CN107512722A - Adjust the expansile method of black cotton regur soil - Google Patents

Adjust the expansile method of black cotton regur soil Download PDF

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Publication number
CN107512722A
CN107512722A CN201710557269.3A CN201710557269A CN107512722A CN 107512722 A CN107512722 A CN 107512722A CN 201710557269 A CN201710557269 A CN 201710557269A CN 107512722 A CN107512722 A CN 107512722A
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black cotton
regur soil
cotton regur
silane
solution
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CN107512722B (en
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苗世顶
黄金秋
张培萍
张鹏
王健
沈兆普
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Jilin University
China Road and Bridge Corp
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Jilin University
China Road and Bridge Corp
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/36Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40Clays

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  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

The invention provides one kind to adjust the expansile method of black cotton regur soil, including:Pretreatment is carried out to black cotton regur soil and obtains black cotton regur soil sample, wherein, the pretreatment includes acidification or the pillared processing of sodium;Silane is hydrolyzed, obtains silane hydrolyzate solution;Silane Grafted is carried out to the pretreated black cotton regur soil using the silane hydrolyzate solution, obtains the black cotton regur soil sample of Silane Grafted.The method provided according to embodiments of the present invention, mainly by black cotton regur soil is acidified or sodium pre-process, after obtaining the black cotton regur soil with certain activity, it is grafted with the silane of various concentrations, condensation reaction is carried out by the hydroxyl of silane and black cotton regur soil lamella, black cotton regur soil is changed into hydrophobicity from hydrophily, and then changes the water absorption behavior of black cotton regur soil.

Description

Adjust the expansile method of black cotton regur soil
Technical field
The present invention relates to building materials field, and the expansile method of black cotton regur soil is adjusted more particularly to one kind.
Background technology
For black cotton regur soil as a kind of aquation high-expansion clay, it is in dark brown that its is apparent, is distributed widely in all over the world.Black cotton The main mineral constituent of soil is montmorillonite, is a kind of highly plastic clay, water-swellable, dehydration shrinkage, when the soil body soaks, soil The combination moisture film of particle surface thickens, and grain spacing widens, and causes volumetric expansion.When soil body dehydration, it is thinned with reference to moisture film, Intergranular causes volume-diminished away from diminution.Water swelling, while dehydration shrinkage, mechanical property can be reduced accordingly a lot.Such as: It is located in Africa, eastern region, belongs to dry season and rainy season alternate tropical monsson climate.During dry season, precipitation is few, and black cotton regur soil is in Existing cementing status, intensity is higher, but many crackles occur.During rainy season, the state of plastic-soft modeling can be presented in black cotton regur soil, by force Spend relatively low.Due to this reason, it will bring and have a strong impact on to the building of earth's surface and road construction etc., therefore black cotton regur soil is not Preferably it is directly used in the infrastructure constructions such as ground or roadbed.
To solve this problem, people are made that many trials:A.Maneli et al. is in " Influence of fly ash,ground-granulated blast furnace slag and lime on unconfined compressive In the texts of strength of black cotton soil " one, black cotton regur soil is handled using trade waste to improve its engineering mechanics Performance, wherein trade waste are mainly flyash, blast-furnace cinder and lime, and trade waste, can as black cotton regur soil curing agent To effectively improve the stability of black cotton regur soil, no lateral spacing resistance to compression maximum can reach 2MPa, reach the requirement of ground surface material; J.B.Oza et al. is in " Study of black cotton soil characteristics with cement waste In dust and lime ", black cotton regur soil is handled using waste and old cement and lime, the plasticity index of black cotton regur soil after processing Have with compression strength and largely change, plasticity index is 10% or so, and compression strength maximum can reach 15MPa, reach MU15 classification standard in GB5101-2003.For black cotton regur soil as roadbed material, Zeng Dejian et al. " Ethiopia is black Mentioned in cotton soil engineering characteristic and roadbed treatment technical research " and Wang Tie " talking African Territories black cotton regur soil basement process " To bentonitic processing scheme in highway construction, that is, take and change the method filled out to solve the problems, such as that bentonite is brought, for black cotton Soil area, propose that disposal method is filled out in different changing according to different expansion potentialities;According to different roadbed forms, take different Exchange filling formula.Although changing the Construction Problems filled out and be capable of solving road to a certain extent, being changed the soil that fills out can then make It is stored on specifying place for trade waste, this can bring a series of problem:The soil needs very large area dug out Storage space, turn into a kind of solid waste.
