CN110408354A - A kind of preparation method of the saturating leakage-repairing glue of high waterproof, seepage control - Google Patents
A kind of preparation method of the saturating leakage-repairing glue of high waterproof, seepage control Download PDFInfo
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- CN110408354A CN110408354A CN201910539837.6A CN201910539837A CN110408354A CN 110408354 A CN110408354 A CN 110408354A CN 201910539837 A CN201910539837 A CN 201910539837A CN 110408354 A CN110408354 A CN 110408354A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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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Abstract
The invention discloses a kind of preparation methods of high saturating leakage-repairing glue of waterproof, seepage control, belong to leak repairing technical field of material.The present invention mixes bagasse and agricultural crop straw, the organic fiber wherein having, sugar ingredient are isolated using high temperature high pressure process and dipping by lye, and hydrolyze organic principle, the fracture of part carbochain, improves in leakage-repairing glue and bonds degree between each ingredient, inhibit the infiltration of moisture, improve the waterproof performance of leakage-repairing glue, also by aluminium ion introduced plant fiber, so that aluminium ion is adsorbed in organic fiber surface using ionic bond, Absorptive complex wave effect, further enhance waterproof performance;The present invention mixes calcium oxide with modified plant fiber, carbohydrate content and other organic compounds, it is scattered in calcium oxide molecule bonding in plant fiber, a large amount of thermal energy can be generated when meeting water reaction in calcium oxide, it can make plant fiber component, carbohydrate content charing, the compactness for further increasing leakage-repairing glue again improves the waterproof performance of leakage-repairing glue.
Description
Technical field
The invention discloses a kind of preparation methods of high saturating leakage-repairing glue of waterproof, seepage control, belong to leak repairing material preparation technology neck
Domain.
Background technique
House roof gap is a great problem that China handles house leakproof at present, and building leakage directly influences house
Using function, user security and service life, huge economic losses also are caused to enterprise.In building leakage governance process, seep
It is not a simple process that leakage, which generates, made of this thing gradually accumulates.It needs to carry out the supervision and management of construction, and needs
Special processing is carried out to the place for being likely to occur leakage in building, and carry out comprehensive waterproof work.Building is mended
Leak adhesive has had certain basic condition, and multifunctional house plugging material is a kind of new material developed in recent years, it
The problem of can solve wall and leakage of underground engineering water, has the characteristics that moisture-proof, impervious, leak stopping, bonding.
The house roof of Architecture Design Institute's design will generally increase the processing of two or three layers of waterproof cloth, but due to work progress
It is cumbersome, quality semi-coast will result in roof crack when construction, and the five of original building cost will be spent by handling roof leak
Times or so.In the prior art, processing roof leak is mainly using first prying open gap with awl, then with pitch glass cloth, waterproof
Cloth is poured with cement, and this method is difficult to solve the problems, such as clearance leakage;Also have and house roof or room are carried out using organic bond
Interior gap leak repairing, but sealing effect is poor, it is difficult to so that gap is kept sealing state for a long time.
There are many method of present house leak repairing, and the broken ceramic tile that has tears waterproof layer open, reform waterproof layer, the direct black top having
Etc., these are all some most traditional house leak repairing measures.Broken ceramic tile, reforms the heavy workload of waterproof layer, to building
Destructive big, economic consumption is high, and people also turns from side to side very much;Direct black top, effect is poor, excessively it is a for the moment, water ticktack have out
Begin, and pitch is very smelly when boiling, itself does not also have the performance of environmental protection.So there is an urgent need to a kind of waterproof effects
Environmentally friendly leak repairing material and method good, the duration is long, destructiveness is small.
With emerging in multitude for all kinds of building constructions, building roof, roof tank, floor and waterpipe jointing and municipal administration are net
It is more and more to build to water factory the gap for being possible to occur.It is expected that there are an all kinds of building amounts of thousands of seats in every city every year, and this
The expansion joint waterproof measure on the roof, clear water reserviors, treatment tank of engineerings is produced because of reasons such as construction, quality, material agings a bit
After life phenomena such as rupture etc. and breakage, directly affect using quality, rent situations such as leak is without sealing often occurs, gives
Engineering use and management causes damages, increase trouble.For this purpose, industry develops a kind of leakage-repairing glue, it is coated on gap
Plugging watertight is completed using the characteristic of leakage-repairing glue in place.Existing leakage-repairing glue is mainly the solid paste or artificialization of stationery class
Work high molecular material, leak repairing effect persistence is unsatisfactory, and preparation method is more complex.
