CN108503306A - A kind of preparation method of lower shrinkage grouting material - Google Patents
A kind of preparation method of lower shrinkage grouting material Download PDFInfo
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- CN108503306A CN108503306A CN201810361041.1A CN201810361041A CN108503306A CN 108503306 A CN108503306 A CN 108503306A CN 201810361041 A CN201810361041 A CN 201810361041A CN 108503306 A CN108503306 A CN 108503306A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/282—Polyurethanes; Polyisocyanates
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- 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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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
- C08G18/4825—Polyethers containing two hydroxy groups
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6677—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
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- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/70—Grouts, e.g. injection mixtures for cables for prestressed concrete
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Abstract
The invention discloses a kind of preparation methods of lower shrinkage grouting material, belong to construction material preparing technical field.Modified cyclodextrin is quaternary ammonium cation cyclodextrin in the present invention,A small amount of quaternary ammonium cation cyclodextrin can in water in colloidal form coat portland cement in grouting material,To the cation on the metal silicate surface in cement repulsive interaction can occur for quaternary ammonium cation cyclodextrin,Modified material of the lignin one side that the present invention is recycled from stalk slag as cyclodextrin,Lignin itself has larger space structure,It will produce larger steric hindrance in cyclodextrin,Be conducive to improve the dispersion performance of cyclodextrin,The high degree of dispersion of cement granules can be kept before solidification,Slurry is set to keep uniform density,Reduce the shrinkage in solidification later stage,Additionally incorporate a certain amount of lignin,The average molecular weight of cyclodextrin can be increased,Improve settled density of the cyclodextrin when surface of constructing bonds,To enhance the compression strength of grouting material,It has a extensive future.
Description
Technical field
The invention discloses a kind of preparation methods of lower shrinkage grouting material, belong to construction material preparing technical field.
Background technology
Grouting material be using high-strength material as aggregate, using cement as bonding agent, be aided with upper flow regime, microdilatancy, prevent from
The substances such as analysis are formulated.A certain amount of water is added in it at the construction field (site), can be used after stirring evenly.Grouting material has gravity flow
Property good, fast hard, early strong, high-strength, ungauged regions, microdilatancy；It is nontoxic, harmless, not aging, pollution-free to water quality and ambient enviroment, from
The features such as close property is good, antirust.There is reliable in quality in construction party face, the advantages that reducing cost, shorten the construction period and is easy to use.From
Fundamentally change plant bottom case stressing conditions, is allowed to equably bear the whole load of equipment, to meet various machineries, electric appliance
Equipment（Jumbo high-precision grinder）Installation requirement, be without pad the installation epoch ideal grouting material.Grouting material is mainly used
In：Foot bolt fastening, the repairing of runway, the fixation of nuclear power generating equipment, the reinforcing of road and bridge engineering, machinery bed, steel construction
With ground Huai Kou, Equipment Foundations back-grouting, plant bury reinforcing bar, concrete structure reinforcement and transformation, old concrete structure is split
It stitching and administers, mechanical and electric equipment installation, track and Steel Structure Installation, static press piling engineering seal stake, and building is reinforced, beam cross-section increasing,
The reparation of thickening and the leakage infiltration of wall body structure, various foundation engineerings collapse grouting and various salvagings etc..
The method poured into a mould according to conventional cement mortar, it usually needs maintenance in 7 days or more can just come into operation.Metallurgical, change
The Bar Anchorage and foundation grouting of the constructions such as work, electric power, building materials, railway, highway, bridge and equipment, suffer from coagulation soil matrix
The hardening of plinth second pouring and the limitation of curing time.The high-strength grout of early stage is mainly made of organic resin epoxy,
It involves great expense, is easy to aging, being more toxic, and the effect is unsatisfactory.