Now, the expansive soil improvement method commonly used both at home and abroad is chemosetting, it is common practice that is mixed in swelled ground solid Agent, it is acted on swelled ground internal particle, so that the water imbibition of the dilatancy of swelled ground and swelled ground can be reduced, carry The engineering property of highly expanded soil, so as to reach the condition of construction needs.At present, the main method of chemosetting, which has, mixes lime, water Mud, flyash etc., wherein incorporation lime and cement are the most universal and practical methods of stabilized expansive soil as curing agent.By surveying Examination, lime etc. are little to the engineering mechanics performance impact of black cotton regur soil, and the sample after processing can not reach engineering mechanics standard.
The content of the invention
The invention provides one kind regulation expansile method of black cotton regur soil to overcome above mentioned problem or solve at least in part Certainly above mentioned problem.
According to an aspect of the invention, there is provided a kind of regulation expansile method of black cotton regur soil, including:
Pretreatment is carried out to black cotton regur soil and obtains black cotton regur soil sample, the pretreatment includes acidification or the pillared processing of sodium;
Silane is hydrolyzed, obtains silane hydrolyzate solution;
Silane Grafted is carried out to black cotton regur soil using the silane hydrolyzate solution, obtains the black cotton regur soil sample of Silane Grafted.
Alternatively, the acidification includes:
The black cotton regur soil is added into H2SO4The first configuration solution is obtained in solution, magnetic agitation 3 is small in 70 DEG C of water-bath When;
It is neutral that the first configuration solution after the stirring, which is washed to pH value, with deionized water;
The first configuration solution after deionized water washing is dried 12 hours at 105 DEG C, obtains the first black cotton Soil sample crude product;
The first black cotton regur soil sample crude product is ground, obtains the first black cotton regur soil sample.
Alternatively, the H2SO4The volume fraction of solution is 7.5%.
Alternatively, the pillared processing of the sodium includes:
Black cotton regur soil is added to Na2CO3The second configuration solution, magnetic agitation 3 hours under normal temperature are obtained in solution;
HCl solution is added into the second configuration solution after the stirring;
The second configuration solution of the addition HCl solution is washed with deionized water, until removing Cl ions;
The second configuration solution after the deionized water is washed is dried 12 hours at 105 DEG C, obtains the examination of the second black cotton regur soil Sample crude product;
The second black cotton regur soil sample crude product is ground, obtains the second black cotton regur soil sample.
Alternatively, the Na2CO3The mass fraction of solution is 8%.
Alternatively, it is described that silane is hydrolyzed, silane hydrolyzate solution is obtained, including:
It is 9 to prepare volume ratio:1 ethanol and the first mixed solution of water;
Silane coupler is added into first mixed solution, with glacial acetic acid by the of the addition silane coupler The pH value of one mixed solution is adjusted to default pH scopes, is stirred, and obtains silane hydrolyzate solution.
Alternatively, the stirring includes:Magnetic agitation 1 hour at normal temperatures.
Alternatively, the default pH value range is 4~5.
Alternatively, it is described that Silane Grafted is carried out to black cotton regur soil using the silane hydrolyzate solution, including:
It is 9 to prepare volume ratio:1 ethanol and the second mixed solution of water;
The black cotton regur soil sample is placed in second mixed solution and is stirred, forms stable suspension;
The silane hydrolyzate solution is instilled in the suspension, the heating water bath preset time at 70 DEG C;
The suspension that instillation after the heating water bath has the silane hydrolyzate solution is washed to neutrality and is dried, Obtain the black cotton regur soil crude product of Silane Grafted;
The black cotton regur soil crude product of the Silane Grafted is ground, obtains the black cotton regur soil sample of Silane Grafted.
