CN109233258A - A kind of preparation method of water shutoff material - Google Patents
A kind of preparation method of water shutoff material Download PDFInfo
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- CN109233258A CN109233258A CN201810727104.0A CN201810727104A CN109233258A CN 109233258 A CN109233258 A CN 109233258A CN 201810727104 A CN201810727104 A CN 201810727104A CN 109233258 A CN109233258 A CN 109233258A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of preparation methods of water shutoff material, belong to water shutoff material field.The carbohydrate in lac that the present invention adds can form intermolecular force with modified polyurethane powder, so that water shutoff material system internal bond strength is stronger, stability is more excellent, material aging can be effectively prevent to fall off, the present invention adds polyethyleneimine, in room temperature, under acid condition, the polyethyleneimine hydrogel of formation can solidify with modified polyurethane and isocyanates acts on the lower carbon dioxide generated with water and reacts, form aminoquinoxaline, tridimensional network is formed since ionic group interacts, lac plays filling effect wherein, binding force between raising system inside, there is bubble and hole after avoiding water shutoff material, improve the compactness of water shutoff material, it avoids permeable.The present invention solves the problems, such as to occur after current water shutoff material use that easy to fall off, anti-corrosive properties are poor.
Description
Technical field
The invention belongs to water shutoff material fields, and in particular to a kind of preparation method of water shutoff material.
Background technique
In the tunnel excavating process of the large-scale construction projects such as railway, highway, subway, as tunnelling footage increases, tunnel
Interior water yield increases, and water content is big in rock mass in tunnel, and water drenching occurs in top plate, keeps roof control more difficult.According to statistics, be crushed,
The ratio for accounting for Tunnel Engineering total amount rich in water and water drenching condition rock mass is up to 30% or so.Tunnel Water Leakage is durable to tunnel structure
Many adverse effects are generated with facility, traffic safety, ground buildings or structures and groundwater environment in stabilization, hole, percolating water promotees
Make concrete lining weathering, degrade, liner structure is caused to destroy；Percolating water can also soften country rock, cause surrouding rock deformation, lead to tunnel
Road load increases；Contain corrosive medium in some water seepage of tunnel, general lining concrete and masonry mortar is caused to corrode damage
It is bad, reduce the bearing capacity of lining cutting；In Han Qu, tunnel leak will cause abutment wall icing, invades clearance of tunnel, also will cause
Lining cutting frost heave rhegma, percolating water accelerate internal unit (communication, illumination, track etc.) corrosion, influence the normal use of equipment, shortens
The service life of line facility increases maintenance cost；Water damage causes subgrade settlement, substrate rhegma, the diseases such as rise soil, and causes
Rail track gauge horizontal distortion transfinites, frost heave cause in hole that route is uneven and hole in leak humidity to reduce wheel track viscous
Put forth effort, can seriously affect traffic safety；Water damage makes electrical isolation failure, short circuit, tripping, influences safe operation, causes electric leakage wound
Occurrences in human life event, therefore there is an urgent need to quickly and effectively water blockoffs, plugging material.
Currently, Tunnel Water Leakage material is slurries both at home and abroad, raw material largely uses toluene di-isocyanate(TDI)
(TDI), in addition to reducing the viscosity of material, it is often added with a large amount of organic solvent in product, such as acetone, dimethylbenzene, first
Benzene, butanone, ethyl acetate, butyl acetate etc..Occur that easy to fall off, anti-corrosive properties are poor asks although there is certain effect, after use
Topic.Therefore, producing a kind of water shutoff material that can solve the above problem has the very big market demand.