In recent years, as economic construction of China and science and technology develop rapidly, the processing water of China's cement-based grouting material
Flat to have obtained larger promotion with technical performance, every technical performance has reached world level, existing cement base class injection material
Expect that cementitious material is based on sulphate aluminium cement, high alumina cement, production cost is higher, and production technology uses and stirring is simply mixed
Mode, product early stage flexural strength is low, and the later stage is cracking, compression strength declines, durability is poor.It is well known that Portland
The required ratio of mud of hydrated cementitious is no more than 0.42, and the ratio of mud is bigger, and slurry setting time is longer, and the intensity of hardenite is got over
Low, shrinkage is bigger, finally slurry strength development will be caused slow, durability is poor.Moreover, will be more than that hydrated cementitious institute water requirement fills
Enter roadbed and base, road structure stability and service life can be seriously affected, the negative effect generated is self-evident.
Therefore, invent a kind of lower shrinkage grouting material has positive effect to construction material technology of preparing.
Invention content
Present invention mainly solves the technical issues of, be often used the larger ratio of mud for current conventional grout material, usually
It is 1:1 is even higher, although obtained fluidity of slurry is preferable, the ratio of mud is bigger, and slurry setting time is longer, hardenite
Intensity is lower, and shrinkage is bigger, and it is slow to eventually lead to slurry strength development, makes that the grouting material solidification later stage is cracking, resistance to compression
The defect that intensity declines, provides a kind of preparation method of lower shrinkage grouting material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of lower shrinkage grouting material, it is characterised in that specifically preparation process is：
（1）200~230g stalks slag, 400~450mL sodium hydroxide solutions are put into the water-bath kettle with blender,
Heating water bath heats up, and starts blender, stirs, filtering, and removal filter residue obtains lignin lye, by lignin lye glacial acetic acid
It is neutralized to neutrality, obtains lignin suspension, high speed centrifugation removes supernatant liquor, and isolated lower sediment, it is heavy to be washed with water
After forming sediment 2~3 times, it is placed in drying in baking oven, obtains lignin powder；
（2）70~75g beta-cyclodextrins and 100~130mL sodium hydroxide solutions are added into beaker, after stirring at room temperature, then adds
Enter 5~10g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath, heat temperature raising, insulation reaction, filtering removal filter
Liquid obtains solid crude product；
（3）Solid crude product is obtained neutralizer, neutralizer is set with 200~250mL hot water dissolvings with dilute hydrochloric acid adjusting pH
In vacuum drying chamber it is dry after, be placed in 3~4h of grinding in mortar, obtain dried powder, by 50~55g dried powders with 200
~220mLDMF dissolves, and obtains DMF lysates, and 150~170mL acetone is added to DMF lysates, obtains white slurry；
（4）Above-mentioned white slurry is filtered into the removal isolated product of filtrate, product is placed in drying in vacuum drying chamber, is obtained
Wood fibre is placed in calcining furnace by modified cyclodextrin, will calcine stove evacuation, is heated to 600~650 DEG C, pyrocarbon
Change, obtain carbonized wooden fiber, expanded perlite is mixed with quartz sand, obtains mixing aggregate；
（5）Count in parts by weight, into the dry three-necked flask with condensing unit be added 30~40 parts of polyetherdiol, 20~
30 parts of rosin, under nitrogen protection, temperature programming is used in combination magnetic stirring apparatus to be dispersed with stirring 30 with the rotating speed of 200~300r/min
~40min, 80~90 parts of hexamethylene diisocyanates are added into above-mentioned three-necked flask, and the reaction was continued 2~3h waits for that three-necked flask drops
10~15 parts of dihydromethyl propionic acids, 20~30 parts of glycerine and 20~25 parts of maleic anhydrides are added in temperature into three-necked flask successively, will
It after 3~5 parts of dibutyl tin laurates are dissolved in 35~40 parts of acetone, is instilled in three-necked flask with constant pressure funnel, side is added dropwise
Side is heated up, and being warming up to certain temperature, the reaction was continued, obtains polyurethane slurry；
（6）It counts in parts by weight, 70~80 parts of polyurethane slurries is placed in blender, 12~15 are added into polyurethane slurry
Part carbonized wooden fiber, 30~40 parts of mixing aggregates, 10~15 parts of lignin powders, 1~2 part of hydroxymethyl cellulose, 40~50 parts
Portland cement continues that 0.8~1.0 part of triethylamine is added into polyurethane slurry, is improved after being stirred to react under agitation
Speed of agitator continues to be dispersed with stirring, and obtains lower shrinkage grouting material.
