayer provided by the invention modifies clay alteration AM-MAH pour point depression of crude oil agent materials, have with
Lower feature：
1) present invention polymerize using water-soluble monomer AM and MAH with inorganic clay in inverse emulsion system to be formed it is organic-
Inorganic composite hydrophilic nano micro-sphere material.
2) method provided by the invention for preparing polymeric microball material, simple process is easily operated, and production cost is low.
3) hydrophilic nano micro-sphere material provided by the invention, its interlayer size are 50-500nm, have good reduction
The performance of condensation point of crude oil, while there is acid and alkali-resistance, there is preferable broad spectrum activity, it is former to can not only be used for land oil field high-content wax
The pour-point depressant of oil, it is also used as the pour-point depressant of offshore oilfield high wax content oil.
Brief description of the drawings
Fig. 1 is that interlayer prepared by the embodiment of the present invention 1 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Fig. 2 is that interlayer prepared by the embodiment of the present invention 2 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Fig. 3 is that interlayer prepared by the embodiment of the present invention 3 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Fig. 4 is that interlayer prepared by the embodiment of the present invention 4 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Fig. 5 is that interlayer prepared by the embodiment of the present invention 5 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Fig. 6 is that interlayer prepared by the embodiment of the present invention 6 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Fig. 7 is that interlayer prepared by the embodiment of the present invention 7 modifies clay alteration AM-MAH pour point depression of crude oil agent material SEM photographs.
Embodiment
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., unless otherwise specified, commercially obtain.
In following embodiments, clay used is unselected clay, and wherein the weight/mass percentage composition of montmorillonite is 80%-98%.
Interlayer dressing agent used is according to patent《A kind of multiple quaternary ammonium salts clay interlaminar modifier and preparation method thereof》(the patent No.：
200810102231.8) preparation method obtain.
The preparation method of above-mentioned multiple quaternary ammonium salts clay interlaminar modifier, comprises the following steps：
1) unrighted acid (castor oil acid) is dissolved in dimethylbenzene, and mixed with catalyst alundum (Al2O3), added
Heat adds diethylenetriamine and reacted, obtain bisamide to 200 DEG C；
2) bisamide is mixed with ethanol, is heated to 30-40 DEG C, polyethylene polyamine (diethylenetriamine) is added, in 70-
80 DEG C are reacted, and obtain multiple quaternary ammonium salts clay interlaminar modifier；
In above-mentioned preparation method, the mol ratio of unrighted acid, diethylenetriamine and polyethylene polyamine is 2:1:1, urge
Agent and the mol ratio of unrighted acid are 0.1:1.
In step 1), the reaction time that diethylenetriamine is reacted with unrighted acid, dimethylbenzene and catalyst is
2h；In step 2), reaction time 3h.
In following embodiments, pour point depression rate determination experiment method is：
(1) the perfluoroalkyl acrylate modified ethylene acetate pour point depressant for crude oil of 5000mg/L the present embodiment synthesis is configured
The aqueous solution；
(2) it is 1 according to volume ratio：0.2 ratio measures crude oil and the aqueous solution obtained above, is mixed under the conditions of 30 DEG C
Close；
(3) the type viscosimeters of BROOK Field III measure viscosity of mixed liquid is utilized.
The preparation of embodiment 1, conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.3g interlayers dressing agent and 4g clays are dissolved in 100g water, mix, obtain the mixed solution of clay；
2) acrylamide 9g and maleic anhydride 9g is added into the mixed solution of above-mentioned clay, and mixing speed is
10000r/min, stirring 20min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 110g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN0.01%, and 20min is stirred under the conditions of low whipping speed 10000r/min to mixing, the Water-In-Oil stablized
Type emulsion；
4) Microemulsion of aforementioned stable is heated into 55 DEG C under the conditions of 500r/min is stirred to be reacted
120min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 1 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 1.
As shown in Figure 1, the interlayer size of resulting materials is 1-2.5um.
After tested, its pour point depression of crude oil rate is 89.4%.
