CN108587589A - A kind of preparation method of inhibition microcapsules - Google Patents
A kind of preparation method of inhibition microcapsules Download PDFInfo
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- CN108587589A CN108587589A CN201810312875.3A CN201810312875A CN108587589A CN 108587589 A CN108587589 A CN 108587589A CN 201810312875 A CN201810312875 A CN 201810312875A CN 108587589 A CN108587589 A CN 108587589A
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- core material
- corrosion inhibiter
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- inhibition
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- 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
- C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
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- 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
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Materials Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
A kind of preparation method of inhibition microcapsules at room temperature mixes pyridine quaternary ammonium salt, thiocarbamide, methenamine and polyacrylamide in proportion, soluble in water, obtains solution A；Sodium carbonate, sodium tripolyphosphate are added in solution A, solution B is obtained；The solution B configured is poured slowly into instrument, handles to obtain the corrosion inhibiter powder for including framework material by second fluid nozzle；Low density polyethylene (LDPE), ethylene vinyl acetate copolymer, polyvinylpyrrolidone and propylene glycol methyl ether acetate mix in proportion, and molten condition is heated under high temperature；Fluid state is formed using the corrosion inhibiter powder obtained in step 1 as core material particles；Using the liquid of the molten condition obtained by step 2 as wall material by second fluid nozzle atomized spray in the core material particles circulated, after core material completes embedding, it is discharged from fluid bed, obtain final products inhibition microcapsules, the present invention has the characteristics of control corrosion inhibiter rate of release, extension action time.
Description
Technical field
The present invention relates to solid microcapsules technology field, more particularly to a kind of preparation method of inhibition microcapsules.
Background technology
In recent years, China increases native country oil field prospecting, exploitation, to obtain more stable resources.In order to improve yield, I
Need to produce large number of equipment, and enable them to work long hours as far as possible, this requires us to adopt various measures to length
The equipment that phase is in oil well bottom does anti-corrosion treatment.
Oil extraction equipment can be had electrochemical corrosion, sour under the particular surroundings in shaft bottom by various types of corrosion
(hydrogen sulfide, carbon dioxide), dissolved oxygen corrosion etc. are lost, but wherein being affected of generating of acid corrosion, so for a long time all
It is the focus of people.Mainly there are two kinds of material antiseptic and Process anti-corrosion in relation to method of inhibiting corrosion at present：Material antiseptic is
The property of equipment and materials itself is improved, hot 317 welding rods are such as equipped with using chrome-molybdenum steel (12Cr2A1MoV), postwelding is through 750
DEG C heat treatment；And Process anti-corrosion is then by filling corrosion inhibiter, playing the role of slowing down corrosion.
Currently, being developed a variety of corrosion inhibiter, there are imidazoles, compounding quaternized pyridinium salt, organophosphor acids etc.
Deng, but be directly to pour into corrosion inhibiter mostly in injection process.Although such kind of mode is simple directly, also some
Perhaps insufficient.
1. oil well BOTTOM LAYER ENVIRONMENT is severe, it is typically located at high temperature, high pressure conditions.If corrosion inhibiter is directly poured into, a large amount of inhibitions
Agent can decompose, volatilizees or not reach during the addition process site of action and just exhaust, these factors all strong influences are existing
There is the effect of corrosion inhibiter；
2. directly pouring into corrosion inhibiter, action time is ofer short duration, cannot play long-term corrosion-resisting function.