Step（1）The mass fraction of the sodium hydroxide solution is 45%, and temperature is 90 after the heating of reaction kettle heating water bath
~95 DEG C, high speed centrifugation rotating speed is 3500~3700r/min, and the high speed centrifugation time is 12~15min, sets oven temperature as 70
~80 DEG C, drying time is 4~5h.
Step（2）The sodium hydroxide solution mass fraction is 90%, and temperature is 50~55 DEG C after heat temperature raising, heat preservation
Reaction time is 3~4h.
Step（3）The hot water temperature is 60~65 DEG C, and dilute hydrochloric acid mass fraction is 10%, and it is 6 to adjust pH with dilute hydrochloric acid
~7, vacuum drying chamber set temperature is 80~90 DEG C, and drying time is 3~4h.
Step（4）The vacuum drying chamber set temperature is 80~90 DEG C, and drying time is 4~5h, after heat temperature raising
Temperature is 600~650 DEG C, and the high temperature carbonization time is 3~4h, and expanded perlite grain size is 200 mesh, and quartz sand particle size is 100 mesh,
Expanded perlite is 1 ︰ 3 with quartz sand mixing quality ratio.
Step（5）The heating rate is 3~5 DEG C/min, and temperature is 90~100 DEG C after heating, three-necked flask cooling
Temperature is 50~60 DEG C afterwards, and constant pressure funnel drop rate is 2~3mL/min, and heating rate is 3~5 DEG C/min, after heating
Temperature is 80~82 DEG C, and the reaction was continued, and the time is 3~4h.
Step（6）Rotating speed is 300~400r/min under the stirring condition, and it is 10~15min to be stirred to react the time, is carried
High speed of agitator continues to be dispersed with stirring the time as 20~30min to 600~800r/min.
The beneficial effects of the invention are as follows：
（1）The present invention obtains lignin lye using discarded stalk as raw material, by heating soda boiling, by lignin lye acetic acid
After neutralization, through high speed centrifugation, washs, is dried to obtain lignin powder, epoxy is added after beta-cyclodextrin is alkalized
Solid crude product is obtained by filtration after ammonium chloride heating reaction, by solid crude product with hot water dissolving, by neutralization, grinding, ties again
Be dried to obtain modified cyclodextrin after crystalline substance purification, expanded perlite be mixed to get with quartz sand and mixes aggregate, by polyetherdiol and
Rosin is placed in three-necked flask, and heating under nitrogen protection is dispersed with stirring, and adds di-isocyanate, hydroxymethyl propionic acid, sweet
The raw materials such as oil and maleic anhydride, are obtained by the reaction polyurethane slurry, and carbonized wooden fiber, mixing bone are mixed into polyurethane slurry
Material, lignin powder, hydroxymethyl cellulose, triethylamine obtain lower shrinkage grouting material, in of the invention by reacting, being dispersed with stirring
Modified cyclodextrin is quaternary ammonium cation cyclodextrin, and a small amount of quaternary ammonium cation cyclodextrin can be in water with glue in grouting material
Body form coats portland cement, and quaternary ammonium cation cyclodextrin can send out the cation on the metal silicate surface in cement
Raw repulsive interaction, cyclodextrin is quickly bonded in aggregate surface, to keep solidification later stage aggregate and cement granules mutually exclusive, reduces
The shrinkage of grouting material and avoid grouting material cracking；
（2）Modified material of the lignin one side that the present invention is recycled from stalk slag as cyclodextrin, utilizes lignin itself
Property with larger space structure will produce larger steric hindrance in cyclodextrin, be conducive to the dispersion for improving cyclodextrin
Performance, sodium sulfite and the lignin of addition occur sulfonating reaction, sulfonic acid group are on the other hand introduced in lignin molecule, can
To improve the hydrophilicity of grouting material, the high degree of dispersion of cement granules can be kept before solidification, and slurry is made to keep uniform
Density reduces the shrinkage in solidification later stage, additionally incorporates a certain amount of lignin, it is possible to increase the average molecular weight of cyclodextrin carries
Settled density of the high cyclodextrin when surface of constructing bonds has a extensive future to enhance the compression strength of grouting material.
