CN107057016B - Mining water shutoff material and preparation facilities - Google Patents
Mining water shutoff material and preparation facilities Download PDFInfo
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- CN107057016B CN107057016B CN201710227421.1A CN201710227421A CN107057016B CN 107057016 B CN107057016 B CN 107057016B CN 201710227421 A CN201710227421 A CN 201710227421A CN 107057016 B CN107057016 B CN 107057016B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5075—Polyethers having heteroatoms other than oxygen having phosphorus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/758—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing two or more cycloaliphatic rings
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The present invention relates to polymeric material fields.Purpose is to provide the mining water shutoff material and preparation facilities of a kind of safety and environmental protection, excellent fireproof performance.The technical solution adopted is that: mining water shutoff material includes two kinds of components of A, B, and the component A is made of 48~52 parts of flame retardant polyether polyol, 36~43 parts of flame retardant polyester polyalcohol, 45~55 parts of isocyanates, 5~8 parts of nanometer calcium carbonate and 2~3 parts of silicone oil by weight；The B component is made of 25~35 parts of polyether polyol, 0.5~0.8 part of catalyst, 8~12 parts of propylene carbonate, 3~4 parts of antimony oxide, 2~3 parts of magnesium hydroxide and 1~2 part of Diethylaminoethanol by weight.Safety and environmental protection of the present invention has excellent flame retardant property and curing performance, is conducive to construction safety and protects the health of construction personnel.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to mining water shutoff material and preparation facilities.
Background technique
Currently, often there is leakage phenomenon when the Underground Engineering Excavations such as mine working, vertical shaft, tunnel, seabed tunnel, subway,
In the underground engineering especially constructed in rock, a large amount of underground water being encountered sometimes and is gushed out, underground water passes through rock fracture pair
Underground engineering can cause serious harm, need using polyurethane water shutoff material control water burst or impervious leakage-stopping.The dam body dam foundation
Antiseepage, the infiltration of foundation pit periphery and substrate Sand can also be handled using polyurethane slip casting method.
Polyurethane chemistry water shutoff material is new anti-of one kind for developing after acrylamide and epoxy resin plasmoid material
Leak stopping cementing material is seeped, polyurethane grouting material activity is big, and impervious leakage-stopping ability is strong, and it can construct with water, different requirements can be met,
It is that use scope is wide, a kind of performance water shutoff material well.Polyurethane water shutoff material meet water after can immediately with water occur chain extension,
Branching and cross-linking reaction cause volume expansion and ultimately generate a kind of not soluble in water, have the nontoxic gel of some strength solid
Knot body.Polyurethane water shutoff material can realize the fast of inbreak hole by its dilatancy, permeability and the excellent feature of leakproofness
Speed filling, prevents the further deterioration of inbreak；The rapid leak stopping of dynamic water can be achieved, the filling with thin crack prevents permeable thing
Therefore generation.
In the prior art, common polyurethane water shutoff material is frequently with toluene di-isocyanate(TDI) ingredient, vapour pressure compared with
Height, volatilization toxicity is big, can stimulate eyes, skin and respiratory system, be potentially carcinogenic, and the body for having seriously affected construction personnel is strong
Health.Meanwhile containing a large amount of organic solvent in existing polyurethane water shutoff material, such as acetone, dimethylbenzene, toluene, butanone, acetic acid second
Ester, butyl acetate etc., not only environmental pollution is serious in use for these solvents, unfavorable to the health of construction personnel, and
Serious to threatening in coal mine downhole safety production, solvent evaporates into air, Yi Fasheng combustion explosion accident.Although common is poly-
Urethane material can generate carbon dioxide in solidification, have certain anti-flammability, but flame retardant effect is far from enough, if generating increasing
Add the amount of carbon dioxide that the slurry material induration after foaming can be made to lose original mechanical strength, easily leads to slip casting failure.Therefore, such as
Viscosity, curing performance, the feature of environmental protection and the safety what coordinates polyurethane water shutoff material are that domestic pharmaceutical industry was stifled to polyurethane in recent years
Water investigation of materials emphasis.