The preparation of embodiment 2, conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.5g interlayers dressing agent and 6g clays are dissolved in 80g water, mix, obtain the mixed solution of clay；
2) acrylamide 11g and maleic anhydride 11g is added into the mixed solution of above-mentioned clay, and mixing speed is
15000r/min, stirring 40min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 120g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN0.03%, and 40min is stirred under the conditions of low whipping speed 15000r/min to mixing, the Water-In-Oil stablized
Type emulsion；
4) Microemulsion of aforementioned stable is heated into 65 DEG C under the conditions of 1000r/min is stirred to be reacted
150min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 2 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 2.
As shown in Figure 2, the interlayer size of resulting materials is 1.5-3.5um.
After tested, its pour point depression of crude oil rate is 90.2%.
The preparation of embodiment 3, conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.4g interlayers dressing agent and 5g clays are dissolved in 90g water, mix, obtain the mixed solution of clay；
2) acrylic acid 10g and maleic anhydride 10g is added into the mixed solution of above-mentioned clay, and mixing speed is
12500r/min, stirring 30min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 115g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN0.02%, and 30min is stirred under the conditions of low whipping speed 12500r/min to mixing, the Water-In-Oil stablized
Type emulsion；
4) Microemulsion of aforementioned stable is heated into 60 DEG C under the conditions of 750r/min is stirred to be reacted
135min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 3 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 3.
From the figure 3, it may be seen that the interlayer size of resulting materials is 1.0-3.5um.
After tested, its pour point depression of crude oil rate is 88.3%.
Embodiment 4, prepare conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.3g interlayers dressing agent and 4g clays are dissolved in 80g water, mix, obtain the mixed solution of clay；
2) propenyl 9g and maleic anhydride 9g is added into the mixed solution of above-mentioned clay, and mixing speed is 15000r/
Min, stirring 20min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 115g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN0.02%, and 30min is stirred under the conditions of low whipping speed 12500r/min to mixing, the Water-In-Oil stablized
Type emulsion；
4) Microemulsion of aforementioned stable is heated into 60 DEG C under the conditions of 750r/min is stirred to be reacted
135min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 4 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 4.
As shown in Figure 4, the interlayer size of resulting materials is 5.0-10.0um.
After tested, its pour point depression of crude oil rate is 91.8%.
Embodiment 5, prepare conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.4g interlayers dressing agent and 5g clays are dissolved in 90g water, mix, obtain the mixed solution of clay；
2) acrylamide 10g and maleic anhydride 10g is added into the mixed solution of above-mentioned clay, and mixing speed is
12500r/min, stirring 30min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 110g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN0.01%, and 20min is stirred under the conditions of low whipping speed 15000r/min to mixing, the Water-In-Oil stablized
Type emulsion；
4) Microemulsion of aforementioned stable is heated into 55 DEG C under the conditions of 500r/min is stirred to be reacted
120min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 5 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 5.
As shown in Figure 5, the interlayer size of resulting materials is 5.0-7.5um.
After tested, its pour point depression of crude oil rate is 88.6%.
Embodiment 6, prepare conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.3g interlayers dressing agent and 6g clays are dissolved in 100g water, mix, obtain the mixed solution of clay；
2) acrylamide 11g and maleic anhydride 11g is added into the mixed solution of above-mentioned clay, and mixing speed is
10000r/min, stirring 40min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 110g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN 0.03%, and 40min is stirred under the conditions of low whipping speed 10000r/min to mixing, the oil bag stablized
Water type emulsion；
4) Microemulsion of aforementioned stable is heated into 65 DEG C under the conditions of 500r/min is stirred to be reacted
120min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 6 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 6.
It will be appreciated from fig. 6 that the interlayer size of resulting materials is 10.0-15.0um.
After tested, its pour point depression of crude oil rate is 87.2%.
Embodiment 7, prepare conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil
1) 0.4g interlayers dressing agent and 4g clays are dissolved in 90g water, mix, obtain the mixed solution of clay；
2) acrylamide 10g and maleic anhydride 10g is added into the mixed solution of above-mentioned clay, and mixing speed is
12500r/min, stirring 30min obtain the aqueous phase solution containing water-soluble monomer and clay to mixing；
3) added into aqueous phase solution 120g hexamethylenes, emulsifying agent (Span80 0.15g, Tween60 0.15g) and
Initiator A IBN 0.03%, and 20min is stirred under the conditions of low whipping speed 10000r/min to mixing, the oil bag stablized
Water type emulsion；
4) Microemulsion of aforementioned stable is heated into 60 DEG C under the conditions of 750r/min is stirred to be reacted
150min, obtain conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil.