Specific implementation mode
200~230g stalks slag, the sodium hydroxide solution that 400~450mL mass fractions are 45% are put into blender
Water-bath kettle in, heating water bath is warming up to 90~95 DEG C, starts blender, stirs 3~5h, filtering, and removal filter residue obtains
Lignin lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension by lignin lye, with
The rotating speed of 3500~3700r/min, 12~15min of high speed centrifugation remove supernatant liquor, and isolated lower sediment is washed with water
It after washing precipitation 2~3 times, is placed in the baking oven that set temperature is 70~80 DEG C, dry 4~5h obtains lignin powder；Into beaker
The sodium hydroxide solution that 70~75g beta-cyclodextrins and 100~130mL mass fractions are 90% is added, stir 10 at room temperature~
After 15min, 5~10g epoxypropyltrimethylchloride chlorides are added, beaker is placed in water-bath, are heated to 50~55
DEG C, 3~4h of insulation reaction, filtering removal filtrate obtains solid crude product；It is 60 by solid crude product 200~250mL temperature
~65 DEG C of hot water dissolving, the dilute hydrochloric acid for being 10% with mass fraction adjust pH to 6~7, obtain neutralizer, neutralizer is placed in
In the vacuum drying chamber that set temperature is 80~90 DEG C, after dry 3~4h, it is placed in 3~4h of grinding in mortar, obtains xeraphium
End, by 50~55g dried powders with 200~220mLDMF dissolve, obtain DMF lysates, to DMF lysates be added 150~
170mL acetone obtains white slurry；Above-mentioned white slurry is filtered into the removal isolated product of filtrate, product is placed in setting
In the vacuum drying chamber that temperature is 80~90 DEG C, dry 4~5h obtains modified cyclodextrin, wood fibre is placed in calcining furnace,
Stove evacuation will be calcined, is heated to 600~650 DEG C, 3~4h of high temperature carbonization obtains carbonized wooden fiber, by 200 purposes
Expanded perlite and the quartz sand of 100 mesh are that 1 ︰ 3 mix in mass ratio, obtain mixing aggregate, count in parts by weight, to dry
30~40 parts of polyetherdiol, 20~30 parts of rosin are added in three-necked flask with condensing unit, under nitrogen protection, with 3~5
DEG C/the heating rate temperature programming of min to 90~100 DEG C, be used in combination magnetic stirring apparatus with the rotating speed stirring point of 200~300r/min
30~40min is dissipated, 80~90 parts of hexamethylene diisocyanates are added into above-mentioned three-necked flask, the reaction was continued 2~3h waits for three-necked flask
50~60 DEG C are cooled to, 10~15 parts of dihydromethyl propionic acids, 20~30 parts of glycerine and 20~25 are added into three-necked flask successively
Part maleic anhydride, after 3~5 parts of dibutyl tin laurates are dissolved in 35~40 parts of acetone, with constant pressure funnel with 2~3mL/
The drop rate of min instills in three-necked flask, heat up when being added dropwise, and control heating rate is 3~5 DEG C/min, it is warming up to 80~
82 DEG C, the reaction was continued 3~4h, obtain polyurethane slurry；It counts in parts by weight, 70~80 parts of polyurethane slurries is placed in blender
In, 12~15 parts of carbonized wooden fibers, 30~40 parts of mixing aggregates, 10~15 parts of lignin powders, 1 are added into polyurethane slurry
~2 parts of hydroxymethyl celluloses, 40~50 parts of portland cements continue under the rotating speed stirring condition of 300~400r/min to poly-
0.8~1.0 part of triethylamine is added in urethane slurry, speed of agitator is improved to 600~800r/ after being stirred to react 10~15min
Min continues to be dispersed with stirring 20~30min, obtains lower shrinkage grouting material.