In addition, the preparation facilities of polyurethane water shutoff material is the reaction kettle for having stirring, heating function, reacting material
Reaction and polymerization are sufficiently mixed in kettle.But the material viscosity of synthesis of polyurethane material is larger, and existing preparation facilities will stir mostly
It mixes leaf to be arranged in reactor bottom, it is difficult to reach ideal mixing effect, and heating device is distributed in the periphery of reaction kettle more, stirs
It mixes effect also and will affect the consistency of temperature of charge, be easy to cause that external temperature of charge is excessively high and center temperature of charge is lower existing
As.Meanwhile the preparation of polyurethane water shutoff material also there are certain requirements the gaseous environment of reaction, and preparation facilities is needed to be equipped with replacement
React the structure of gas reactor.
Summary of the invention
The object of the present invention is to provide a kind of safety and environmental protections, the mining water shutoff material and preparation facilities of excellent fireproof performance.
For achieving the above object, the technical scheme adopted by the invention is that: mining water shutoff material and preparation facilities, institute
Stating mining water shutoff material includes two kinds of components of A, B, and the component A is by weight by 48~52 parts of flame retardant polyether polyol, fire-retardant
36~43 parts of polyester polyol, 45~55 parts of isocyanates, 5~8 parts of nanometer calcium carbonate and 2~3 parts of silicone oil compositions；The B group
Point by weight by 25~35 parts of polyether polyol, 0.5~0.8 part of catalyst, 8~12 parts of propylene carbonate, antimony oxide 3~
4 parts, 2~3 parts of magnesium hydroxide and 1~2 part of Diethylaminoethanol composition.
The flame retardant polyether polyol is phosphorous polyether polyol, and the mass fraction of phosphorus is in the phosphorous polyether polyol
10%~12%, hydroxyl value is 150~230mgKOH/g；The hydroxyl value of the flame retardant polyester polyalcohol is 200~395 mgKOH/g, is glued
Degree is 2000~4000mPas/25 DEG C；The isocyanates uses 4,4 '-dicyclohexyl methyl hydride diisocyanates or different Fo Er
One or both of ketone diisocyanate is mixed with arbitrary proportion；The degree of functionality of the polyether polyol is 3, viscosity 180
~380 mPas/25 DEG C.
Preferred: the flame retardant polyester polyalcohol is one or both of PF-3805 or PF-2011 mixed with arbitrary proportion
It closes.
Preferred: the flame retardant polyester polyalcohol is that PF-3805 and PF-2011 is mixed in the ratio of 3:2.
Preferred: the partial size of the nano-calcium carbonate sodium is 65~75nm.
Preferred: the catalyst is one of dibutyl tin dilaurate, stannous octoate, triethylene diamine or two
Kind is mixed with arbitrary proportion.
Preferred: the catalyst is that dibutyl tin dilaurate and triethylene diamine are mixed in the ratio of 5:2.
Preferred: the polyether polyol is that one or both of NJ-305, NJ-310 are mixed with arbitrary proportion.
Preferred: the mining water shutoff material is prepared according to the following steps:
Flame retardant polyether polyol and flame retardant polyester polyalcohol are added in preparation facilities, vacuum under the conditions of 102~112 DEG C
It is dehydrated 2~3h, then stops heating and nanometer calcium carbonate being added stirring 20~30min under nitrogen protection；It is cooled to temperature
45~55 DEG C, isocyanates is added into preparation facilities, reaction temperature is controlled at 75~85 DEG C, maintains nitrogen protection stirring 150
~200min；It adds silicone oil to stir evenly, obtains component A.
Polyether polyol, catalyst, propylene carbonate, antimony oxide, magnesium hydroxide, Diethylaminoethanol are thrown in proportion
Enter in preparation facilities, stir evenly at room temperature, obtains component B.