Invention content
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of preparation sides of inhibition microcapsules
Corrosion inhibiter is combined with solid microcapsules and produces inhibition microcapsules, both protects corrosion inhibiter in this way by method, its physicochemical property is made to tie up
It is fixed to keep steady, and can extend its action time by micropore quantity, and anti-corrosion capability is performed to most preferably.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of preparation method of inhibition microcapsules, includes the following steps：
Step 1：It is prepared by core material：
At room temperature, it is 5 by mass ratio:1:1 pyridine quaternary ammonium salt, thiocarbamide, methenamine and quality is pyridine quaternary ammonium salt
1/15 polyacrylamide mixing, it is soluble in water, it is slowly stirred 5min so that solute is evenly dispersed, obtains solution A；
By framework material sodium carbonate, the sodium tripolyphosphate with the quality such as polyacrylamide, with 1:Solution is added in 1 mass ratio
In A, it is slowly stirred until solid matter all dissolvings, obtains solution B；
Under extraneous normal pressure power, spray-dried instrument inlet air temperature is set as 80 DEG C, and leaving air temp is set as 40 DEG C, by what is configured
Solution B is poured slowly into instrument, is atomized, is dried by second fluid nozzle, obtains including skeleton after about 0.5~1.0h
The corrosion inhibiter powder of material；
Step 2：It is prepared by wall material：
Wall material selects：Low density polyethylene (LDPE) (LDPE), vinyl-vinyl acetate copolymer (EVA), polyvinylpyrrolidone
(PVP) and propylene glycol methyl ether acetate (PGMEA) mass ratio is about 5:5:5:1, gross mass be corrosion inhibiter powder quality 1/3~
1/2, it is mixed uniformly, molten condition is heated under 130~135 DEG C of high temperature；
Step 3：Fluidisation spraying：
It using the corrosion inhibiter powder obtained in step 1 as core material particles, is placed on distribuor of fluidized bed, is passed through 30 DEG C and does
Dry air makes core material is evenly dispersed to be suspended in carrying air, forms fluid state；
It after about 3min, using the liquid of the molten condition obtained by step 2 as wall material, is rapidly added in fluidized bed plant, leads to
Cross second fluid nozzle atomization, be uniformly sprayed in the core material particles circulated in the form of bottom is sprayed, the wall material of molten condition with
The reduction (temperature is less than wall material fusing point in fluid bed, can become solid-state from molten condition) for temperature gradually solidifies and is deposited in core
Material surface forms the moderate uniform wall film of thickness, fluidized-bed spraying, core is completed after about 0.8~1.2h by repeated multiple times cycle
After material completes embedding, it is discharged from fluid bed, obtains final products inhibition microcapsules.
Beneficial effects of the present invention：
The addition of core material middle skeleton material makes capsule density increase, and oil well bottom can be reached under natural conditions；It can change
Become the states of matter of the internal corrosion inhibiter for including；Internal corrosion inhibiter is protected by solid microcapsules, corrosion inhibiter is enable to exist
Stable state is kept before playing effect；Corrosion inhibiter rate of release can be controlled by adjusting the quantity of micropore on cyst wall, is made
Corrosion inhibiter is discharged with iptimum speed, is extended action time, is played best effect；It can prevent internal harmful to human body or environment
Substance loss in air.
Description of the drawings
Fig. 1 is the preparation flow figure of the present invention.
Fig. 2 is the structural schematic diagram of the present invention.
Fig. 3 is the optical microscope image (× 200) of inhibition microcapsules.
Specific implementation mode
Invention is further described in detail below in conjunction with the accompanying drawings.
Embodiment 1
Step 1：It is prepared by core material：
At room temperature, the polyacrylamide of 50g pyridine quaternary ammonium salts, 10g thiocarbamides, 10g methenamines and about 10/3g is molten
In 200ml water, it is slowly stirred 5min so that solute is evenly dispersed, obtains solution A；
By framework material sodium carbonate, the sodium tripolyphosphate with the quality such as polyacrylamide, with 1:Solution is added in 1 mass ratio
In A, it is slowly stirred until solid matter all dissolvings, obtains solution B；
Under extraneous normal pressure power, spray-dried instrument inlet air temperature is set as 80 DEG C, and leaving air temp is set as 40 DEG C, by what is configured
Solution B is poured slowly into instrument, is atomized, is dried by second fluid nozzle, is obtained after 0.5h comprising framework material
Corrosion inhibiter powder；
As shown in Figure 1, from corrosion inhibiter to dry link, is handled by the modes such as liquefying, being atomized, obtain including framework material
Corrosion inhibiter powder.
Step 2：It is prepared by wall material：
Wall material selects：Low density polyethylene (LDPE) (LDPE), vinyl-vinyl acetate copolymer (EVA), polyvinylpyrrolidone
(PVP) and propylene glycol methyl ether acetate (PGMEA) quality is respectively 10g, 10g, 10g, 2g, and gross mass is about 32g, is mixed
Uniformly, it is heated to molten condition under 130 DEG C of high temperature；
As shown in Figure 1, wall material after melt process, becomes liquid.
Step 3：Fluidisation spraying：
It using the corrosion inhibiter powder obtained in step 1 as core material particles, is placed on distribuor of fluidized bed, is passed through 30 DEG C and does
Dry air makes core material is evenly dispersed to be suspended in carrying air, forms fluid state；
After 3min, using the liquid of the molten condition obtained by step 2 as wall material, it is rapidly added in fluidized bed plant, passes through
Second fluid nozzle is atomized, and is uniformly sprayed in the core material particles circulated in the form of bottom is sprayed, the wall material of molten condition with
The reduction (temperature is less than wall material fusing point in fluid bed, can become solid-state from molten condition) of temperature gradually solidifies and is deposited in core material
Surface forms the moderate uniform wall film of thickness by repeated multiple times cycle, and fluidized-bed spraying is completed after 0.8h, and core material completes packet
After burying, it is discharged from fluid bed, obtains final products inhibition microcapsules.
As shown in Figure 1, by liquid wall material in corrosion inhibiter powder in step 1 and step 2, through fluid bed embedding, discharge, obtain
To product.
After testing, the design feature of product shows the internal structure of inhibition microcapsules as shown in Figure 2；MIcrosope image is as schemed
Shown in 3, inhibition microcapsules, particle size distribution range is 400~1000 μm, and wall material thickness is 0.2~10 μm, adapts to pH value 5-8, is fitted
Answer 50-100 DEG C of temperature.
Embodiment 2
Step 1：It is prepared by core material：
At room temperature, 100g pyridine quaternary ammonium salts, 20g thiocarbamides, 20g methenamines and 20/3 polyacrylamide are dissolved in
In 500ml water, it is slowly stirred 5min so that solute is evenly dispersed, obtains solution A；
By framework material sodium carbonate, the sodium tripolyphosphate with the quality such as polyacrylamide, with 1:Solution is added in 1 mass ratio
In A, it is slowly stirred until solid matter all dissolvings, obtains solution B；
Under extraneous normal pressure power, spray-dried instrument inlet air temperature is set as 80 DEG C, and leaving air temp is set as 40 DEG C, by what is configured
Solution B is poured slowly into instrument, is atomized, is dried by second fluid nozzle, is obtained after 1.0h comprising framework material
Corrosion inhibiter powder；
Step 2：It is prepared by wall material：
Wall material selects：Low density polyethylene (LDPE) (LDPE), vinyl-vinyl acetate copolymer (EVA), polyvinylpyrrolidone
(PVP) and propylene glycol methyl ether acetate (PGMEA) quality is respectively 20g, 20g, 20g, 4g, and gross mass is about 76g, is mixed
Uniformly, it is heated to molten condition under 135 DEG C of high temperature；
Step 3：Fluidisation spraying：
It using the corrosion inhibiter powder obtained in step 1 as core material particles, is placed on distribuor of fluidized bed, is passed through 30 DEG C and does
Dry air makes core material is evenly dispersed to be suspended in carrying air, forms fluid state；
After 3min, using the liquid of the molten condition obtained by step 2 as wall material, it is rapidly added in fluidized bed plant, passes through
Second fluid nozzle is atomized, and is uniformly sprayed in the core material particles circulated in the form of bottom is sprayed, the wall material of molten condition with
The reduction (temperature is less than wall material fusing point in fluid bed, can become solid-state from molten condition) of temperature gradually solidifies and is deposited in core material
Surface forms the moderate uniform wall film of thickness by repeated multiple times cycle, and fluidized-bed spraying is completed after 1.0h, and core material completes packet
After burying, it is discharged from fluid bed, obtains final products inhibition microcapsules.
Embodiment 3
Step 1：It is prepared by core material：
At room temperature, 100g pyridine quaternary ammonium salts, 20g thiocarbamides, 20g methenamines and 20/3 polyacrylamide are dissolved in
In 500ml water, it is slowly stirred 5min so that solute is evenly dispersed, obtains solution A；
By framework material sodium carbonate, the sodium tripolyphosphate with the quality such as polyacrylamide, with 1:Solution is added in 1 mass ratio
In A, it is slowly stirred until solid matter all dissolvings, obtains solution B；
Under extraneous normal pressure power, spray-dried instrument inlet air temperature is set as 80 DEG C, and leaving air temp is set as 40 DEG C, by what is configured
Solution B is poured slowly into instrument, is atomized, is dried by second fluid nozzle, is obtained after 1.0h comprising framework material
Corrosion inhibiter powder；
Step 2：It is prepared by wall material：
Wall material selects：Low density polyethylene (LDPE) (LDPE), vinyl-vinyl acetate copolymer (EVA), polyvinylpyrrolidone
(PVP) and propylene glycol methyl ether acetate (PGMEA) quality is respectively 20g, 20g, 20g, 4g, and gross mass is about 76g, is mixed
Uniformly, it is heated to molten condition under 130 DEG C of high temperature；
Step 3：Fluidisation spraying：
It using the corrosion inhibiter powder obtained in step 1 as core material particles, is placed on distribuor of fluidized bed, is passed through 30 DEG C and does
Dry air makes core material is evenly dispersed to be suspended in carrying air, forms fluid state；
After 3min, using the liquid of the molten condition obtained by step 2 as wall material, it is rapidly added in fluidized bed plant, passes through
Second fluid nozzle is atomized, and is uniformly sprayed in the core material particles circulated in the form of bottom is sprayed, the wall material of molten condition with
The reduction (temperature is less than wall material fusing point in fluid bed, can become solid-state from molten condition) of temperature gradually solidifies and is deposited in core material
Surface forms the moderate uniform wall film of thickness by repeated multiple times cycle, and fluidized-bed spraying is completed after 1.2h, and core material completes packet
After burying, it is discharged from fluid bed, obtains final products inhibition microcapsules.
Operation principle of the present invention：Inhibition microcapsules are poured into oil well, oil well bottom can be reached under field conditions (factors).Because
There is the presence of part water in oil well depths, and the water-soluble material on cyst wall will dissolve, and form a series of micro channels according to quantity.It is internal
Corrosion inhibiter oil well environment is entered by the channel of these new formation.
In recovery process, water is poured by the external world in the side line of oil well, and remaining crude oil is taken out of from bottom.In this process
Middle corrosion inhibiter will reach the part corroded with certain rate along with oil water mixture, play alleviation, inhibiting effect.
In the process, on cyst wall micropore quantity, be the key factor for determining action time length of the invention.Pass through
The quality for adjusting wall material oil-soluble (LDPE, EVA) and water-soluble substances (PVP) can control the number of micropore, and then influence
To the action time of inhibition microcapsules, achieve the purpose that effectively to inhibit corrosion.
Claims (1)
1. a kind of preparation method of inhibition microcapsules, which is characterized in that include the following steps：
Step 1：It is prepared by core material：
At room temperature, it is 5 by mass ratio:1:1 pyridine quaternary ammonium salt, thiocarbamide, methenamine and quality is pyridine quaternary ammonium salt 1/15
Polyacrylamide mixing, it is soluble in water, be slowly stirred 5min so that solute is evenly dispersed, obtains solution A；
By framework material sodium carbonate, the sodium tripolyphosphate with the quality such as polyacrylamide, with 1:1 mass ratio is added in solution A,
It is slowly stirred until solid matter all dissolvings, obtains solution B；
Under extraneous normal pressure power, spray-dried instrument inlet air temperature is set as 80 DEG C, and leaving air temp is set as 40 DEG C, the solution that will have been configured
B is poured slowly into instrument, is atomized, is dried by second fluid nozzle, is obtained after 0.5~1.0h comprising framework material
Corrosion inhibiter powder；
Step 2：It is prepared by wall material：
Wall material selects：Low density polyethylene (LDPE), vinyl-vinyl acetate copolymer, polyvinylpyrrolidone and propylene glycol monomethyl ether second
Acid esters mass ratio is 5:5:5:1, gross mass is the 1/3~1/2 of the corrosion inhibiter powder quality that step 2 obtains, is mixed
It is even, it is heated to molten condition under 130~135 DEG C of high temperature；
Step 3：Fluidisation spraying：
It using the corrosion inhibiter powder obtained in step 1 as core material particles, is placed on distribuor of fluidized bed, is passed through 30 DEG C of dry skies
Gas makes core material is evenly dispersed to be suspended in carrying air, forms fluid state；
After about 3min, using the liquid of the molten condition obtained by step 2 as wall material, it is rapidly added in fluidized bed plant, passes through two
Fluid tip is atomized, and is uniformly sprayed in the core material particles circulated in the form of bottom is sprayed, the wall material of molten condition is with temperature
The reduction of degree gradually solidifies and is deposited in core surfaces, by repeated multiple times cycle, forms the moderate uniform wall film of thickness, and 0.8
Fluidized-bed spraying is completed after~1.2h it is discharged from fluid bed, obtains the micro- glue of final products inhibition after core material completes embedding
Capsule.