Fig. 7 is organic-inorganic composite hydrophilic nano-microballoons material SEM photograph prepared by embodiment 7.
As shown in Figure 7, the interlayer size of resulting materials is 2.5-5.0um.
After tested, its pour point depression of crude oil rate is 92.3%.
Claims (7)
1. a kind of method for preparing conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil, including：
1) it is interlayer dressing agent and clay is soluble in water, mix, obtain the mixed solution of interlayer dressing agent and clay；
2) acrylamide and maleic anhydride monomer are added into the mixed solution of above-mentioned interlayer dressing agent and clay, and is stirred to mixed
It is even, obtain the aqueous phase solution containing monomer；
3) hexamethylene, emulsifying agent and initiator are added into the above-mentioned aqueous phase solution containing monomer, and is stirred to mixing, is obtained
Microemulsion；
4) above-mentioned Microemulsion is reacted in a heated condition, it is viscous obtains the modification of conversed phase micro emulsion copolymerization interlayer
Land reform AM-MAH pour point depressant for crude oil.
2. according to the method for claim 1, it is characterised in that：In step 1), the interlayer dressing agent is multiple quaternary ammonium
Salts clay interlaminar modifier；
The mass fraction of interlayer dressing agent, clay and water is followed successively by 0.3-0.5,4-6 and 80-100.
3. method according to claim 1 or 2, it is characterised in that：In step 2), the mass fraction of acrylamide is 9-
11；The mass fraction of maleic anhydride is 9-11.
4. according to the method any one of claim 1-3, it is characterised in that：In step 3), the mass fraction of hexamethylene
For 110-120；
The initiator is azobisisobutyronitrile AIBN, and its mass fraction is 0.01-0.03；
The emulsifying agent is that mass ratio is 1：1 Span80 and Tweeen60 mixture, the mass fraction of emulsifying agent is 0.2-
0.4。
5. according to the method any one of claim 1-4, it is characterised in that：In step 4), the reaction is under agitation
Carry out；
The rotating speed of the stirring is 500-1000r/min；
The temperature of reaction is 50-70 DEG C, reaction time 120-150min.
6. the conversed phase micro emulsion copolymerization interlayer modification clay alteration that the method any one of claim 1-5 is prepared
AM-MAH pour point depressant for crude oil.
7. the conversed phase micro emulsion copolymerization interlayer modification clay alteration AM-MAH pour point depressant for crude oil described in claim 6 is preparing the content of wax
Application in the pour-point depressant of crude oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960900.4A CN107652408B (en) | 2017-10-17 | 2017-10-17 | Reverse microemulsion polymerization interlayer modified clay AM-MAH crude oil pour point depressant and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960900.4A CN107652408B (en) | 2017-10-17 | 2017-10-17 | Reverse microemulsion polymerization interlayer modified clay AM-MAH crude oil pour point depressant and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107652408A true CN107652408A (en) | 2018-02-02 |
| CN107652408B CN107652408B (en) | 2020-03-06 |
Family
ID=61118648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710960900.4A Active CN107652408B (en) | 2017-10-17 | 2017-10-17 | Reverse microemulsion polymerization interlayer modified clay AM-MAH crude oil pour point depressant and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107652408B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109570211A (en) * | 2018-10-24 | 2019-04-05 | 昆明理工大学 | A kind of method of renovation of organic pollution soil |
| CN113185657A (en) * | 2021-03-31 | 2021-07-30 | 宁波锋成先进能源材料研究院有限公司 | Nano material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289523A (en) * | 2008-06-17 | 2008-10-22 | 中国海洋石油总公司 | Reversed phase emulsion polymerization organic-inorganic composite hydrophilic nano-microballoons, preparation and applications thereof |
| CN102108292A (en) * | 2009-12-29 | 2011-06-29 | 中国石油天然气股份有限公司 | Crude oil viscosity-reducing and depressant composite |
| CN102127409A (en) * | 2011-01-10 | 2011-07-20 | 中国科学院化学研究所 | Crude oil viscosity-breaking pour-point depressant composition, and preparation method and application thereof |
| CN106634916A (en) * | 2017-01-19 | 2017-05-10 | 北京奥友兴业科技发展有限公司 | Preparation method of novel water-based viscosity and pour point reducer |
-
2017