And traditional house leakage-repairing glue the problem of can not being further increased there is also waterproofness difference and leak resistance, therefore,
How to improve conventional house leakage-repairing glue waterproofness difference and the shortcomings that leak resistance can not further increase, is provided in the hope of exploring to develop
The house leakage-repairing glue of good comprehensive performance is necessary to leak repairing technical field of material.
Summary of the invention
The technical problems to be solved by the invention: for the bad defect of current leakage-repairing glue waterproof performance, one kind is provided
The preparation method of the high saturating leakage-repairing glue of waterproof, seepage control.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of saturating leakage-repairing glue of high waterproof, seepage control the preparation method comprises the following steps:
By in reaction product, epoxy resin, lignin, polyetheramine, calcium carbonate investment heating furnace, heating in-furnace temperature is increased to
120~150 DEG C, constant temperature stands 40~50min, is stirred under this constant temperature with agitating device with the revolving speed of 500~550r/min
30~40min is mixed, 0~40 DEG C is cooled to after stirring and is discharged up to the impermeable leakage-repairing glue of high water resistance;
The preparation of reaction product are as follows:
(1) modified-reaction product is put into Rotary Evaporators, in revolving speed be 150~180r/min and temperature is 90~100 DEG C
Under conditions of rotary evaporation until enriched product is made in product quality constant weight, enriched product and calcium oxide are put into planetary ball mill
In, in ratio of grinding media to material be 10:1 and revolving speed is that grinding product is made in 150~180r/min ground and mixed, 30~40min;
(2) by grinding product and organosilan investment blender, in revolving speed be 400~500r/min and temperature is 160~180
40~50min is mixed under conditions of DEG C, is put into vacuum oven after mixing, in vacuum degree be 100~200MPa and temperature is
Reaction product is made in dry 5~6h under conditions of 60~80 DEG C;
The preparation of modified-reaction product are as follows:
(1) it will be crushed in bagasse and agricultural crop straw investment pulverizer, put into baking oven after crushing, be 65~75 DEG C in temperature
Under conditions of dry 2~3h obtain dried material, be in mass ratio in 1:5 investment reaction kettle by dried material and distilled water, will
Air pressure is increased to 1.2~1.6MPa in reaction kettle, increases reactor temperature to 130~150 DEG C, and constant temperature and pressure reaction 60~
Reacting slurry is made in 70min;
(2) by reacting slurry and SiO 2 powder investment beaker, 20 are stirred with the revolving speed of 260~300r/min with blender
Mixed serum is made in~30min, and the sodium hydroxide solution that mass fraction is 15~20% is added dropwise into beaker and adjusts pH value to 11
~12, it places the beaker in resistance heating set, jacket temperature is increased to 70~80 DEG C, with blender with 300~360r/
The revolving speed of min stirs 60~80 obtained solidliquid mixtures;
(3) by solidliquid mixture and aluminium chloride investment reaction kettle, reactor temperature is increased, with agitating device with 500~
The revolving speed of 600r/min stirs 60~80min and reacting slurry is made, and the hydrochloric acid that mass fraction is 5~7% is added dropwise into reacting slurry
Solution adjusts pH value to 6.0~6.5, is stirred to react 30~40min, filter residue, as modified-reaction product are obtained by filtration after stirring.
Preferably according to parts by weight, the reaction product is 9~12 parts, epoxy resin is 32~36 parts, lignin
For 1.2~1.6 parts, polyetheramine be 2~3 parts, calcium carbonate is 1.5~1.8 parts.
The mass ratio of enriched product described in the preparation of reaction product and calcium oxide is 15:1.
The mass ratio of grinding product described in the preparation of reaction product and organosilan is 6:1.
The mass ratio of bagasse described in the preparation of modified-reaction product and agricultural crop straw is 6:1.