Summary of the invention
The technical problems to be solved by the invention: for occurring after current water shutoff material use, easy to fall off, anti-corrosive properties are poor
Problem provides a kind of preparation method of water shutoff material.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of water shutoff material includes the following steps:
(1) 5:1 ~ 2 in mass ratio；0.5 takes nanometer hydroxyapatite, carboxymethyl chitosan, lac mixing, by ratio of grinding media to material 20 ~ 30:
1 is added zirconium oxide ball milling pearl, and ball milling obtains ball milling material, takes ball milling material 1:3 in mass ratio ~ 6 that solvent A mixing is added, refrigerates, is added
The pore creating material of 2 ~ 4 times of ball milling material quality, supersonic oscillations obtain dispersion liquid, take dispersion liquid that 3 ~ 5 times of dispersion liquid quality of lemon is added
Acid solution mixing, stands, obtains feed liquid, spare；
(2) 3:1 ~ 2 take isocyanates, polyether polyol mixing in mass ratio, lead to nitrogen protection, and constant temperature stirring is cooled to 70 ~ 80
DEG C, reaction material is obtained, takes reaction material that the plasticizer of reaction material quality 4 ~ 8% is added, adjusting revolving speed is to be stirred, it is cooled to 60 ~
65 DEG C, be added the defoaming agent of reaction material quality 4 ~ 8%, the catalyst of reaction material quality 4 ~ 8%, 3 ~ 6 times of reaction material quality solvent
B adjusts revolving speed, is stirred, cooling, and discharging obtains modified polyurethane；
(3) 3:1:5 ~ 8 take polyethyleneimine, coupling agent in mass ratio, and modified polyurethane is mixed in batch mixer, and high-speed stirred is adjusted
PH is saved, the feed liquid that modified polyurethane quality 15 ~ 25% is added is uniformly mixed, and stands 2 ~ 5h to get water shutoff material.
Pore creating material in the step (1): 6:1 ~ 2 take paracide, potassium chloride mixing to get pore creating material in mass ratio.
Solvent A in the step (1): 8:0.1 ~ 0.4 takes glacial acetic acid, toluene mixing to get solvent A in mass ratio.
Plasticizer in the step (2): in mass ratio 5:1 ~ 2 take epoxidized soybean oil, triethyl citrate mixing to get
Plasticizer.
Defoaming agent in the step (2): 4:1 ~ 2 in mass ratio take silicone emulsion, dimethyl silicone polymer mixing to get
Defoaming agent.
Catalyst in the step (2): stannous octoate, isooctyl acid lead, any one in dibutyl tin dilaurate.
Solvent B in the step (2): 5:1 ~ 2 take dimethyl carbonate, acetone mixing to get solvent B in mass ratio.
High-speed stirred in the step (3) is to stir 20 ~ 35min with 1200 ~ 1400r/min.
Coupling agent in the step (3): any one in silane resin acceptor kh-550, KH-560, KH-570.
PH adjusting agent used in pH is adjusted in the step (3): 1:4 ~ 8 take citric acid, NaH in mass ratio2PO4Solution is mixed
It closes to get pH adjusting agent.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is mixed with carboxymethyl chitosan, lac through ball milling, acidleach refrigeration surpasses using nanometer hydroxyapatite as raw material
The processes such as sonication can effectively improve nanostructure, drop low-surface-energy when acting on modified polyurethane, reach uniform work
With, avoid part from excessively reuniting, the hole for reducing therefore occurring, and biocompatibility can be greatly promoted, improve water shutoff material
Toughness；
(2) carbohydrate in the lac that the present invention adds can form intermolecular force with modified polyurethane powder, so that water blockoff material
Material system internal bond strength is stronger, stability is more excellent, material aging can be effectively prevent to fall off, and the present invention adds polyethyleneimine,
Under room temperature, acid condition, the polyethyleneimine hydrogel of formation can solidify with modified polyurethane and isocyanates is acted on water
The carbon dioxide of lower generation reacts, and forms aminoquinoxaline, to form tridimensional network since ionic group interacts,
Lac plays filling effect wherein, improves the binding force between system inside, bubble and hole occurs after avoiding water shutoff material,
The compactness for improving water shutoff material avoids permeable.
Specific embodiment
Pore creating material: 6:1 ~ 2 take paracide, potassium chloride mixing to get pore creating material in mass ratio.
Plasticizer: 5:1 ~ 2 take epoxidized soybean oil, triethyl citrate mixing to get plasticizer in mass ratio.
Defoaming agent: 4:1 ~ 2 take silicone emulsion in mass ratio, and dimethyl silicone polymer mixes to get defoaming agent.
Catalyst: stannous octoate, isooctyl acid lead, any one in dibutyl tin dilaurate.