Alternatively, the default time includes:2 hours, 4 hours, 8 hours or 12 hours.
The invention provides one kind to adjust the expansile method of black cotton regur soil, and in the present invention, first black cotton regur soil is acidified Processing or the pillared processing of sodium, are obtained after having certain active black cotton regur soil, then silane is hydrolyzed, and obtain hydrolyzed silane solution, It is grafted with the silane of various concentrations, condensation reaction is carried out by the hydroxyl of silane and black cotton regur soil lamella, by black cotton regur soil from parent It is water-based to be changed into hydrophobicity, and then change the water absorption behavior of black cotton regur soil.Due to the particularity of silane molecule structure, i.e. silane point Son is chain structure, and the group at both ends has different hydrophilic and hydrophobics, when being reacted with black cotton regur soil, the meeting of hydrophilic radical one end Condensation reaction occurs with the hydroxyl of black cotton regur soil piece interlayer, hydrophobic one end is then exposed to sheet surfaces, reaches thin using this point Water purpose, and then reduce the dilatancy of black cotton regur soil.By modified black cotton regur soil, the recovery for not only realizing discarded black cotton regur soil is asked Topic, meanwhile, also solve the problems, such as the occupation of land of a large amount of black cotton regur soil.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention, And can be practiced according to the content of specification, and in order to allow above and other objects of the present invention, feature and advantage can Become apparent, below especially exemplified by the embodiment of the present invention.
According to the accompanying drawings will be brighter to the detailed description of the specific embodiment of the invention, those skilled in the art Above-mentioned and other purposes, the advantages and features of the present invention.
Brief description of the drawings
By reading the detailed description of hereafter preferred embodiment, it is various other the advantages of and benefit it is common for this area Technical staff will be clear understanding.Accompanying drawing is only used for showing the purpose of preferred embodiment, and is not considered as to the present invention Limitation.And in whole accompanying drawing, identical part is denoted by the same reference numerals.In the accompanying drawings:
Fig. 1 is the expansile method flow schematic diagram of regulation black cotton regur soil according to embodiments of the present invention;
Fig. 2 is the XRD of the black cotton regur soil sample by different modes processing according to embodiments of the present invention.
Embodiment
The exemplary embodiment of the disclosure is more fully described below with reference to accompanying drawings.Although the disclosure is shown in accompanying drawing Exemplary embodiment, it being understood, however, that may be realized in various forms the disclosure without should be by embodiments set forth here Limited.On the contrary, these embodiments are provided to facilitate a more thoroughly understanding of the present invention, and can be by the scope of the present disclosure Completely it is communicated to those skilled in the art.
Fig. 1 be the expansile method flow schematic diagram of regulation black cotton regur soil that provides according to embodiments of the present invention as shown in figure 1, The expansile method of regulation black cotton regur soil provided according to embodiments of the present invention includes:
Step S102, pretreatment is carried out to black cotton regur soil and obtains black cotton regur soil sample, wherein, pretreatment includes acidification or sodium Pillared processing;
Step S104, silane is hydrolyzed, and obtains silane hydrolyzate solution;
Step S106, Silane Grafted is carried out to the surface of pretreated black cotton regur soil using silane hydrolyzate solution, obtains silicon The black cotton regur soil sample of alkane grafting.
The embodiments of the invention provide one kind to adjust the expansile method of black cotton regur soil, in embodiments of the present invention, first to black Cotton soil carries out acidification or the pillared processing of sodium, then silane is hydrolyzed, and obtains hydrolyzed silane solution, and then use silane hydrolyzate Liquid carries out Silane Grafted to the surface of black cotton regur soil.Due to the particularity of silane molecule structure, i.e. silane molecule is chain structure, two The group at end has different hydrophilic and hydrophobics, and when being reacted with black cotton regur soil, hydrophilic radical one end can be with black cotton regur soil piece interlayer Hydroxyl condensation reaction occurs, hydrophobic one end then be exposed to sheet surfaces, reaches hydrophobic purpose, and then reduction using this point The dilatancy of black cotton regur soil.By modified black cotton regur soil, the recovery problem of discarded black cotton regur soil is not only realized, meanwhile, also solve The occupation of land problems of a large amount of black cotton regur soil.