Agricultural crop straw described in the preparation of modified-reaction product is more preferably corn stover, rice straw and small
Wheat Straw one or more of them mixes in any proportion.
The mass ratio of reacting slurry described in the preparation of modified-reaction product and SiO 2 powder is 15:1.
The mass ratio of solidliquid mixture described in the preparation of modified-reaction product and aluminium chloride is 15:1.
Reactor temperature described in the preparation of modified-reaction product is increased to 110~120 DEG C.
The method have the benefit that:
(1) bagasse, stalk are pulverized and mixed by the present invention first, dry after crushing to be made anti-with distilled water high-temperature high-voltage reaction again
Slurries are answered, then mix reacting slurry with silica, lye is added and obtained solidliquid mixture is mixed, then will consolidate
Liquid mixture and aluminium chloride high temperature hybrid reaction are added dropwise the reaction of salt acid for adjusting pH value, filter residue are obtained by filtration after reaction, as modified
Reaction product, then by the concentrate drying of modified-reaction product, grinding, organosilan blending reaction is added, reaction product is made, finally
By other material melts stirring cooling dischargings such as reaction product, epoxy resin, lignin up to the saturating leakage-repairing glue of high waterproof, seepage control, originally
Invention mixes bagasse and agricultural crop straw, and the organic fibre wherein having is isolated using high temperature high pressure process and dipping by lye
Dimension, sugar ingredient, and organic principle is hydrolyzed, carbochain fracture in part improves organic components and connects to ingredient each in leakage-repairing glue
Contacting surface product, bonds degree between each ingredient to improve in leakage-repairing glue, helps to reinforce the bonding degree after leak repairing adhesive curing, make
Space structure intensity after leak repairing adhesive curing increases, and improves compactness, inhibits the infiltration of moisture, improve the waterproofness of leakage-repairing glue
Can, also by aluminium ion introduced plant fiber, so that aluminium ion is adsorbed in organic fiber table using ionic bond, Absorptive complex wave effect
Face, and react aluminium ion and silica under the conditions of lye and generate meta-aluminic acid root and silicate component and be free in slurries,
To fully dispersed and more efficient contact organic fiber ingredient, by adjusting pH value to faintly acid using high temperature boiling,
Make to form nanometer grade silica and aluminium oxide in fibre composition, has filled up hole in plant fiber component, further enhanced anti-
Aqueous energy;
(2) present invention mixes calcium oxide with modified plant fiber, carbohydrate content and other organic compounds, makes calcium oxide
Molecule bonding is scattered in plant fiber, to make leakage-repairing glue when in use, calcium hydroxide is generated after contacting with water, and gradually give birth to
The mechanical property of leakage-repairing glue, more resistance to erosion are improved using the good rigidity of ingredients calcium carbonate and intensity at ingredients calcium carbonate,
Each pore structure in fiberfill fibers simultaneously, further increases the waterproof performance of leakage-repairing glue, and calcium oxide can give birth to when meeting water reaction
At a large amount of thermal energy, plant fiber component, carbohydrate content charing can be made, spacing contracting between each atom of organic principle in carbonization process
It is short, form a large amount of covalent bonds, further increase the compactness of leakage-repairing glue again, improve the waterproof performance of leakage-repairing glue, calcium oxide at
Dividing after meeting water contact and reacts acutely rapid, heat supply makes rapidly fibre composition fast charring, the leak repairing speed of leakage-repairing glue is effectively improved,
It has broad application prospects.