Solvent A: 8:0.1 ~ 0.4 takes glacial acetic acid, toluene mixing to get solvent A in mass ratio.
Solvent B: 5:1 ~ 2 take dimethyl carbonate, acetone mixing to get solvent B in mass ratio.
Coupling agent: any one in silane resin acceptor kh-550, KH-560, KH-570.
PH adjusting agent: 1:4 ~ 8 NaH that takes citric acid, concentration 0.1mol/L in mass ratio2PO4Solution mixes to get pH tune
Save agent.
A kind of preparation method of water shutoff material, includes the following steps:
(1) 5:1 ~ 2:0.5 in mass ratio takes nanometer hydroxyapatite, deacetylation is 80% carboxymethyl chitosan, lac is in ball
Grinding jar mixing is added zirconium oxide ball milling pearl by 20 ~ 30:1 of ratio of grinding media to material and obtains ball milling material with 300 ~ 350r/min, 35 ~ 60min of ball milling,
It takes ball milling material 1:3 in mass ratio ~ 6 that solvent A mixing is added, after -25 DEG C of freezen protectives, making for 2 ~ 4 times of ball milling material quality is added
Hole agent, 40 ~ 60min of supersonic oscillations, obtains dispersion liquid, takes dispersion liquid that the lemon that 3 ~ 5 times of mass fractions of dispersion liquid quality are 15% is added
The mixing of lemon acid solution, stands 3 ~ 5h at room temperature, obtains feed liquid, spare；
(2) 3:1 ~ 2 take isocyanates, polyether polyol to mix in reaction kettle in mass ratio, are passed through with 60 ~ 80mL/min rate
Nitrogen protection, under 90 ~ 110 DEG C, 300 ~ 500r/min revolving speed, constant temperature is stirred to react 2 ~ 4h, is cooled to 70 ~ 80 DEG C, must react
Material takes reaction material that the plasticizer of reaction material quality 4 ~ 8% is added, and adjusting revolving speed is 500 ~ 700r/min, is stirred 1 ~ 3h, drops
The defoaming agent of reaction material quality 4 ~ 8%, the catalyst of reaction material quality 4 ~ 8%, 3 ~ 6 times of reaction material quality is added to 60 ~ 65 DEG C in temperature
Solvent B, adjusting revolving speed is 700 ~ 800r/min, is stirred 30 ~ 40min, and cooled to room temperature, discharging must be modified and gather
Urethane；
(3) 3:1:5 ~ 8 in mass ratio take polyethyleneimine, coupling agent, and modified polyurethane is mixed in batch mixer, with 1200 ~
Modified polyurethane is added after pH adjusting agent adjusting pH to 6.0 ~ 6.5 is added in 20 ~ 35min of high-speed stirred under the conditions of 1400r/min
The feed liquid of quality 15 ~ 25% is uniformly mixed, and stands 2 ~ 5h to get water shutoff material.
Embodiment 1
Pore creating material: 6:1 in mass ratio takes paracide, potassium chloride mixing to get pore creating material.
Plasticizer: 5:1 in mass ratio takes epoxidized soybean oil, triethyl citrate mixing to get plasticizer.
Defoaming agent: 4:1 in mass ratio takes silicone emulsion, and dimethyl silicone polymer mixes to get defoaming agent.
Catalyst: stannous octoate.
Solvent A: 8:0.1 in mass ratio takes glacial acetic acid, toluene mixing to get solvent A.
Solvent B: 5:1 in mass ratio takes dimethyl carbonate, acetone mixing to get solvent B.
Coupling agent: silane resin acceptor kh-550.
PH adjusting agent: 1:4 in mass ratio takes the NaH of citric acid, concentration 0.1mol/L2PO4Solution mixing is to get pH adjusting
Agent.