Example 1
200g stalks slag, the sodium hydroxide solution that 400mL mass fractions are 45% are put into the water-bath kettle with blender
In, heating water bath is warming up to 90 DEG C, starts blender, stirs 3h, filtering, removal filter residue obtains lignin lye, by lignin
Lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension, with the rotating speed of 3500r/min, high speed
12min is centrifuged, supernatant liquor is removed, isolated lower sediment is washed with water after precipitating 2 times, and it is 70 DEG C to be placed in set temperature
Baking oven in, dry 4h obtains lignin powder；The hydrogen that 70g beta-cyclodextrins and 100mL mass fractions are 90% is added into beaker
Sodium hydroxide solution adds 5g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath after stirring 10min at room temperature,
50 DEG C, insulation reaction 3h are heated to, filtering removal filtrate obtains solid crude product；By solid crude product 200mL temperature
For 60 DEG C of hot water dissolving, the dilute hydrochloric acid for being 10% with mass fraction adjusts pH to 6, obtains neutralizer, neutralizer is placed in setting
In the vacuum drying chamber that temperature is 80 DEG C, after dry 3h, it is placed in mortar and grinds 3h, obtain dried powder, by 50g dried powders
It is dissolved with 200mLDMF, obtains DMF lysates, 150mL acetone is added to DMF lysates, obtains white slurry；By above-mentioned white
Slurry filters the removal isolated product of filtrate, product is placed in the vacuum drying chamber that set temperature is 80 DEG C, and dry 4h is obtained
To modified cyclodextrin, wood fibre is placed in calcining furnace, stove evacuation will be calcined, is heated to 600 DEG C, high temperature carbonization
3h obtains carbonized wooden fiber, and the expanded perlite of 200 mesh is mixed for 1 ︰ 3 in mass ratio with the quartz sand of 100 mesh, is obtained
Aggregate is mixed, is counted in parts by weight, 30 parts of polyetherdiol, 20 portions of pines are added into the dry three-necked flask with condensing unit
Perfume (or spice) with the heating rate temperature programming of 3 DEG C/min to 90 DEG C, is used in combination magnetic stirring apparatus with 200r/min's under nitrogen protection
Rotating speed is dispersed with stirring 30min, and 80 parts of hexamethylene diisocyanates are added into above-mentioned three-necked flask, and the reaction was continued 2h waits for three-necked flask
50 DEG C are cooled to, 10 parts of dihydromethyl propionic acids, 20 parts of glycerine and 20 parts of maleic anhydrides are added into three-necked flask successively, by 3 parts
After dibutyl tin laurate is dissolved in 35 parts of acetone, three-necked flask is instilled with the drop rate of 2mL/min with constant pressure funnel
In, heat up when being added dropwise, control heating rate is 3 DEG C/min, is warming up to 80 DEG C, and the reaction was continued 3h obtains polyurethane slurry；It presses
70 parts of polyurethane slurries are placed in blender by parts by weight meter, and 12 parts of carbonized wooden fibers, 30 are added into polyurethane slurry
Part mixing aggregate, 10 parts of lignin powders, 1 part of hydroxymethyl cellulose, 40 parts of portland cements, in the rotating speed stirring bar of 300r/min
Under part, continue that 0.8 part of triethylamine is added into polyurethane slurry, be stirred to react after 10min and improve speed of agitator to 600r/min,
Continue to be dispersed with stirring 20min, obtains lower shrinkage grouting material.