Specific embodiment
In mass ratio it is to crush in 6:1 investment pulverizer with agricultural crop straw by bagasse, is put into baking oven after crushing, In
2~3h of drying obtains dried material under conditions of temperature is 65~75 DEG C, is in mass ratio that 1:5 is thrown by dried material and distilled water
Enter in reaction kettle, air pressure in reaction kettle is increased to 1.2~1.6MPa, increases reactor temperature to 130~150 DEG C, constant temperature
Constant pressure reacts 60~70min and reacting slurry is made;It is in mass ratio 15:1 investment by above-mentioned reacting slurry and SiO 2 powder
In beaker, 20~30min is stirred with the revolving speed of 260~300r/min with blender, mixed serum is made, matter is added dropwise into beaker
It measures the sodium hydroxide solution that score is 15~20% and adjusts pH value to 11~12, place the beaker in resistance heating set, by heating mantle
Temperature is increased to 70~80 DEG C, stirs 60~80min with blender with the revolving speed of 300~360r/min and solidliquid mixture is made;
Be in mass ratio in 15:1 investment reaction kettle by above-mentioned solidliquid mixture and aluminium chloride reactor temperature is increased to 110~
120 DEG C, 60~80min is stirred with the revolving speed of 500~600r/min with agitating device, reacting slurry is made, dripped into reacting slurry
Add the hydrochloric acid solution that mass fraction is 5~7% to adjust pH value to 6.0~6.5, is stirred to react 30~40min, is filtered after stirring
To filter residue, as modified-reaction product;Above-mentioned modified-reaction product is put into Rotary Evaporators, is 150~180r/ in revolving speed
Rotary evaporation under conditions of min and temperature are 90~100 DEG C until enriched product is made in product quality constant weight, by enriched product with
Calcium oxide is in 15:1 investment planetary ball mill, in the item that ratio of grinding media to material is 10:1 and revolving speed is 150~180r/min in mass ratio
Grinding product is made in 30~40min of ground and mixed under part;It is in mass ratio that 6:1 investment is total by above-mentioned grinding product and organosilan
In mixed machine, 40~50min is mixed under conditions of revolving speed is 400~500r/min and temperature is 160~180 DEG C, is thrown after mixing
Enter in vacuum oven, reaction is made in dry 5~6h under conditions of vacuum degree is 100~200MPa and temperature is 60~80 DEG C
Product;According to parts by weight, by 9~12 parts of above-mentioned reaction products, 32~36 parts of epoxy resin, 1.2~1.6 parts of lignin, 2~
In 3 parts of polyetheramines, 1.5~1.8 parts of calcium carbonate investment heating furnaces, heating in-furnace temperature is increased to 120~150 DEG C, constant temperature is quiet
40~50min is set, 30~40min is stirred with the revolving speed of 500~550r/min with agitating device under this constant temperature, after stirring
0~40 DEG C is cooled to discharge up to the saturating leakage-repairing glue of high waterproof, seepage control.
Embodiment 1
Agricultural crop straw are as follows: corn stover
The preparation of modified-reaction product:
In mass ratio it is to crush in 6:1 investment pulverizer with corn stover by bagasse, is put into baking oven after crushing, be in temperature
Dry 2h obtains dried material under conditions of 65 DEG C, is in mass ratio that 1:5 is put into reaction kettle by dried material and distilled water, will
Air pressure is increased to 1.2MPa in reaction kettle, increases reactor temperature to 130 DEG C, constant temperature and pressure reacts 60min and reaction slurry is made
Liquid;
It is in mass ratio in 15:1 investment beaker, with blender with 260r/min's by above-mentioned reacting slurry and SiO 2 powder
Revolving speed stir 20min, be made mixed serum, into beaker be added dropwise mass fraction be 15% sodium hydroxide solution adjust pH value to
11, it places the beaker in resistance heating set, jacket temperature is increased to 70 DEG C, stirred with blender with the revolving speed of 300r/min
Solidliquid mixture is made in 60min;
It is in mass ratio to be increased to reactor temperature in 15:1 investment reaction kettle by above-mentioned solidliquid mixture and aluminium chloride
110 DEG C, reacting slurry is made with the revolving speed stirring 60min of 500r/min with agitating device, quality point is added dropwise into reacting slurry
Number adjusts pH value to 6.0 for 5% hydrochloric acid solution, is stirred to react 30min, filter residue is obtained by filtration after stirring, as modified-reaction produces
Object;
The preparation of reaction product:
Above-mentioned modified-reaction product is put into Rotary Evaporators, is 150r/min and condition backspin at a temperature of 90 °C in revolving speed
Turn to be evaporated up to the obtained enriched product of product quality constant weight, is in mass ratio 15:1 investment planet ball by enriched product and calcium oxide
In grinding machine, grinding product is made in ground and mixed 30min under conditions of ratio of grinding media to material is 10:1 and revolving speed is 150r/min;
In mass ratio it is in 6:1 investment blender by above-mentioned grinding product and organosilan, is 400r/min and temperature in revolving speed
40min is mixed under conditions of being 160 DEG C, is put into vacuum oven after mixing, in vacuum degree be 100MPa and temperature is 60 DEG C
Under conditions of dry 5h reaction product is made;
The preparation of the high saturating leakage-repairing glue of waterproof, seepage control:
According to parts by weight, by 9 parts of above-mentioned reaction products, 32 parts of epoxy resin, 1.2 parts of lignin, 2 parts of polyetheramines, 1.5 parts of carbon
In sour calcium investment heating furnace, heating in-furnace temperature is increased to 120 DEG C, constant temperature stands 40min, with stirring under this constant temperature
Device stirs 30min with the revolving speed of 500r/min, and 0 DEG C is cooled to after stirring and is discharged up to the saturating leakage-repairing glue of high waterproof, seepage control.