A kind of preparation method of water shutoff material, includes the following steps:
(1) 5:1:0.5 in mass ratio takes nanometer hydroxyapatite, deacetylation is 80% carboxymethyl chitosan, lac is in ball milling
Tank mixing is added zirconium oxide ball milling pearl by ratio of grinding media to material 20:1 and obtains ball milling material with 300r/min ball milling 35min, takes ball milling material by matter
Solvent A mixing is added than 1:3 in amount, and after -25 DEG C of freezen protectives, the pore creating material of 2 times of ball milling material quality, supersonic oscillations are added
40min obtains dispersion liquid, takes dispersion liquid that the citric acid solution that 3 times of mass fractions of dispersion liquid quality are 15% is added and mixes, at room temperature
3h is stood, feed liquid is obtained, it is spare；
(2) 3:1 in mass ratio takes isocyanates, polyether polyol to mix in reaction kettle, is passed through nitrogen with 60mL/min rate
Protection, under 90 DEG C, 300r/min revolving speed, constant temperature is stirred to react 2h, is cooled to 70 DEG C, obtains reaction material, takes reaction material to be added anti-
It should expect that the plasticizer of quality 4%, adjusting revolving speed are 500r/min, be stirred 1h, be cooled to 60 DEG C, reaction material quality 4% is added
Defoaming agent, the catalyst of reaction material quality 4%, 3 times of reaction material quality of solvent B, adjusting revolving speed is 700r/min, and stirring is mixed
30min, cooled to room temperature are closed, discharging obtains modified polyurethane；
(3) 3:1:5 in mass ratio takes polyethyleneimine, coupling agent, and modified polyurethane is mixed in batch mixer, with 1200r/min item
High-speed stirred 20min under part, after pH adjusting agent adjusting pH to 6.0 is added, the feed liquid mixing that modified polyurethane quality 15% is added is equal
It is even, 2h is stood to get water shutoff material.
Embodiment 2
Pore creating material: 6:2 in mass ratio takes paracide, potassium chloride mixing to get pore creating material.
Plasticizer: 5:2 in mass ratio takes epoxidized soybean oil, triethyl citrate mixing to get plasticizer.
Defoaming agent: 4:2 in mass ratio takes silicone emulsion, and dimethyl silicone polymer mixes to get defoaming agent.
Catalyst: isooctyl acid lead.
Solvent A: 8:0.4 in mass ratio takes glacial acetic acid, toluene mixing to get solvent A.
Solvent B: 5:2 in mass ratio takes dimethyl carbonate, acetone mixing to get solvent B.
Coupling agent: silane coupling agent KH-560.
PH adjusting agent: 1:8 in mass ratio takes the NaH of citric acid, concentration 0.1mol/L2PO4Solution mixing is to get pH adjusting
Agent.
A kind of preparation method of water shutoff material, includes the following steps:
(1) 5:2:0.5 in mass ratio takes nanometer hydroxyapatite, deacetylation is 80% carboxymethyl chitosan, lac is in ball milling
Tank mixing is added zirconium oxide ball milling pearl by ratio of grinding media to material 30:1 and obtains ball milling material with 350r/min ball milling 60min, takes ball milling material by matter
Solvent A mixing is added than 1:6 in amount, and after -25 DEG C of freezen protectives, the pore creating material of 4 times of ball milling material quality, supersonic oscillations are added
60min obtains dispersion liquid, takes dispersion liquid that the citric acid solution that 5 times of mass fractions of dispersion liquid quality are 15% is added and mixes, at room temperature
5h is stood, feed liquid is obtained, it is spare；
(2) 3:2 in mass ratio takes isocyanates, polyether polyol to mix in reaction kettle, is passed through nitrogen with 80mL/min rate
Protection, under 110 DEG C, 500r/min revolving speed, constant temperature is stirred to react 4h, is cooled to 80 DEG C, obtains reaction material, takes reaction material to be added anti-
It should expect that the plasticizer of quality 8%, adjusting revolving speed are 700r/min, be stirred 3h, be cooled to 65 DEG C, reaction material quality 8% is added
Defoaming agent, the catalyst of reaction material quality 8%, 6 times of reaction material quality of solvent B, adjusting revolving speed is 800r/min, and stirring is mixed
40min, cooled to room temperature are closed, discharging obtains modified polyurethane；
(3) 3:1:8 in mass ratio takes polyethyleneimine, coupling agent, and modified polyurethane is mixed in batch mixer, with 1400r/min item
High-speed stirred 35min under part, after pH adjusting agent adjusting pH to 6.5 is added, the feed liquid mixing that modified polyurethane quality 25% is added is equal
It is even, 5h is stood to get water shutoff material.