In use, component A and B component are mixed slip casting in the ratio of 1:0.8~1.2.
Preferred: for the preparation facilities that the mining water shutoff material uses for reaction kettle, the reaction kettle includes body, described
Rabbling mechanism is set in body, and the rabbling mechanism is by being arranged in the motor driven at the top of body；The top of the body is equipped with
Feed pipe, bottom are equipped with discharge nozzle, middle part is equipped with vacuum pumping opening, and the feed pipe and discharge nozzle are equipped with control valve, institute
It states and heating tube is set on organism sidewall；Be fixed with material disc below the feed pipe, the material disc by organism sidewall obliquely
It is tilted towards body center；The vacuum pumping opening is arranged above highest liquid level；The rabbling mechanism include agitating shaft, cross bar and
Paddle, the cross bar are fixed on agitating shaft and perpendicular with agitating shaft, and the paddle is two, described two paddles
Symmetrically it is fixed on the end face of cross bar with reverse acting spiral shape；Stabilizer blade is arranged in organism bottom.
Preferred: the position of the inner sidewall face vacuum pumping opening of the body is equipped with baffle.
The invention has the following advantages: safety and environmental protection, has excellent flame retardant property and curing performance, is conducive to apply
The health of work safety and protection construction personnel.Specifically, the present invention is more using flame retardant polyether polyol and flame retardant polyester
First alcohol substantially increases the flame retardant property of product as raw material, avoids and occurs combustion explosion thing in underground construction operation process
Therefore situation.Polyurethane material is modified using nanometer calcium carbonate in component A, improves the pressure after polyurethane material solidifies
Contracting intensity, the foam structure formed after also solidifying polyurethane material is complete, size is smaller, is evenly distributed.And it be not added with
In the case where solvent, product viscosity is small, and concrete castability is strong, and safety and environmental protection is easy for construction.The preparation facilities of water shutoff material of the present invention
Structure is simple, and stirring and mixing effect is good under the action of material disc and helical form paddle, and has and vacuumize air-exchanging structure, energy
Enough meet the reaction condition of mining water shutoff material preparation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of preparation facilities of the present invention.
Specific embodiment
Rabbling mechanism is arranged in the body 1 in the preparation facilities of mining water shutoff material as shown in Figure 1, including body 1,
The rabbling mechanism is driven by the motor 2 that 1 top of body is arranged in, and is connected between the motor 2 and rabbling mechanism for axial seal
It connects, may insure the sealing performance in body 1 in this way, be conducive to control the gaseous environment in body 1.The top of the body 1
Discharge nozzle 4 is equipped with equipped with feed pipe 3, bottom, middle part is equipped with vacuum pumping opening 5, the feed pipe 3 and discharge nozzle 4 equipped with control
Heating tube 6 is arranged on 1 side wall of body for valve processed.Be fixed with material disc 7 below the feed pipe 3, the material disc 7 by
1 side wall of body is tilted towards 1 center of body obliquely, can play the role of dispersed material in this way, avoid material in 1 bottom of body
Side accumulation, be conducive to material and reach better stirring and mixing effect, make the temperature of material and mixing it is with higher consistent
Property.The vacuum pumping opening 5 is arranged above highest liquid level, i.e., vacuum pumping opening 5 is located at the 1 higher position in middle part of body, such as
Shown in Fig. 1, vacuum pumping opening 5 is located at the middle and upper part on 1 right side of body, is connected to inside the side wall and body 1 of body 1.Into one
Step, material is splashed into vacuum pumping opening 5 in order to prevent, blocks pump-line, the inner sidewall face vacuum pumping opening of the body 1
5 position is equipped with baffle 11, and baffle 11 can prevent material from entering in vacuum pumping opening 5.