Embodiment 2
Agricultural crop straw are as follows: rice straw
The preparation of modified-reaction product:
In mass ratio it is to crush in 6:1 investment pulverizer with rice straw by bagasse, is put into baking oven after crushing, be in temperature
Dry 2.5h obtains dried material under conditions of 70 DEG C, is in mass ratio that 1:5 is put into reaction kettle by dried material and distilled water,
Air pressure in reaction kettle is increased to 1.4MPa, increases reactor temperature to 140 DEG C, constant temperature and pressure reacts 65min and reaction is made
Slurries;
It is in mass ratio in 15:1 investment beaker, with blender with 280r/min's by above-mentioned reacting slurry and SiO 2 powder
Revolving speed stir 25min, be made mixed serum, into beaker be added dropwise mass fraction be 17% sodium hydroxide solution adjust pH value to
11, it places the beaker in resistance heating set, jacket temperature is increased to 75 DEG C, stirred with blender with the revolving speed of 330r/min
Solidliquid mixture is made in 70min;
It is in mass ratio to be increased to reactor temperature in 15:1 investment reaction kettle by above-mentioned solidliquid mixture and aluminium chloride
115 DEG C, reacting slurry is made with the revolving speed stirring 70min of 550r/min with agitating device, quality point is added dropwise into reacting slurry
Number adjusts pH value to 6.2 for 6% hydrochloric acid solution, is stirred to react 35min, filter residue is obtained by filtration after stirring, as modified-reaction produces
Object;
The preparation of reaction product:
Above-mentioned modified-reaction product is put into Rotary Evaporators, is revolved under conditions of revolving speed is 170r/min and temperature is 95 DEG C
Turn to be evaporated up to the obtained enriched product of product quality constant weight, is in mass ratio 15:1 investment planet ball by enriched product and calcium oxide
In grinding machine, grinding product is made in ground and mixed 35min under conditions of ratio of grinding media to material is 10:1 and revolving speed is 170r/min;
In mass ratio it is in 6:1 investment blender by above-mentioned grinding product and organosilan, is 450r/min and temperature in revolving speed
45min is mixed under conditions of being 170 DEG C, is put into vacuum oven after mixing, in vacuum degree be 150MPa and temperature is 70 DEG C
Under conditions of dry 5.5h reaction product is made;
The preparation of the high saturating leakage-repairing glue of waterproof, seepage control:
According to parts by weight, by 10 parts of above-mentioned reaction products, 34 parts of epoxy resin, 1.4 parts of lignin, 2 parts of polyetheramines, 1.7 parts
Calcium carbonate is put into heating furnace, and heating in-furnace temperature is increased to 140 DEG C, and constant temperature stands 45min, with stirring under this constant temperature
It mixes device and 35min is stirred with the revolving speed of 520r/min, 20 DEG C are cooled to after stirring and is discharged up to the saturating leakage-repairing glue of high waterproof, seepage control.
Embodiment 3
Agricultural crop straw: wheat stalk
The preparation of modified-reaction product:
In mass ratio it is to crush in 6:1 investment pulverizer with wheat stalk by bagasse, is put into baking oven after crushing, be in temperature
Dry 3h obtains dried material under conditions of 75 DEG C, is in mass ratio that 1:5 is put into reaction kettle by dried material and distilled water, will
Air pressure is increased to 1.6MPa in reaction kettle, increases reactor temperature to 150 DEG C, constant temperature and pressure reacts 70min and reaction slurry is made
Liquid;
It is in mass ratio in 15:1 investment beaker, with blender with 300r/min's by above-mentioned reacting slurry and SiO 2 powder
Revolving speed stir 30min, be made mixed serum, into beaker be added dropwise mass fraction be 20% sodium hydroxide solution adjust pH value to
12, it places the beaker in resistance heating set, jacket temperature is increased to 80 DEG C, stirred with blender with the revolving speed of 360r/min
Solidliquid mixture is made in 80min;
It is in mass ratio to be increased to reactor temperature in 15:1 investment reaction kettle by above-mentioned solidliquid mixture and aluminium chloride
120 DEG C, reacting slurry is made with the revolving speed stirring 80min of 600r/min with agitating device, quality point is added dropwise into reacting slurry
Number adjusts pH value to 6.5 for 7% hydrochloric acid solution, is stirred to react 40min, filter residue is obtained by filtration after stirring, as modified-reaction produces
Object;
The preparation of reaction product:
Above-mentioned modified-reaction product is put into Rotary Evaporators, under conditions of revolving speed is 180r/min and temperature is 100 DEG C
Enriched product and calcium oxide are 15:1 investment planet until the obtained enriched product of product quality constant weight by rotary evaporation in mass ratio
In ball mill, grinding product is made in ground and mixed 40min under conditions of ratio of grinding media to material is 10:1 and revolving speed is 180r/min;
In mass ratio it is in 6:1 investment blender by above-mentioned grinding product and organosilan, is 500r/min and temperature in revolving speed
50min is mixed under conditions of being 180 DEG C, is put into vacuum oven after mixing, in vacuum degree be 200MPa and temperature is 80 DEG C
Under conditions of dry 6h reaction product is made;
The preparation of the high saturating leakage-repairing glue of waterproof, seepage control:
According to parts by weight, by 12 parts of above-mentioned reaction products, 36 parts of epoxy resin, 1.6 parts of lignin, 3 parts of polyetheramines, 1.8 parts
Calcium carbonate is put into heating furnace, and heating in-furnace temperature is increased to 150 DEG C, and constant temperature stands 50min, with stirring under this constant temperature
It mixes device and 40min is stirred with the revolving speed of 550r/min, 40 DEG C are cooled to after stirring and is discharged up to the saturating leakage-repairing glue of high waterproof, seepage control.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking modified-reaction product.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking reaction product.
Comparative example 3: the saturating leakage-repairing glue of high waterproof, seepage control of Shandong company production.
Curing time test: the leakage-repairing glue in embodiment and comparative example is used in house leak repairing, curing time is measured.
Anti-permeability test: the leakage-repairing glue in embodiment and comparative example is used in house leak repairing, in the ring of rain
Under border, after a week, infiltration has been seen whether.