Example 2
210g stalks slag, the sodium hydroxide solution that 420mL mass fractions are 45% are put into the water-bath kettle with blender
In, heating water bath is warming up to 92 DEG C, starts blender, stirs 4h, filtering, removal filter residue obtains lignin lye, by lignin
Lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension, with the rotating speed of 3600r/min, high speed
14min is centrifuged, supernatant liquor is removed, isolated lower sediment is washed with water after precipitating 2 times, and it is 75 DEG C to be placed in set temperature
Baking oven in, dry 4.5h obtains lignin powder；It is 90% that 72g beta-cyclodextrins and 115mL mass fractions are added into beaker
Sodium hydroxide solution adds 7g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath after stirring 12min at room temperature
In, 52 DEG C, insulation reaction 3.5h are heated to, filtering removal filtrate obtains solid crude product；By solid crude product 220mL
The hot water dissolving that temperature is 62 DEG C, the dilute hydrochloric acid for being 10% with mass fraction adjust pH to 6, obtain neutralizer, neutralizer is placed in
In the vacuum drying chamber that set temperature is 85 DEG C, after dry 3.5h, it is placed in mortar and grinds 3.5h, obtain dried powder, by 52g
Dried powder is dissolved with 210mLDMF, obtains DMF lysates, and 160mL acetone is added to DMF lysates, obtains white slurry；It will
Above-mentioned white slurry filters the removal isolated product of filtrate, product is placed in the vacuum drying chamber that set temperature is 85 DEG C,
Dry 4.5h, obtains modified cyclodextrin, wood fibre is placed in calcining furnace, will calcine stove evacuation, be heated to 620
DEG C, high temperature carbonization 3.5h obtains carbonized wooden fiber, is in mass ratio by the expanded perlite of 200 mesh and the quartz sand of 100 mesh
1 ︰ 3 is mixed, and is obtained mixing aggregate, is counted in parts by weight, and 35 parts are added into the dry three-necked flask with condensing unit and gathers
With the heating rate temperature programming of 4 DEG C/min to 95 DEG C, magnetic stirring apparatus is used in combination under nitrogen protection in ether glycol, 25 parts of rosin
It is dispersed with stirring 35min with the rotating speed of 250r/min, 85 parts of hexamethylene diisocyanates are added into above-mentioned three-necked flask, the reaction was continued
2.5h waits for that three-necked flask is cooled to 55 DEG C, successively 12 parts of dihydromethyl propionic acids of addition, 25 parts of glycerine and 22 parts into three-necked flask
Maleic anhydride, after 4 parts of dibutyl tin laurates are dissolved in 37 parts of acetone, with constant pressure funnel with the dropwise addition speed of 2mL/min
Rate instills in three-necked flask, heat up when being added dropwise, and control heating rate is 4 DEG C/min, is warming up to 81 DEG C, the reaction was continued 3.5h,
Obtain polyurethane slurry；It counts in parts by weight, 75 parts of polyurethane slurries is placed in blender, 13 are added into polyurethane slurry
Part carbonized wooden fiber, 35 parts of mixing aggregates, 12 parts of lignin powders, 1 part of hydroxymethyl cellulose, 45 parts of portland cements,
Under the rotating speed stirring condition of 350r/min, continues that 0.9 part of triethylamine is added into polyurethane slurry, carried after being stirred to react 12min
High speed of agitator continues to be dispersed with stirring 25min to 700r/min, obtains lower shrinkage grouting material.
Example 3
230g stalks slag, the sodium hydroxide solution that 450mL mass fractions are 45% are put into the water-bath kettle with blender
In, heating water bath is warming up to 95 DEG C, starts blender, stirs 5h, filtering, removal filter residue obtains lignin lye, by lignin
Lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension, with the rotating speed of 3700r/min, high speed
15min is centrifuged, supernatant liquor is removed, isolated lower sediment is washed with water after precipitating 3 times, and it is 80 DEG C to be placed in set temperature
Baking oven in, dry 5h obtains lignin powder；The hydrogen that 75g beta-cyclodextrins and 130mL mass fractions are 90% is added into beaker
Sodium hydroxide solution adds 10g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath after stirring 15min at room temperature
In, 55 DEG C, insulation reaction 4h are heated to, filtering removal filtrate obtains solid crude product；By solid crude product 250mL temperature
Degree is 65 DEG C of hot water dissolving, adjusts pH to 7 for 10% dilute hydrochloric acid with mass fraction, obtains neutralizer, neutralizer is placed in and is set