In order to enhance mixing effect, the rabbling mechanism includes agitating shaft 8, cross bar 9 and paddle 10, and the cross bar 9 is solid
Be scheduled on it is on agitating shaft 8 and perpendicular with agitating shaft 8, the quantity of cross bar 9 can be set it is multiple, at least three, such paddle
10 could form helicoidal structure.The paddle 10 is two, and described two paddles 10 are symmetrically with reverse acting spiral shape
It is fixed on the end face of cross bar 9, end face here refers to the radial section of cross bar 9, as shown in Figure 1, the end face of cross bar 9 is left and right
The radial section at both ends.Stabilizer blade 12 is arranged in 1 bottom of body, and stabilizer blade 12 plays a supportive role to body 1.
Flame retardant polyether polyol and flame retardant polyester polyalcohol when in use, are first put in proportion by preparation facilities of the invention
In body 1, vacuum pumping opening 5 is connected to vacuum pump, and opens heating tube 6 and controls temperature at 102~112 DEG C, carries out vacuum
Dehydration.Heating tube 6 is closed after dehydration, nanometer calcium carbonate is added into body, and vacuum pumping opening 5 is connected to nitrogen gas tank,
It is passed through nitrogen protection into body 1, opens motor 2 and rabbling mechanism is driven to be stirred.45~55 DEG C are down to temperature in body 1
Afterwards, isocyanates is added, the control of heating tube 6 temperature is opened and maintains 75~85 DEG C, maintain nitrogen protection to be stirred, after 3h
Addition silicone oil, which stirs evenly, can be obtained component A.Then raw material is put in proportion into body 1 when preparing B component, opens motor 2
Driving rabbling mechanism is stirred for uniformly.
Lower mask body provides preferred embodiment so that those skilled in the art more understand technical solution of the present invention and
Effect.
Embodiment one
The mining water shutoff material is prepared according to the following steps:
By ten thousand Hua Huaxue of 5kgFR-1830() and 380 mgKOH/g of 4kgPF-3805(hydroxyl value, 3500 mPas/25 of viscosity
DEG C) be added in reaction kettle.Vacuum pumping opening 5 is connected to vacuum pump and opens heating tube 6, vacuum is de- under the conditions of 102~112 DEG C
Water 2.5h is then shut off vacuum pump and heating tube 6 and the nanometer calcium carbonate that 0.6kg partial size is 70nm is added.By vacuum pumping opening 5
It is connect with nitrogen gas tank, stirs 25min under nitrogen protection.45~55 DEG C are cooled to temperature, the different Buddhist of 5kg is added into reaction kettle
That ketone diisocyanate is again turned on heating tube 6 and controls reaction temperature at 75~85 DEG C, maintains nitrogen protection stirring
180min；It adds 0.2kg silicone oil to stir evenly, obtains component A.
By 3kgNJ-305(degree of functionality 3, mPas/25 DEG C of viscosity 280), 0.05kg dibutyl tin dilaurate,
0.02kg triethylene diamine, 1kg propylene carbonate, 0.3kg antimony oxide, 0.2kg magnesium hydroxide, 0.1kg Diethylaminoethanol
It puts into reaction kettle, stirs evenly at room temperature, obtain B component.
Component A and B component packing are saved, in use, component A and B component mix slip casting in the ratio of 1:1.
Embodiment two
The mining water shutoff material is prepared according to the following steps:
By ten thousand Hua Huaxue of 4.8kg FR-2026() and 4kg PF-2011(hydroxyl value 220 mgKOH/g, 2000 mPa of viscosity
S/25 DEG C) it is added in reaction kettle.Vacuum pumping opening 5 is connected to vacuum pump and opens heating tube 6, it is true under the conditions of 102~112 DEG C
Sky dehydration 2h is then shut off vacuum pump and heating tube 6 and the nanometer calcium carbonate that 0.5kg partial size is 70nm is added.By vacuum suction
Mouth 5 is connect with nitrogen gas tank, stirs 20min under nitrogen protection.45~55 DEG C are cooled to temperature, is added into reaction kettle
4.5kg4,4 '-dicyclohexyl methyl hydride diisocyanates are again turned on heating tube 6 and control reaction temperature at 75~85 DEG C, maintain
Nitrogen protection stirs 150min；It adds 0.2kg silicone oil to stir evenly, obtains component A.