Black cotton regur soil is a kind of tropical soil being distributed widely in all over the world, has strong hydration swelling, unsuitable straight Connect and be used for roadbed construction.Black cotton regur soil used in the present invention is Kenya Nairobi south loop wire highway department soil, through analysis:The black cotton regur soil The mineral facies such as montmorillonite, feldspar and quartz are mainly contained, black cotton regur soil is a kind of high hydration swelling soil, is by SEM observations A kind of lamellar structure, contain substantial amounts of hydroxyl between black cotton regur soil lamella, and black cotton regur soil lamella carries negative electricity, is easy to adsorb in water Aquation cation, form double electrical layerses.
When carrying out acidification to black cotton regur soil, black cotton regur soil first can be added into H2SO4First is obtained in (sulfuric acid) solution to match somebody with somebody Solution is put, magnetic agitation 3 hours in 70 DEG C of water-bath, wherein, preferred volume fraction is 7.5% H2SO4Solution;Secondly, use It is neutrality that deionized water is washed to pH value to the first configuration solution after stirring;First after deionized water is washed is matched somebody with somebody again Put solution to dry 12 hours at 105 DEG C, obtain the first black cotton regur soil sample crude product;Finally, the first black cotton regur soil sample crude product is carried out Grinding, obtain the first black cotton regur soil sample.
When to the pillared processing of black cotton regur soil progress sodium, black cotton regur soil first can be added to Na2CO3Obtained in (sodium carbonate) solution The second configuration solution, magnetic agitation 3 hours under normal temperature, wherein, preferred mass fraction is 8%Na2CO3Solution;Next, to HCl solution is added in the second configuration solution after stirring;The the second configuration solution for adding HCl solution is carried out with deionized water again Washing, until removing Cl ions;The second configuration solution after deionized water is washed again is dried 12 hours at 105 DEG C, obtains the Two black cotton regur soil sample crude products;Finally, the second black cotton regur soil sample crude product is ground, obtains the second black cotton regur soil sample.
Preferably, it is hydrolyzed to silane, can be according to following steps when obtaining silane hydrolyzate solution:
It is 9 to prepare volume ratio:1 ethanol and the first mixed solution of water;Silane coupler is added molten to the first mixing In liquid, the pH value for the first mixed solution for adding silane coupler is adjusted to default pH scopes with glacial acetic acid, is stirred, Obtain silane hydrolyzate solution.
Wherein, default pH ranges preferably from 4~5, within this range, contributes to the hydrolysis of silane coupler.And entering , can be in magnetic agitation 1 hour at normal temperatures during row stirring.
Difference black cotton regur soil described above and the processing procedure of hydrolyzed silane solution, in embodiments of the present invention, mainly Using the structural particularity that silane molecule is chain structure, black cotton regur soil dilatancy is reduced using silane coupler.Therefore, using silicon Alkane hydrating solution is particularly important to carrying out Silane Grafted by pretreated black cotton regur soil.
In embodiments of the present invention, carrying out surface grafting to black cotton regur soil using silane hydrolyzate solution can include:
It is 9 to prepare volume ratio:1 ethanol and the second mixed solution of water;
The above-mentioned black cotton regur soil sample by pretreatment is placed in the second mixed solution and is stirred, forms stable suspension Liquid;
Silane hydrolyzate solution is instilled in suspension, the heating water bath preset time at 70 DEG C;
The suspension that instillation after heating water bath has the silane hydrolyzate solution is washed to neutrality and is dried, is obtained The black cotton regur soil crude product of Silane Grafted;
The black cotton regur soil crude product of Silane Grafted is ground, obtains the black cotton regur soil sample of Silane Grafted.