In fixed vacuum drying chamber at a temperature of 90 °C, after dry 4h, it is placed in mortar and grinds 4h, obtain dried powder, by 55g xeraphiums
End is dissolved with 220mLDMF, obtains DMF lysates, and 170mL acetone is added to DMF lysates, obtains white slurry；It will be above-mentioned white
Toner slurry filters the removal isolated product of filtrate, product is placed in the vacuum drying chamber that set temperature is 90 DEG C, dry 5h,
Modified cyclodextrin is obtained, wood fibre is placed in calcining furnace, stove evacuation will be calcined, is heated to 650 DEG C, high temperature carbonization
4h obtains carbonized wooden fiber, and the expanded perlite of 200 mesh is mixed for 1 ︰ 3 in mass ratio with the quartz sand of 100 mesh, is obtained
Aggregate is mixed, is counted in parts by weight, 40 parts of polyetherdiol, 30 portions of pines are added into the dry three-necked flask with condensing unit
Perfume (or spice) with the heating rate temperature programming of 5 DEG C/min to 100 DEG C, is used in combination magnetic stirring apparatus with 300r/min's under nitrogen protection
Rotating speed is dispersed with stirring 40min, and 90 parts of hexamethylene diisocyanates are added into above-mentioned three-necked flask, and the reaction was continued 3h waits for three-necked flask
60 DEG C are cooled to, 15 parts of dihydromethyl propionic acids, 30 parts of glycerine and 25 parts of maleic anhydrides are added into three-necked flask successively, by 5 parts
After dibutyl tin laurate is dissolved in 40 parts of acetone, three-necked flask is instilled with the drop rate of 3mL/min with constant pressure funnel
In, heat up when being added dropwise, control heating rate is 5 DEG C/min, is warming up to 82 DEG C, and the reaction was continued 4h obtains polyurethane slurry；It presses
80 parts of polyurethane slurries are placed in blender by parts by weight meter, and 15 parts of carbonized wooden fibers, 40 are added into polyurethane slurry
Part mixing aggregate, 15 parts of lignin powders, 2 parts of hydroxymethyl celluloses, 50 parts of portland cements, in the rotating speed stirring bar of 400r/min
Under part, continue that 1.0 parts of triethylamines are added into polyurethane slurry, be stirred to react after 15min and improve speed of agitator to 800r/min,
Continue to be dispersed with stirring 30min, obtains lower shrinkage grouting material.
Comparative example
With the lower shrinkage grouting material of Guangdong company production as a comparison case to lower shrinkage grouting material produced by the present invention and
Lower shrinkage grouting material in comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Fluidity test is detected using slurries fluidity tester；
Intensity test is detected by grouting material existing national standards GB50204；
Flexural strength test is pressed《Cement-based grouting material application technology specification GB/T50448-2008》It is detected；
Surface situation of change test：After grouting material in example 1~3 and comparative example is completed solidification, place 7 days and 14 days
Afterwards, face checking situation is observed.
1 grouting material performance measurement result of table
According to the lower shrinkage grouting material good fluidity produced by the present invention of data among the above, slurry setting time is longer, by force
Degree is higher, and the solidification later stage happens without cracking, and compression strength is high, has broad application prospects.
Claims (7)
1. a kind of preparation method of lower shrinkage grouting material, it is characterised in that specifically preparation process is：
（1）200~230g stalks slag, 400~450mL sodium hydroxide solutions are put into the water-bath kettle with blender,
Heating water bath heats up, and starts blender, stirs, filtering, and removal filter residue obtains lignin lye, by lignin lye glacial acetic acid
It is neutralized to neutrality, obtains lignin suspension, high speed centrifugation removes supernatant liquor, and isolated lower sediment, it is heavy to be washed with water
After forming sediment 2~3 times, it is placed in drying in baking oven, obtains lignin powder；
（2）70~75g beta-cyclodextrins and 100~130mL sodium hydroxide solutions are added into beaker, after stirring at room temperature, then adds
Enter 5~10g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath, heat temperature raising, insulation reaction, filtering removal filter
Liquid obtains solid crude product；
（3）Solid crude product is obtained neutralizer, neutralizer is set with 200~250mL hot water dissolvings with dilute hydrochloric acid adjusting pH