By 2.5kg NJ-310(degree of functionality 3, mPas/25 DEG C of viscosity 240), 0.04kg dibutyl tin dilaurate,
0.01kg stannous octoate, 0.8kg propylene carbonate, 0.3kg antimony oxide, 0.2kg magnesium hydroxide, 0.1kg Diethylaminoethanol
It puts into reaction kettle, stirs evenly at room temperature, obtain B component.
Component A and B component packing are saved, in use, component A and B component mix slip casting in the ratio of 1:0.8.
Embodiment three
The mining water shutoff material is prepared according to the following steps:
By ten thousand Hua Huaxue of 5.2kg FR-2026(), 380 mgKOH/g of 1.8kgPF-3805(hydroxyl value, 3500 mPa of viscosity
S/25 DEG C) and 220 mgKOH/g of 2kg PF-2011(hydroxyl value, mPas/25 DEG C of viscosity 2000) it is added in reaction kettle.By vacuum
Bleeding point 5 is connected to vacuum pump and simultaneously opens heating tube 6, vacuum dehydration 3h under the conditions of 102~112 DEG C, be then shut off vacuum pump and
Simultaneously the nanometer calcium carbonate that 0.8kg partial size is 70nm is added in heating tube 6.Vacuum pumping opening 5 is connect with nitrogen gas tank, in nitrogen protection
Lower stirring 30min.45~55 DEG C are cooled to temperature, 5.5kg4,4 '-dicyclohexyl methyl hydride diisocyanates are added into reaction kettle
Ester is again turned on heating tube 6 and controls reaction temperature at 75~85 DEG C, nitrogen protection is maintained to stir 200min；Add 0.3kg
Silicone oil stirs evenly, and obtains component A.
By 3.5kg NJ-310(degree of functionality 3, mPas/25 DEG C of viscosity 240), 0.05kg dibutyl tin dilaurate,
0.03kg stannous octoate, 1.2kg propylene carbonate, 0.4kg antimony oxide, 0.3kg magnesium hydroxide, 0.2kg Diethylaminoethanol
It puts into reaction kettle, stirs evenly at room temperature, obtain B component.
Component A and B component packing are saved, in use, component A and B component mix slip casting in the ratio of 1:1.2.
Example IV
The mining water shutoff material is prepared according to the following steps:
By ten thousand Hua Huaxue of 5kg FR-1830(), 380 mgKOH/g of 2.4kgPF-3805(hydroxyl value, 3500 mPas/ of viscosity
25 DEG C) and 220 mgKOH/g of 1.6kg PF-2011(hydroxyl value, mPas/25 DEG C of viscosity 2000) it is added in reaction kettle.By vacuum
Bleeding point 5 is connected to vacuum pump and opens heating tube 6, and vacuum dehydration 2.5h under the conditions of 102~112 DEG C is then shut off vacuum pump
With heating tube 6 and be added 0.7kg partial size be 70nm nanometer calcium carbonate.Vacuum pumping opening 5 is connect with nitrogen gas tank, is protected in nitrogen
Shield is lower to stir 25min.45~55 DEG C are cooled to temperature, 5kg isophorone diisocyanate is added into reaction kettle, beats again
The control of 6 reaction temperature of heating tube is opened at 75~85 DEG C, nitrogen protection is maintained to stir 180min；It is equal to add the stirring of 0.2kg silicone oil
It is even, obtain component A.