Table 1: leakage-repairing glue performance measurement result
Detection project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
Curing time (h) | 12 | 12 | 11 | 16 | 18 | 15 |
Water absorption rate (%) | 0.006 | 0.006 | 0.005 | 0.015 | 0.016 | 0.009 |
Anti-permeability | Without infiltration | Without infiltration | Without infiltration | Obvious infiltration | Obvious infiltration | Obvious infiltration |
In summary, high waterproof, seepage control saturating leakage-repairing glue curing time of the invention is short as can be seen from Table 1, and leak repairing speed is fast, inhales
Water rate is low, and generates without infiltration, and waterproof performance is good, has broad prospect of application.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the saturating leakage-repairing glue of high waterproof, seepage control, it is characterised in that specific preparation step are as follows:
By in reaction product, epoxy resin, lignin, polyetheramine, calcium carbonate investment heating furnace, heating in-furnace temperature is increased to
120~150 DEG C, constant temperature stands 40~50min, is stirred under this constant temperature with agitating device with the revolving speed of 500~550r/min
30~40min is mixed, 0~40 DEG C is cooled to after stirring and is discharged up to the saturating leakage-repairing glue of high waterproof, seepage control;
The specific preparation step of the reaction product are as follows:
(1) modified-reaction product is put into Rotary Evaporators, in revolving speed be 150~180r/min and temperature is 90~100 DEG C
Under conditions of rotary evaporation until enriched product is made in product quality constant weight, enriched product and calcium oxide are put into planetary ball mill
In, in ratio of grinding media to material be 10:1 and revolving speed is that grinding product is made in 150~180r/min ground and mixed, 30~40min;
(2) by grinding product and organosilan investment blender, in revolving speed be 400~500r/min and temperature is 160~180
40~50min is mixed under conditions of DEG C, is put into vacuum oven after mixing, in vacuum degree be 100~200MPa and temperature is
Reaction product is made in dry 5~6h under conditions of 60~80 DEG C;
The specific preparation step of the modified-reaction product are as follows:
(1) it will be crushed in bagasse and agricultural crop straw investment pulverizer, put into baking oven after crushing, be 65~75 DEG C in temperature
Under conditions of dry 2~3h obtain dried material, be in mass ratio in 1:5 investment reaction kettle by dried material and distilled water, will
Air pressure is increased to 1.2~1.6MPa in reaction kettle, increases reactor temperature to 130~150 DEG C, and constant temperature and pressure reaction 60~
Reacting slurry is made in 70min;
(2) by reacting slurry and SiO 2 powder investment beaker, 20 are stirred with the revolving speed of 260~300r/min with blender
Mixed serum is made in~30min, and the sodium hydroxide solution that mass fraction is 15~20% is added dropwise into beaker and adjusts pH value to 11
~12, it places the beaker in resistance heating set, jacket temperature is increased to 70~80 DEG C, with blender with 300~360r/
The revolving speed of min stirs 60~80 obtained solidliquid mixtures;
(3) by solidliquid mixture and aluminium chloride investment reaction kettle, reactor temperature is increased, with agitating device with 500~
The revolving speed of 600r/min stirs 60~80min and reacting slurry is made, and the hydrochloric acid that mass fraction is 5~7% is added dropwise into reacting slurry
Solution adjusts pH value to 6.0~6.5, is stirred to react 30~40min, filter residue, as modified-reaction product are obtained by filtration after stirring.
2. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: preferably press
Parts by weight meter, the reaction product is 9~12 parts, epoxy resin is 32~36 parts, lignin is 1.2~1.6 parts, polyethers
Amine is 2~3 parts, calcium carbonate is 1.5~1.8 parts.
3. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: reaction product
Specific preparation step (1) described in the mass ratio of enriched product and calcium oxide be 15:1.
4. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: reaction product
Specific preparation step (2) described in the mass ratio of grinding product and organosilan be 6:1.
5. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: modified-reaction
The mass ratio of bagasse described in the specific preparation step (1) of product and agricultural crop straw is 6:1.
6. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: modified-reaction
Agricultural crop straw described in the specific preparation step (1) of product is more preferably corn stover, rice straw and Wheat Straw
Stalk one or more of them mixes in any proportion.
7. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: modified-reaction
The mass ratio of reacting slurry described in the specific preparation step (2) of product and SiO 2 powder is 15:1.
8. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: modified-reaction
The mass ratio of solidliquid mixture described in the specific preparation step (3) of product and aluminium chloride is 15:1.
9. a kind of preparation method of high saturating leakage-repairing glue of waterproof, seepage control according to claim 1, it is characterised in that: modified-reaction
Reactor temperature described in the specific preparation step (3) of product is increased to 110~120 DEG C.
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CN113683899A (en) * | 2021-09-02 | 2021-11-23 | 程小冬 | High-strength high-viscosity asphalt and preparation method thereof |
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CN103834341A (en) * | 2013-12-31 | 2014-06-04 | 浙江杰立建设集团有限公司 | Leak repairing adhesive for house and preparation method thereof |
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CN103834341A (en) * | 2013-12-31 | 2014-06-04 | 浙江杰立建设集团有限公司 | Leak repairing adhesive for house and preparation method thereof |
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CN113683899A (en) * | 2021-09-02 | 2021-11-23 | 程小冬 | High-strength high-viscosity asphalt and preparation method thereof |
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