Embodiment 3
Pore creating material: 6:1 in mass ratio takes paracide, potassium chloride mixing to get pore creating material.
Plasticizer: 5:2 in mass ratio takes epoxidized soybean oil, triethyl citrate mixing to get plasticizer.
Defoaming agent: 4:1 in mass ratio takes silicone emulsion, and dimethyl silicone polymer mixes to get defoaming agent.
Catalyst: dibutyl tin dilaurate.
Solvent A: 8:0.3 in mass ratio takes glacial acetic acid, toluene mixing to get solvent A.
Solvent B: 5:1 in mass ratio takes dimethyl carbonate, acetone mixing to get solvent B.
Coupling agent: Silane coupling reagent KH-570.
PH adjusting agent: 1:6 in mass ratio takes the NaH of citric acid, concentration 0.1mol/L2PO4Solution mixing is to get pH adjusting
Agent.
A kind of preparation method of water shutoff material, includes the following steps:
(1) 5:1:0.5 in mass ratio takes nanometer hydroxyapatite, deacetylation is 80% carboxymethyl chitosan, lac is in ball milling
Tank mixing is added zirconium oxide ball milling pearl by ratio of grinding media to material 25:1 and obtains ball milling material with 325r/min ball milling 47min, takes ball milling material by matter
Solvent A mixing is added than 1:5 in amount, and after -25 DEG C of freezen protectives, the pore creating material of 3 times of ball milling material quality, supersonic oscillations are added
50min obtains dispersion liquid, takes dispersion liquid that the citric acid solution that 4 times of mass fractions of dispersion liquid quality are 15% is added and mixes, at room temperature
4h is stood, feed liquid is obtained, it is spare；
(2) 3:1 in mass ratio takes isocyanates, polyether polyol to mix in reaction kettle, is passed through nitrogen with 70mL/min rate
Protection, under 100 DEG C, 400r/min revolving speed, constant temperature is stirred to react 3h, is cooled to 75 DEG C, obtains reaction material, takes reaction material to be added anti-
It should expect that the plasticizer of quality 6%, adjusting revolving speed are 600r/min, be stirred 2h, be cooled to 63 DEG C, reaction material quality 6% is added
Defoaming agent, the catalyst of reaction material quality 6%, 5 times of reaction material quality of solvent B, adjusting revolving speed is 750r/min, and stirring is mixed
35min, cooled to room temperature are closed, discharging obtains modified polyurethane；
(3) 3:1:6 in mass ratio takes polyethyleneimine, coupling agent, and modified polyurethane is mixed in batch mixer, with 1300r/min item
High-speed stirred 27min under part, after pH adjusting agent adjusting pH to 6.3 is added, the feed liquid mixing that modified polyurethane quality 20% is added is equal
It is even, 3h is stood to get water shutoff material.
Comparative example: the water shutoff material of company of Nanning City production.
Sealing ratiod measurement: carrying out the measurement of sealing ratiod in accordance with the following steps: taking fill out sand tube, is put into 60 DEG C of insulating box and adds
Heat 2 hours surveys its permeability (permeability before injecting) with the common measurement method in this field；Then by the present invention and comparison
The water shutoff material of example was according to 0.45ml/ minutes/cm2Rate injected (every cm therein2It is the section relative to fill out sand tube
For product, similarly hereinafter), injection pressure 0.1MPa after injecting 0.3PV, stops injection, then measures permeability again (after injection
Permeability), so that its sealing ratiod can be calculated according to the permeability of front and back twice, (sealing ratiod %=(injects preceding permeability-note
Enter rear permeability)/inject preceding permeability × 100%).Abrasion resistance measurement: taking fill out sand tube, is put into 60 DEG C of insulating box and adds
Heat 2 hours surveys its permeability (permeability before injecting) with the common measurement method in this field；Then by the present invention and comparison
The water shutoff material of example was according to 0.45ml/ minutes/cm2Rate injected, injection pressure 0.1MPa, inject 0.3PV after, so
It waits and coagulates 30 hours afterwards, finally carry out displacement with deionized water, the deionized water volume by fill out sand tube is 40PV fill out sand tube hole
Then volume calculates the final sealing ratiod after washing away.Specific test result is shown in Table 1.
Table 1:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Sealing ratiod % | 98.6 | 98.4 | 98.2 | 86.1~87.2 |
| Wash away rear sealing ratiod % | 96.4 | 96.6 | 95.9 | 76.5~77.3 |
| Fill out sand tube corrosion condition after three months | It is corrosion-free | It is corrosion-free | It is corrosion-free | Slight erosion |
In summary, water shutoff material water plugging effect of the invention is more preferable, and resistance to erosion is not easily to fall off, is worth being widely used.
Claims (10)
1. a kind of preparation method of water shutoff material, which is characterized in that the preparation method includes the following steps:
(1) 5:1 ~ 2 in mass ratio；0.5 takes nanometer hydroxyapatite, carboxymethyl chitosan, lac mixing, by ratio of grinding media to material 20 ~ 30:
1 is added zirconium oxide ball milling pearl, and ball milling obtains ball milling material, takes ball milling material 1:3 in mass ratio ~ 6 that solvent A mixing is added, refrigerates, is added
The pore creating material of 2 ~ 4 times of ball milling material quality, supersonic oscillations obtain dispersion liquid, take dispersion liquid that 3 ~ 5 times of dispersion liquid quality of lemon is added
Acid solution mixing, stands, obtains feed liquid, spare；
(2) 3:1 ~ 2 take isocyanates, polyether polyol mixing in mass ratio, lead to nitrogen protection, and constant temperature stirring is cooled to 70 ~ 80
DEG C, reaction material is obtained, takes reaction material that the plasticizer of reaction material quality 4 ~ 8% is added, adjusting revolving speed is to be stirred, it is cooled to 60 ~
65 DEG C, be added the defoaming agent of reaction material quality 4 ~ 8%, the catalyst of reaction material quality 4 ~ 8%, 3 ~ 6 times of reaction material quality solvent
B adjusts revolving speed, is stirred, cooling, and discharging obtains modified polyurethane；
(3) 3:1:5 ~ 8 take polyethyleneimine, coupling agent in mass ratio, and modified polyurethane is mixed in batch mixer, and high-speed stirred is adjusted
PH is saved, the feed liquid that modified polyurethane quality 15 ~ 25% is added is uniformly mixed, and stands 2 ~ 5h to get water shutoff material.
2. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the pore-creating in the step (1)
Agent: 6:1 ~ 2 take paracide, potassium chloride mixing to get pore creating material in mass ratio.
3. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the solvent in the step (1)
A: 8:0.1 ~ 0.4 takes glacial acetic acid, toluene mixing to get solvent A in mass ratio.
4. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the plasticising in the step (2)
Agent: 5:1 ~ 2 take epoxidized soybean oil, triethyl citrate mixing to get plasticizer in mass ratio.
5. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the defoaming in the step (2)
Agent: 4:1 ~ 2 take silicone emulsion in mass ratio, and dimethyl silicone polymer mixes to get defoaming agent.
6. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the catalysis in the step (2)
Agent: stannous octoate, isooctyl acid lead, any one in dibutyl tin dilaurate.
7. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the solvent in the step (2)
B: 5:1 ~ 2 take dimethyl carbonate, acetone mixing to get solvent B in mass ratio.
8. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the high speed in the step (3)
Stirring is to stir 20 ~ 35min with 1200 ~ 1400r/min.
9. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that the coupling in the step (3)
Agent: any one in silane resin acceptor kh-550, KH-560, KH-570.
10. a kind of preparation method of water shutoff material according to claim 1, which is characterized in that adjust pH in the step (3)
PH adjusting agent used: 1:4 ~ 8 take citric acid, NaH in mass ratio2PO4Solution mixes to get pH adjusting agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109777383A (en) * | 2019-03-18 | 2019-05-21 | 四川捷贝通能源科技有限公司 | A kind of multicore microballoon selective water shutoff agent and preparation method thereof |
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Application publication date: 20190118 |