By 1.5kg NJ-310(degree of functionality 3, mPas/25 DEG C of viscosity 240), 1.8kgNJ-305(degree of functionality 3, viscosity
280 mPas/25 DEG C), 0.05kg dibutyl tin dilaurate, 0.02kg triethylene diamine, 1kg propylene carbonate,
0.3kg antimony oxide, 0.2kg magnesium hydroxide, 0.2kg Diethylaminoethanol are put into reaction kettle, are stirred evenly at room temperature, are obtained B
Component；Component A and B component packing are saved, in use, component A and B component mix slip casting in the ratio of 1:1.
Embodiment five
The mining water shutoff material is prepared according to the following steps:
By ten thousand Hua Huaxue of 5kg FR-2026(), 380 mgKOH/g of 2kgPF-3805(hydroxyl value, 3500 mPas/25 of viscosity
DEG C) and 220 mgKOH/g of 2.2kg PF-2011(hydroxyl value, mPas/25 DEG C of viscosity 2000) it is added in reaction kettle.Vacuum is taken out
Port 5 is connected to vacuum pump and simultaneously opens heating tube 6, vacuum dehydration 2.5h under the conditions of 102~112 DEG C, be then shut off vacuum pump and
Simultaneously the nanometer calcium carbonate that 0.8kg partial size is 70nm is added in heating tube 6.Vacuum pumping opening 5 is connect with nitrogen gas tank, in nitrogen protection
Lower stirring 30min.45~55 DEG C are cooled to temperature, 5kg4,4 '-dicyclohexyl methyl hydride diisocyanates are added into reaction kettle
Ester is again turned on heating tube 6 and controls reaction temperature at 75~85 DEG C, nitrogen protection is maintained to stir 200min；Add 0.3kg
Silicone oil stirs evenly, and obtains component A.
By 2kg NJ-310(degree of functionality 3, mPas/25 DEG C of viscosity 240), 1.5kgNJ-305(degree of functionality 3, viscosity 280
MPas/25 DEG C), 0.05kg dibutyl tin dilaurate, 0.02kg stannous octoate, 1.2kg propylene carbonate, 0.4kg oxygen
Change antimony, 0.3kg magnesium hydroxide, 0.2kg Diethylaminoethanol to put into reaction kettle, stirs evenly at room temperature, obtain B component.
Component A and B component packing are saved, in use, component A and B component mix slip casting in the ratio of 1:0.8.
Product testing
The product that embodiment one to embodiment five (abbreviation example one to example five) is prepared carries out performance detection, in detection
Hold including density, viscosity, wrap aqueous, frothing percentage, curing time, compression strength and oxygen index (OI).Measuring method is as follows:
Density by GB/T8077-2000 5.3 regulation carry out, viscosity by 5.1 in GB/T2794-1995 provide into
Row.
Wrap aqueous: measurement sample mixed with the water of 10 times of quality, measure from start to mix be not discharged into container when
Time, water used meet GB/T6682-2008 requirement tertiary effluent.
Frothing percentage: A, B component are mixed in the ratio provided in embodiment, foam volume and original A, B after measurement solidification
The ratio of volume components.
Curing time: in the ratio provided in embodiment by A, B component mix start timing, no longer rise to foams and
Hand touches foams without viscous hand phenomenon, stops timing.
Compression strength: in the ratio provided in embodiment by A, B component it is mixing cured after, place 168h, by GB/T1041-
1992 carry out intensity test.
Oxygen index value: it is carried out by the regulation of GB/T8624-2012.It is as shown in the table to obtain testing result:
Table an example one arrives the performance parameter of five product of example
Oxygen index (OI) in upper table is minimum concentration needed for material carries out flaming combustion in nitrogen oxygen atmosphere stream, oxygen index (OI)
Height indicates that material is nonflammable.For water shutoff material oxygen index value of the invention 27% or more, the product of example three to example five is even super
30% has been crossed, fire retardant product is belonged to, has had superior flame retardant property.Meanwhile the more existing skill of compressive strength of water shutoff material of the present invention
Art is greatly improved, this illustrates that solidified body structural strength of the invention is big, and the foam structure being formed by curing is stablized.In addition, this
Invention product has low viscosity, the aqueous and high foaming rate of high packet, and comprehensive performance is good, and mining need are more adapted to compared with the prior art
It wants, the safety accident of underground construction can be reduced.