- 2017-10-17 CN CN201710960900.4A patent/CN107652408B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289523A (en) * | 2008-06-17 | 2008-10-22 | 中国海洋石油总公司 | Reversed phase emulsion polymerization organic-inorganic composite hydrophilic nano-microballoons, preparation and applications thereof |
| CN102108292A (en) * | 2009-12-29 | 2011-06-29 | 中国石油天然气股份有限公司 | Crude oil viscosity-reducing and depressant composite |
| CN102127409A (en) * | 2011-01-10 | 2011-07-20 | 中国科学院化学研究所 | Crude oil viscosity-breaking pour-point depressant composition, and preparation method and application thereof |
| CN106634916A (en) * | 2017-01-19 | 2017-05-10 | 北京奥友兴业科技发展有限公司 | Preparation method of novel water-based viscosity and pour point reducer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109570211A (en) * | 2018-10-24 | 2019-04-05 | 昆明理工大学 | A kind of method of renovation of organic pollution soil |
| CN113185657A (en) * | 2021-03-31 | 2021-07-30 | 宁波锋成先进能源材料研究院有限公司 | Nano material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107652408B (en) | 2020-03-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102584507B (en) | Special composite oil phase for high-temperature sensitized and emulsified explosive production process | |
| CN103755868B (en) | Shale gas slippery water pressure break friction reducer and preparation method thereof | |
| CN101289523B (en) | Reversed phase emulsion polymerization organic-inorganic composite hydrophilic nano-microballoons, preparation and applications thereof | |
| CN102732225A (en) | Thermal storage and insulation microcapsule for building material and preparation method thereof | |
| CN107488248A (en) | A kind of nano imvite and polymer composite viscosity reducer and preparation method thereof | |
| CN104762066B (en) | Compound microcapsules of storing energy through phase change and preparation method thereof | |
| CN102617769A (en) | Nanometer composite porous gel microsphere and preparation method thereof | |
| CN105085799A (en) | Preparation method and application of dilatation-retarding nano elastic microsphere in-depth profile controlling and oil displacing agent | |
| CN101805423A (en) | Method for preparing polyacrylamide nano microsphere system | |
| CN108329420A (en) | Low-tension polymer microballoon profile control agent and its preparation method and application | |
| CN107383273B (en) | A kind of viscous crude activator and preparation method thereof | |
| CN104357019A (en) | Low-temperature thermal control phase change microcapsule and preparation method thereof | |
| CN103409118B (en) | A kind of synthetic method of water-base drilling fluid ultrahigh-temperature stablizer | |
| CN110105933A (en) | Gel particle sealing agent and its preparation method and application | |
| CN107652408A (en) | A kind of conversed phase micro emulsion copolymerization interlayer modification clay alteration AM MAH pour point depressant for crude oil and preparation method thereof | |
| CN107236531A (en) | Shale gas pressure break environment-friendly type slippery water friction reducer and preparation method thereof | |
| CN106566522B (en) | A kind of timing rupture release type microcapsule degelling agent and preparation method thereof | |
| CN106957635A (en) | The microcapsule phase-change particle and preparation method of composite Nano copper and nano-graphene piece | |
| CN112851856A (en) | Salt-tolerant polymer microsphere plugging agent and preparation method thereof | |
| CN109082267A (en) | A method of addition manganese dioxide particle improves n-octadecane/polystyrene phase microcapsules hot property | |
| CN108456279A (en) | A kind of pour point depressant for crude oil and the preparation method and application thereof | |
| CN104211851B (en) | A kind of preparation method of mono-disperse polymer composite magnetic microballoon | |
| CN103936944B (en) | A kind of method of reversed phase emulsion polymerization organic-inorganic composite hydrophilic nano microsphere | |
| CN108559475A (en) | A kind of heat-resistant salt-resistant polyvinyl acetate ester microsphere and its preparation and application | |
| CN107603577A (en) | A kind of conversed phase micro emulsion copolymerization interlayer modification clay alteration AM VA pour point depressant for crude oil and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Applicant after: China Offshore Oil Group Co., Ltd. Applicant after: CNOOC research institute limited liability company Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Applicant before: China National Offshore Oil Corporation Applicant before: CNOOC Research Institute |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |