CN110079285A - A kind of super-hydrophobic particle and preparation method thereof for underwater leak stopping - Google Patents
A kind of super-hydrophobic particle and preparation method thereof for underwater leak stopping Download PDFInfo
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- CN110079285A CN110079285A CN201910357384.5A CN201910357384A CN110079285A CN 110079285 A CN110079285 A CN 110079285A CN 201910357384 A CN201910357384 A CN 201910357384A CN 110079285 A CN110079285 A CN 110079285A
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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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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Abstract
The super-hydrophobic particle and preparation method thereof that the present invention relates to a kind of for underwater leak stopping, the hydrophobic membrane with micron order hydrophobic material for being successively wrapped in particle core surfaces and the hydrophobic membrane with nanoscale hydrophobic material of the super-hydrophobic particle are by by the mixture of hydrophobic type resin and corresponding curing agent, it mixes and stirs with micron order hydrophobic material and nanoscale hydrophobic material respectively and to form mixed liquor A and mixed liquid B, mixed liquor A and mixed liquid B are successively mixed and stirred with particle core material again, successively obtained in the surface-crosslinked solidification of particle core material.Compared with prior art, the present invention solves the problems such as curing time existing for current plugging material is long, bearing capacity is poor, leak stopping success rate is low, with quick, efficient, lasting leak stopping performance, and its preparation process is simple, application technology is convenient, has boundless application prospect.
Description
Technical field
The present invention relates to plugging material technical field, more particularly, to a kind of super-hydrophobic particle for underwater leak stopping and its
Preparation method.
Background technique
Effective closure to underwater leak paths is the major issue that Civil Engineering engineering faces.To guarantee to block quality,
Need to provide anhydrous construction environment, this considerably increases Practical Project amounts, reduce and block efficiency.Thus, it is how effectively real
It is now underwater to block, it has also become hot spot concerned by people.
Currently, generalling use GEL USED FOR PLUGGING WELL LOST CIRCULATION carries out underwater leak stopping.A kind of water-soluble polymer of GEL USED FOR PLUGGING WELL LOST CIRCULATION, leak stopping slurry
Liquid easily enters in the drop ply of crack or blowhole, and is detained in gap and blowhole, with the cementing conjunction of drop ply rock, reaches
Leak stopping purpose.But GEL USED FOR PLUGGING WELL LOST CIRCULATION curing time at drop ply is long, is easy mutually to mix with formation fluid, thinning, thus in leakage portion
Bit stream mistake causes leak stopping to be failed.Solid concentration is low in the sealing agent simultaneously, and the particle size distribution of solid phase particles is narrow, for splitting
The biggish seepage place of width range is stitched, plugging effect is poor, and universality is not strong.
Patent CN104726078A discloses a kind of GEL USED FOR PLUGGING WELL LOST CIRCULATION, and the sealing agent is by 4-8 parts of Sodium Polyacrylates, 15-25
Part staple, 0.05-0.1 parts of ammonium persulfates, 1-5 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 15-25 parts of wood powders, 30-65
Part acrylamide is made.The sealing agent can penetrate into seepage place in the case where compression, pass through the bonding of gel and seepage place
Underwater block is realized in effect.But it is long the time required to sealing agent solidification, and when pressure is big, easily sealing leakage glue is broken up, leak stopping effect
Rate is not high.Therefore, it needs to develop the underwater leak stopping material that a kind of leak-stopping speed is fast, high-efficient, plugging effect is lasting.
Summary of the invention
The object of the invention is in order to overcome the above-mentioned curing time of plugging material in the prior art is long, bearing capacity is poor,
The problems such as leak stopping success rate is low and provide a kind of with quick, efficient, lasting leak stopping performance, and its preparation process is simple, answers
It is convenient with technology, the super-hydrophobic particle and preparation method thereof for underwater leak stopping with boundless application prospect.
The purpose of the present invention can be achieved through the following technical solutions:
The present invention provides a kind of super-hydrophobic particle for underwater leak stopping, including particle core material and is successively wrapped in particle
The hydrophobic membrane with micron order hydrophobic material and the hydrophobic membrane with nanoscale hydrophobic material of core surfaces.
Preferably, the particle core material is the granular material of continuous grading, is selected from quartz sand, desert sand, river sand, sea
One or more of sand and CHARACTERISTICS OF TAILINGS SAND, partial size 0.1-1.2mm.
Preferably, it is successively wrapped in the hydrophobic membrane with micron order hydrophobic material of particle core surfaces and there is nanoscale
The hydrophobic membrane of hydrophobic material by by the mixture of hydrophobic type resin and corresponding curing agent, respectively with micron order hydrophobic material and
Nanoscale hydrophobic material mixes and stirs to form mixed liquor A and mixed liquid B, then mixed liquor A and mixed liquid B are successively mixed with particle core material
With, successively particle core material it is surface-crosslinked solidification obtain.
Preferably:
The hydrophobic type resin is selected from fluorine silicon resin, fluororesin, organic siliconresin, benzyl transparent silicon resin and polyamides
One or more of amine-modified epoxy resin；
The curing agent is selected from one of isocyanates, m-phenylene diamine (MPD), triethylene tetramine and tetraethylenepentamine or several
Kind.
Further preferably:
When the hydrophobic type resin uses fluorine silicon resin or fluororesin, the curing agent uses isocyanates；
When the hydrophobic type resin is using organic siliconresin, benzyl transparent silicon resin or polyamide modified epoxy resin,
The curing agent uses one or more of m-phenylene diamine (MPD), triethylene tetramine, tetraethylenepentamine.
Preferably:
The micron order hydrophobic material in waterproof powder, organosilicon powder hydrophober and Kynoar micro mist one
Kind or several, partial size 5-70um；
The nanoscale hydrophobic material is selected from Nano-meter SiO_22、Al2O3, one or more of CuO, partial size 5-
80nm。
Preferably, which is made by the component of following parts by weight: 92-94 parts of particle core material, hydrophobic type resin
2-5 parts, 0.5-2 parts of curing agent, 2-4 parts of micron order hydrophobic material and 0.5-1 parts of nanoscale hydrophobic material.
The present invention also provides a kind of preparation methods of super-hydrophobic particle for underwater leak stopping, comprising the following steps:
(1) particle core material is heated, after drying its surface moisture, stands, is cooling；
(2) micron order hydrophobic material and hydrophobic resin and corresponding curing agent are mixed, is stirred evenly, mixed liquor is made
A；
(3) nanoscale hydrophobic material and hydrophobic resin and corresponding curing agent are mixed, is stirred evenly, mixed liquor is made
B；
(4) cooling to particle core material, mixed liquor A and mixed liquid B is successively added, stirs evenly, is formed and is successively wrapped in
Grain core surfaces the hydrophobic membrane with micron order hydrophobic material and the hydrophobic membrane with nanoscale hydrophobic material, be made described in
Super-hydrophobic particle for underwater leak stopping.
Preferably:
In step (1), it is heated to 150-200 DEG C and is dried；
In step (4), when particle core material is cooled to 60-80 DEG C, mixed liquor A and mixed liquid B is successively added.
The surface of covering material used in the present invention (hydrophobic type resin and curing agent) can be far below water, therefore covering material exists
Particle core surfaces cladding, can form hydrophobic membrane, simultaneously because the bonding and solidification of resin improve the machine of particle core material
Tool intensity, and then improve its bearing capacity.
So that it is had a superhydrophobic characteristic principle according to lotus leaf surface mastoid process structure, the present invention by building surface there are it is micro--
It receives the hydrophobic membrane of second level coarse structure, further enhances the hydrophobicity of particle, reach super-hydrophobic rank.Meanwhile passing through tree
The coarse structure that micron order hydrophobic material and nanoscale hydrophobic material are formed firmly is attached on by the bonding and solidification of rouge
Grain core surfaces effectively promote the durability that the particle dredges super hydrophobic functional.When immersion, the super-hydrophobic particle can spontaneous reunion,
To reduce its contact area with water, can quickly seepage place forms stable underwater aggregate structure under water, may refer to
Bright book attached drawing Fig. 1 (a) and Fig. 1 (b).It will form powerful stiction between the particle of continuous grading, enhance inside and outside its anti-blocking layer
The ability of pressure difference improves shut-off capacity.
Compared with prior art, the invention has the following advantages that the super-hydrophobic particle for being used for underwater leak stopping solves mesh
The problems such as curing time existing for preceding plugging material is long, bearing capacity is poor, leak stopping success rate is low has quickly, efficiently, persistently
Leak stopping performance, and its preparation process is simple, application technology is convenient, has boundless application prospect.
Detailed description of the invention
Fig. 1 (a) is super-hydrophobic particle of the present invention under water from agglomeration, and Fig. 1 (b) is the partial enlarged view of Fig. 1 (a).
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The CHARACTERISTICS OF TAILINGS SAND of 92 parts of continuous gradings (partial size 0.1-1.2mm) is heated to 200 DEG C, dries its surface moisture, it is quiet
It sets；And 3 parts of micron order organosilicon powders and 1.5 parts of fluorine silicon resins and 0.5 part of isocyanates mix are uniform, mixed liquor A is made；
By 1 part of Nano-meter SiO_22It is uniform with 1.5 parts of fluorine silicon resins and 0.5 part of isocyanates mix, mixed liquid B is made；To continuous grading
When particle core material is cooled to 80 DEG C, mixed liquor A and mixed liquid B is successively added, stirs evenly, obtains this for underwater leak stopping
Super-hydrophobic particle.
Embodiment 2
The common river sand of 93 parts of continuous gradings (partial size 0.1-1.2mm) is heated to 180 DEG C, dries its surface moisture,
It stands；And 2 parts of Kynoar micro mists and 1.5 parts of organic siliconresins and 0.5 part of m-phenylene diamine (MPD) curing agent mix are uniform, it is made
Mixed liquor A；1 part of nanometer CuO and 1.5 parts of organic siliconresins and 0.5 part of m-phenylene diamine (MPD) curing agent mix are uniform, mixed liquor is made
B；When the particle core material of continuous grading is cooled to 70 DEG C, mixed liquor A and mixed liquid B is successively added, stirs evenly, obtains this
Super-hydrophobic particle for underwater leak stopping.
Embodiment 3
The CHARACTERISTICS OF TAILINGS SAND of 94 parts of continuous gradings (partial size 0.1-1.2mm) is heated to 150 DEG C, dries its surface moisture, it is quiet
It sets；And 2 parts of micron order waterproof powder and 1.5 parts of benzyl transparent silicon resins and 0.5 part of triethylene tetramine mix are uniform, it is made mixed
Close liquid A；By 0.6 part of Nano-meter SiO_22It is uniform with 1 part of benzyl transparent silicon resin and 0.4 part of triethylene tetramine mix, mixing is made
Liquid B；When the particle core material of continuous grading is cooled to 60 DEG C, mixed liquor A and mixed liquid B is successively added, stirs evenly, obtains
This is used for the super-hydrophobic particle of underwater leak stopping.
When the super-hydrophobic particle immersion for being used for underwater leak stopping for produced by the present invention, the super-hydrophobic particle can spontaneous reunion,
To reduce its contact area with water, can quickly seepage place forms stable underwater aggregate structure under water, realize underwater seep
The Rapid-Repair at position is leaked, and the super-hydrophobicity of the particle can effectively promote its water pressure resistance ability, realize the efficient of underwater repair
Change, long-actingization.Referring to Figure of description Fig. 1 (a) and Fig. 1 (b).
Water droplet is carried out in the contact angle on its surface to the super-hydrophobic particle for being used for underwater leak stopping made from embodiment 1,2 and 3
The performance tests such as test and resistance to hydrostatic pressure, curing time, and compared with the big crack sealing agent of currently used 803 type, as a result
It is shown in Table 1.
1 super-hydrophobic particle performance test of table
As shown in Table 1, the super-hydrophobic and resistance to hydrostatic pressure of the super-hydrophobic particle for underwater leak stopping prepared by the present invention
It can be excellent.
For the durability of testing product, the super-hydrophobic particle and 803 of underwater leak stopping will be used for made from embodiment 1,2 and 3
After sealing agent is placed 6 months under natural conditions, water droplet is carried out in the contact angle test and resistance to hydrostatic pressure on its surface, curing time
Test, the results are shown in Table 2.
2 super-hydrophobic particle durability test of table (after 6 months)
As shown in Table 2, super-hydrophobic and resistance to quiet behind super-hydrophobic particle 6 months for underwater leak stopping prepared by the present invention
Hydraulic pressure performance is still excellent, has good endurance quality.
Embodiment 4
The quartz sand of 92 parts of continuous gradings (partial size 0.1-1.2mm) is heated to 200 DEG C, dries its surface moisture, it is quiet
It sets；And 4 parts of micron order organosilicon powders and 3 parts of fluorine silicon resins and 1.5 parts of isocyanates mixs are uniform, mixed liquor A is made；It will
0.5 part of Nano-meter SiO_22It is uniform with 2 parts of fluorine silicon resins and 0.5 part of isocyanates mix, mixed liquid B is made；To continuous grading
When grain core material is cooled to 80 DEG C, mixed liquor A and mixed liquid B is successively added, stirs evenly, obtains this for the super of underwater leak stopping
Hydrophobic granule.
Desert sand (partial size 0.1-1.2mm) of 93 parts of continuous gradings is heated to 200 DEG C by embodiment 5, dries its surface
Moisture is stood；And 2 parts of micron order organosilicon powders and 1.5 parts of fluorine silicon resins and 0.3 part of isocyanates mix are uniform, it is made
Mixed liquor A；By 0.5 part of Nano-meter SiO_22It is uniform with 1 part of fluorine silicon resin and 0.2 part of isocyanates mix, mixed liquid B is made；To even
When the particle core material of continuous gradation is cooled to 80 DEG C, mixed liquor A and mixed liquid B is successively added, stirs evenly, obtains this and be used for water
The super-hydrophobic particle of lower leak stopping.
Embodiment 6
The present embodiment is substantially the same manner as Example 1, the difference is that, in the present embodiment, the selection of nanoscale hydrophobic material
Nanometer Al2O3It is mixed with CuO according to mass ratio 1:1.Partial size is 5-80nm.
Embodiment 7
The present embodiment is substantially the same manner as Example 1, the difference is that, in the present embodiment, the selection of micron order hydrophobic material
Organosilicon powder hydrophober and Kynoar micro mist are mixed according to mass ratio 1:1.Partial size is 5-70um.
Embodiment 8
The present embodiment is substantially the same manner as Example 1, the difference is that, in the present embodiment, hydrophobic type resin uses fluorine silicon
Resin and fluororesin are mixed according to 1:1, and curing agent uses isocyanates.
Embodiment 9
The present embodiment is substantially the same manner as Example 1, the difference is that, in the present embodiment, hydrophobic type resin uses polyamides
Amine-modified epoxy resin, curing agent use tetraethylenepentamine.
Embodiment 10
The present embodiment is substantially the same manner as Example 1, the difference is that, in the present embodiment, particle core material is continuous grading
Partial size be 0.1-1.2mm river sand and sea sand mixture.
The above-mentioned description to embodiment is for ease of ordinary skill in the art to understand and use the invention.It is ripe
The personnel for knowing art technology obviously easily can make various modifications to these embodiments, and general original described herein
It ought to use in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, this field
Technical staff's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be in guarantors of the invention
Within the scope of shield.
Claims (8)
1. a kind of super-hydrophobic particle for underwater leak stopping, which is characterized in that including particle core material and be successively wrapped in particle
The hydrophobic membrane with micron order hydrophobic material and the hydrophobic membrane with nanoscale hydrophobic material of core surfaces.
2. a kind of super-hydrophobic particle for underwater leak stopping according to claim 1, which is characterized in that the particle cores
Material is the granular material of continuous grading, selected from one or more of quartz sand, desert sand, river sand, sea sand and CHARACTERISTICS OF TAILINGS SAND, grain
Diameter is 0.1-1.2mm.
3. a kind of super-hydrophobic particle for underwater leak stopping according to claim 1, which is characterized in that be successively wrapped in
The hydrophobic membrane with micron order hydrophobic material and the hydrophobic membrane with nanoscale hydrophobic material of grain core surfaces pass through will be hydrophobic
The mixture of type resin and corresponding curing agent, mixes and stirs to be formed and mixes with micron order hydrophobic material and nanoscale hydrophobic material respectively
Liquid A and mixed liquid B, then mixed liquor A and mixed liquid B are successively mixed and stirred with particle core material, it is successively surface-crosslinked solid in particle core material
Change obtains.