In vacuum drying chamber it is dry after, be placed in 3~4h of grinding in mortar, obtain dried powder, by 50~55g dried powders with 200
~220mLDMF dissolves, and obtains DMF lysates, and 150~170mL acetone is added to DMF lysates, obtains white slurry；
（4）Above-mentioned white slurry is filtered into the removal isolated product of filtrate, product is placed in drying in vacuum drying chamber, is obtained
Wood fibre is placed in calcining furnace by modified cyclodextrin, will calcine stove evacuation, is heated to 600~650 DEG C, pyrocarbon
Change, obtain carbonized wooden fiber, expanded perlite is mixed with quartz sand, obtains mixing aggregate；
（5）Count in parts by weight, into the dry three-necked flask with condensing unit be added 30~40 parts of polyetherdiol, 20~
30 parts of rosin, under nitrogen protection, temperature programming is used in combination magnetic stirring apparatus to be dispersed with stirring 30 with the rotating speed of 200~300r/min
~40min, 80~90 parts of hexamethylene diisocyanates are added into above-mentioned three-necked flask, and the reaction was continued 2~3h waits for that three-necked flask drops
10~15 parts of dihydromethyl propionic acids, 20~30 parts of glycerine and 20~25 parts of maleic anhydrides are added in temperature into three-necked flask successively, will
It after 3~5 parts of dibutyl tin laurates are dissolved in 35~40 parts of acetone, is instilled in three-necked flask with constant pressure funnel, side is added dropwise
Side is heated up, and being warming up to certain temperature, the reaction was continued, obtains polyurethane slurry；
（6）It counts in parts by weight, 70~80 parts of polyurethane slurries is placed in blender, 12~15 are added into polyurethane slurry
Part carbonized wooden fiber, 30~40 parts of mixing aggregates, 10~15 parts of lignin powders, 1~2 part of hydroxymethyl cellulose, 40~50 parts
Portland cement continues that 0.8~1.0 part of triethylamine is added into polyurethane slurry, is improved after being stirred to react under agitation
Speed of agitator continues to be dispersed with stirring, and obtains lower shrinkage grouting material.
2. a kind of preparation method of lower shrinkage grouting material according to claim 1, it is characterised in that：Step（1）It is described
Sodium hydroxide solution mass fraction be 45%, reaction kettle heating water bath heating after temperature be 90~95 DEG C, high speed centrifugation rotating speed
For 3500~3700r/min, the high speed centrifugation time is 12~15min, sets oven temperature as 70~80 DEG C, drying time 4
~5h.
3. a kind of preparation method of lower shrinkage grouting material according to claim 1, it is characterised in that：Step（2）It is described
Sodium hydroxide solution mass fraction be 90%, temperature is 50~55 DEG C after heat temperature raising, and the insulation reaction time is 3~4h.
4. a kind of preparation method of lower shrinkage grouting material according to claim 1, it is characterised in that：Step（3）It is described
Hot water temperature be 60~65 DEG C, dilute hydrochloric acid mass fraction be 10%, with dilute hydrochloric acid adjust pH be 6~7, vacuum drying chamber setting
Temperature is 80~90 DEG C, and drying time is 3~4h.
5. a kind of preparation method of lower shrinkage grouting material according to claim 1, it is characterised in that：Step（4）It is described
Vacuum drying chamber set temperature be 80~90 DEG C, drying time is 4~5h, and temperature is 600~650 DEG C after heat temperature raising, high
Warm carbonization time is 3~4h, and expanded perlite grain size is 200 mesh, and quartz sand particle size is 100 mesh, expanded perlite and quartz sand
Mixing quality ratio is 1 ︰ 3.
6. a kind of preparation method of lower shrinkage grouting material according to claim 1, it is characterised in that：Step（5）It is described
Heating rate be 3~5 DEG C/min, temperature is 90~100 DEG C after heating, and temperature is 50~60 DEG C after three-necked flask cooling, permanent
Pressure dropping funel drop rate is 2~3mL/min, and heating rate is 3~5 DEG C/min, and temperature is 80~82 DEG C after heating, is continued
Reaction time is 3~4h.
7. a kind of preparation method of lower shrinkage grouting material according to claim 1, it is characterised in that：Step（6）It is described
Stirring condition under rotating speed be 300~400r/min, it is 10~15min to be stirred to react the time, improve speed of agitator to 600~
800r/min continues to be dispersed with stirring the time as 20~30min.
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| CN112028540A (en) * | 2020-09-14 | 2020-12-04 | 赵良文 | Environment-friendly water-retaining mortar plasticizer and preparation method thereof |
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