Claims (10)
1. a kind of mining water shutoff material, it is characterised in that: the mining water shutoff material includes two kinds of components of A, B, and the component A is pressed
Poidometer is by 48~52 parts of flame retardant polyether polyol, 36~43 parts of flame retardant polyester polyalcohol, 45~55 parts of isocyanates, nano-sized carbon
5~8 parts and 2~3 parts of silicone oil compositions of sour calcium；The B component by weight by 25~35 parts of polyether polyol, catalyst 0.5~
0.8 part, 8~12 parts of propylene carbonate, 1~2 part of 3~4 parts of antimony oxide, 2~3 parts of magnesium hydroxide and Diethylaminoethanol group
At；
The flame retardant polyether polyol is phosphorous polyether polyol, and the mass fraction of phosphorus is 10% in the phosphorous polyether polyol
~12%, hydroxyl value is 150~230mgKOH/g；The hydroxyl value of the flame retardant polyester polyalcohol is 200~395mgKOH/g, and viscosity is
2000~4000mPas/25 DEG C；The isocyanates uses 4,4 '-dicyclohexyl methyl hydride diisocyanates or isophorone two
One or both of isocyanates is mixed with arbitrary proportion；The degree of functionality of the polyether polyol be 3, viscosity be 180~
380mPa·s/25℃。
2. mining water shutoff material according to claim 1, it is characterised in that: the flame retardant polyester polyalcohol is PF-3805
Or one or both of PF-2011 is mixed with arbitrary proportion.
3. mining water shutoff material according to claim 1, it is characterised in that: the flame retardant polyester polyalcohol is PF-
3805 are mixed with PF-2011 in the ratio of 3:2.
4. mining water shutoff material according to claim 1, it is characterised in that: the partial size of the nanometer calcium carbonate be 65~
75nm。
5. mining water shutoff material according to claim 1, it is characterised in that: the catalyst is di lauric dibutyl
One or both of tin, stannous octoate, triethylene diamine are mixed with arbitrary proportion.
6. mining water shutoff material according to claim 1, it is characterised in that: the catalyst is di lauric dibutyl
Tin and triethylene diamine are mixed in the ratio of 5:2.
7. mining water shutoff material according to claim 1, it is characterised in that: the polyether polyol is NJ-305, NJ-
One or both of 310 are mixed with arbitrary proportion.
8. according to claim 1 to mining water shutoff material described in any one of 7, it is characterised in that: the mining water blockoff
Material is prepared according to the following steps:
Flame retardant polyether polyol and flame retardant polyester polyalcohol are added in preparation facilities, vacuum dehydration under the conditions of 102~112 DEG C
Then 2~3h stops heating and nanometer calcium carbonate being added stirring 20~30min under nitrogen protection；45 are cooled to temperature~
55 DEG C, isocyanates is added into preparation facilities, reaction temperature is controlled at 75~85 DEG C, maintenance nitrogen protection stirring 150~
200min；It adds silicone oil to stir evenly, obtains component A；
Polyether polyol, catalyst, propylene carbonate, antimony oxide, magnesium hydroxide, Diethylaminoethanol are put in proportion into system
In standby device, stirs evenly at room temperature, obtain component B；
In use, component A and B component are mixed slip casting in the ratio of 1:0.8~1.2.