4. a kind of super-hydrophobic particle for underwater leak stopping according to claim 3, it is characterised in that:
The hydrophobic type resin is selected from fluorine silicon resin, fluororesin, organic siliconresin, benzyl transparent silicon resin and polyamide and changes
One or more of property epoxy resin；
The curing agent is selected from one or more of isocyanates, m-phenylene diamine (MPD), triethylene tetramine and tetraethylenepentamine.
5. a kind of super-hydrophobic particle for underwater leak stopping according to claim 3, it is characterised in that:
The micron order hydrophobic material be selected from one of waterproof powder, organosilicon powder hydrophober and Kynoar micro mist or
It is several, partial size 5-70um；
The nanoscale hydrophobic material is selected from Nano-meter SiO_22、Al2O3, one or more of CuO, partial size 5-80nm.
6. a kind of super-hydrophobic particle for underwater leak stopping according to claim 3, which is characterized in that the super-hydrophobic particle
Be made by the component of following parts by weight: 92-94 parts of particle core material, 2-5 parts of hydrophobic type resin, 0.5-2 parts of curing agent, micron order are hated
2-4 parts and 0.5-1 parts of nanoscale hydrophobic material of water material.
7. the preparation method of the super-hydrophobic particle for underwater leak stopping as described in claim 1~6 is any, which is characterized in that
The following steps are included:
(1) particle core material is heated, after drying its surface moisture, stands, is cooling；
(2) micron order hydrophobic material and hydrophobic resin and corresponding curing agent are mixed, is stirred evenly, mixed liquor A is made；
(3) nanoscale hydrophobic material and hydrophobic resin and corresponding curing agent are mixed, is stirred evenly, mixed liquid B is made；
(4) cooling to particle core material, mixed liquor A and mixed liquid B is successively added, stirs evenly, is formed and is successively wrapped in particle cores
The hydrophobic membrane with micron order hydrophobic material and the hydrophobic membrane with nanoscale hydrophobic material on material surface are made described and are used for
The super-hydrophobic particle of underwater leak stopping.
8. the preparation method of the super-hydrophobic particle according to claim 7 for underwater leak stopping, it is characterised in that:
In step (1), it is heated to 150-200 DEG C and is dried；
In step (4), when particle core material is cooled to 60-80 DEG C, mixed liquor A and mixed liquid B is successively added.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295677A (en) * | 2019-05-22 | 2019-10-01 | 同济大学 | Integrated super-hydrophobic particle and its preparation method and application is insulated for assembled architecture seam waterproof |
| CN110305670A (en) * | 2019-05-22 | 2019-10-08 | 同济大学 | A kind of super-hydrophobic particle and preparation method thereof for surface layer water storage |
| CN111851870A (en) * | 2020-03-31 | 2020-10-30 | 同济大学 | Building roof waterproof and heat insulation integrated super-hydrophobic particle, and preparation method and application thereof |
| CN112094077A (en) * | 2020-03-31 | 2020-12-18 | 同济大学 | Ecological planting plate for surface water storage and preparation method thereof |
| CN112480902A (en) * | 2020-11-26 | 2021-03-12 | 四川省帕提科斯能源科技有限公司 | Intelligent encapsulated acid and use method thereof |
| CN114774094A (en) * | 2022-04-22 | 2022-07-22 | 中国海洋石油集团有限公司 | Permanent type blast hole plugging material used after screen pipe perforation and preparation method |
| CN115337676A (en) * | 2022-08-19 | 2022-11-15 | 同济大学 | Super-hydrophobic-super-oleophilic filter material for oil-water separation of oily sewage and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295677A (en) * | 2019-05-22 | 2019-10-01 | 同济大学 | Integrated super-hydrophobic particle and its preparation method and application is insulated for assembled architecture seam waterproof |
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| CN111851870A (en) * | 2020-03-31 | 2020-10-30 | 同济大学 | Building roof waterproof and heat insulation integrated super-hydrophobic particle, and preparation method and application thereof |
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| CN114774094A (en) * | 2022-04-22 | 2022-07-22 | 中国海洋石油集团有限公司 | Permanent type blast hole plugging material used after screen pipe perforation and preparation method |
| CN115337676A (en) * | 2022-08-19 | 2022-11-15 | 同济大学 | Super-hydrophobic-super-oleophilic filter material for oil-water separation of oily sewage and preparation method and application thereof |
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