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| CN201810312875.3A CN108587589A (en) | 2018-04-09 | 2018-04-09 | A kind of preparation method of inhibition microcapsules |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762546A (en) * | 2019-01-28 | 2019-05-17 | 西南科技大学 | A kind of preparation method of the acrylamide being loaded with corrosion inhibiter-bentonite capsule |
| CN109796851A (en) * | 2019-02-18 | 2019-05-24 | 中南大学 | A kind of slow-release graphene anticorrosive paint and preparation method thereof |
| CN109880605A (en) * | 2019-03-27 | 2019-06-14 | 中国石油化工股份有限公司 | A kind of gas injection anti-channeling curing agent spansule and anti-migration agent and preparation method thereof |
| CN113265184A (en) * | 2021-05-08 | 2021-08-17 | 北京科技大学 | Self-repairing coating capable of simultaneously recovering corrosion resistance and adhesive force and preparation method thereof |
| CN113846328A (en) * | 2021-09-23 | 2021-12-28 | 沈阳防锈包装材料有限责任公司 | Slow-release gas-phase antirust agent and preparation method thereof |
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| CN102250604A (en) * | 2011-05-27 | 2011-11-23 | 门正国 | Controlled releasing microcapsule for scale prevention, wax prevention or viscosity reduction of oil well |
| CN104650838A (en) * | 2013-11-22 | 2015-05-27 | 中国石油天然气股份有限公司 | Salt tolerant corrosion and scale inhibitor for underground oil-gas wells and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20090142498A1 (en) * | 2006-03-10 | 2009-06-04 | Stefan Faber | Coat or coating to counteract crystalline deposits |
| CN102250604A (en) * | 2011-05-27 | 2011-11-23 | 门正国 | Controlled releasing microcapsule for scale prevention, wax prevention or viscosity reduction of oil well |
| CN104650838A (en) * | 2013-11-22 | 2015-05-27 | 中国石油天然气股份有限公司 | Salt tolerant corrosion and scale inhibitor for underground oil-gas wells and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762546A (en) * | 2019-01-28 | 2019-05-17 | 西南科技大学 | A kind of preparation method of the acrylamide being loaded with corrosion inhibiter-bentonite capsule |
| CN109762546B (en) * | 2019-01-28 | 2021-06-25 | 西南科技大学 | Preparation method of corrosion inhibitor-loaded acrylamide-bentonite capsule |
| CN109796851A (en) * | 2019-02-18 | 2019-05-24 | 中南大学 | A kind of slow-release graphene anticorrosive paint and preparation method thereof |
| CN109880605A (en) * | 2019-03-27 | 2019-06-14 | 中国石油化工股份有限公司 | A kind of gas injection anti-channeling curing agent spansule and anti-migration agent and preparation method thereof |
| CN109880605B (en) * | 2019-03-27 | 2020-04-14 | 中国石油化工股份有限公司 | Curing agent sustained-release capsule and channeling-preventing agent for gas injection and channeling prevention and preparation method thereof |
| CN113265184A (en) * | 2021-05-08 | 2021-08-17 | 北京科技大学 | Self-repairing coating capable of simultaneously recovering corrosion resistance and adhesive force and preparation method thereof |
| CN113265184B (en) * | 2021-05-08 | 2022-01-25 | 北京科技大学 | Self-repairing coating capable of simultaneously recovering corrosion resistance and adhesive force and preparation method thereof |
| CN113846328A (en) * | 2021-09-23 | 2021-12-28 | 沈阳防锈包装材料有限责任公司 | Slow-release gas-phase antirust agent and preparation method thereof |
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Application publication date: 20180928 |