9. mining water shutoff material according to claim 8, it is characterised in that: the preparation dress that the mining water shutoff material uses
It is set to reaction kettle, the reaction kettle includes body (1), rabbling mechanism is arranged in the body (1), the rabbling mechanism is by being arranged
Motor (2) driving at the top of body (1)；The top of the body (1) be equipped with feed pipe (3), bottom be equipped with discharge nozzle (4),
Middle part is equipped with vacuum pumping opening (5), and the feed pipe (3) and discharge nozzle (4) are equipped with control valve, body (1) side wall
Upper setting heating tube (6)；It is fixed with material disc (7) below the feed pipe (3), the material disc (7) is oblique by body (1) side wall
It tilts down to body (1) center；The vacuum pumping opening (5) is arranged above highest liquid level；The rabbling mechanism includes stirring
Mix axis (8), cross bar (9) and paddle (10), the cross bar (9) be fixed on it is on agitating shaft (8) and perpendicular with agitating shaft (8),
The paddle (10) is two, and described two paddles (10) are fixed on the end of cross bar (9) symmetrically with reverse acting spiral shape
On face；Stabilizer blade (12) are arranged in body (1) bottom.
10. mining water shutoff material according to claim 9, it is characterised in that: the inner sidewall face vacuum of the body (1)
The position of bleeding point (5) is equipped with baffle (11).
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| CN110627990A (en) * | 2019-09-25 | 2019-12-31 | 九江智达环能科技有限公司 | Degradable liquid cross-linked plugging material and preparation method and application thereof |
| CN111286003A (en) * | 2020-04-03 | 2020-06-16 | 扬州晨化新材料股份有限公司 | Preparation method of mining high-strength flame-retardant polyurethane reinforcing material |
| CN113278123B (en) * | 2021-05-19 | 2022-08-19 | 核工业华南花都建设工程公司 | Polyurethane grouting material for foundation pit water stop and preparation method thereof |
| CN113789113B (en) * | 2021-08-25 | 2022-04-15 | 河北化工医药职业技术学院 | Waterproof coating with flame-retardant and fireproof performances |
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| CN85103075A (en) * | 1985-04-22 | 1987-01-28 | 煤炭工业部煤炭科学研究院北京开采研究所 | Reinforcing, water blockoff polyurethane material |
| DE19647982A1 (en) * | 1996-11-21 | 1998-05-28 | Basf Ag | Dispersions containing polyurethanes with carbonyl groups in a keto function |
| DE19741257A1 (en) * | 1997-09-19 | 1999-03-25 | Basf Ag | Process for the production of polyurethane foams |
| DE102006036220A1 (en) * | 2006-08-03 | 2008-02-07 | Clariant International Limited | Polyetheramine macromonomers with two adjacent hydroxyl groups and their use for the preparation of polyurethanes |
| CN102516493B (en) * | 2011-11-30 | 2013-09-11 | 上海东大化学有限公司 | Polyurethane strengthening water shutoff material special for mining and preparation method thereof |
| CN102702728A (en) * | 2012-01-05 | 2012-10-03 | 北京东方雨虹防水技术股份有限公司 | Polyurethane grouting water plugging-reinforcing material, and preparation method and application method thereof |
| CN103694676B (en) * | 2013-12-13 | 2016-08-17 | 山东一诺威新材料有限公司 | Environment-friendlypolyurethane polyurethane water shutoff material and preparation method thereof |
| CN104744667B (en) * | 2013-12-27 | 2017-10-13 | 上海东大化学有限公司 | Polyurethane water shutoff agent and preparation method thereof and application method |
| CN103724594B (en) * | 2013-12-31 | 2015-12-30 | 合肥工业大学 | A kind of environment-friendly water-based polyurethane grouting for water-blocking material and preparation method thereof |
| CN104045807B (en) * | 2014-06-30 | 2016-05-25 | 合肥工业大学 | A kind of environment-protecting polyurethane water reinforcement material and preparation method thereof |
| CN104498004A (en) * | 2014-11-27 | 2015-04-08 | 山东一诺威新材料有限公司 | Chemical grouting material for coal-rock mass water shutoff and reinforcement and preparation method thereof |
| CN104559138B (en) * | 2014-12-31 | 2017-07-25 | 江苏苏博特新材料股份有限公司 | A kind of hydrophilic two-component grouting leak-stopping material |
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