Alternatively, by silane hydrolyzate solution instill after suspension the heating water bath time at 70 DEG C can be 2 hours, it is 4 small When, 8 hours or 12 hours.
The regulation expansile method of black cotton regur soil provided in an embodiment of the present invention, mainly by being acidified to black cotton regur soil or sodium Change pretreatment, be 3- aminopropyl trimethoxysilanes to black using silane coupler after obtaining the black cotton regur soil with certain activity Cotton soil carries out surface modification, is grafted with the silane of various concentrations, is condensed by the hydroxyl of silane and black cotton regur soil lamella Reaction, black cotton regur soil is changed into hydrophobicity from hydrophily, and then changes the water absorption behavior of black cotton regur soil.Due to silane molecule structure Particularity, silane molecule is chain structure, and the group at both ends has different hydrophilic and hydrophobics, reacted with black cotton regur soil When, with the hydroxyl of black cotton regur soil piece interlayer condensation reaction can occur for hydrophilic radical one end, and hydrophobic one end is then exposed to sheet surfaces, Reach hydrophobic purpose using this point, and then reduce the dilatancy of black cotton regur soil.By modified black cotton regur soil, not only realize useless The recovery problem of black cotton regur soil is abandoned, meanwhile, also solve the problems, such as the occupation of land of a large amount of black cotton regur soil.
The technical scheme provided based on above-described embodiment, black cotton regur soil progress silane surface is connect present invention also offers multiple The embodiment of branch, and carried out dilatancy test.
In order to facilitate contrast, Silane Grafted first can be directly carried out to former black cotton regur soil, and without pretreatment, such as following realities Apply a 1-3.
Embodiment 1
Former black cotton regur soil directly carries out Silane Grafted
1. the hydrolysis of silane:The silane coupler that volume fraction is 0.5% is added to 100mL ethanol/water (volume ratio For 9:1) in mixed solution, pH value is adjusted between 4-5 with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
2. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100ml ethanol/waters (volume ratio 9:1) mixed solution In, it is put in beaker and stirs, wait to be uniformly dispersed, forms stable suspension, solution of silane is slowly dropped into suspension.70 DEG C water-bath 4 hours.After question response terminates, filter, wash to neutrality, 80 DEG C of oven dryings 12 hours;Mortar grinder is standby, obtains The black cotton regur soil sample of Silane Grafted.
Free swelling rate is 120% after measured.
Embodiment 2
Former black cotton regur soil directly carries out Silane Grafted
1. the hydrolysis of silane:The silane coupler that volume fraction is 1% is added to 100mL ethanol/waters (volume ratio 9: 1) in mixed solution, pH value is adjusted between 4-5 with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
2. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension, 70 DEG C of water-baths 4 hours;After reaction terminates, filter, washing to neutrality, dried 12 hours in 80 DEG C of baking ovens, it is standby that mortar is levigate, obtains To the black cotton regur soil sample of Silane Grafted.
Free swelling rate is 61% after measured.
Embodiment 3
Former black cotton regur soil directly carries out Silane Grafted
1. the hydrolysis of silane:The silane coupler that volume fraction is 2% is added to 100mL ethanol/waters (volume ratio 9: 1) in mixed solution, pH value is adjusted between 4-5 with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
2. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension, 70 DEG C of water-baths 4 hours;After reaction terminates, filter, washing to neutrality, dried 12 hours in 80 DEG C of baking ovens, it is standby that mortar is levigate, obtains To the black cotton regur soil sample of Silane Grafted.
Free swelling rate is 41% after measured.
Following examples can be pre-processed black cotton regur soil, then carry out Silane Grafted.
Embodiment 4
1. pair black cotton regur soil carries out acidification, the H that volume fraction is 7.5% is added into 15g black cotton regur soil2SO4In solution, The solution configured is put in magnetic agitation 3 hours in 70 DEG C of water-bath;Filtered, washed with deionized water afterwards, until filtrate PH value is neutrality, is put into the drying 12 hours of 105 DEG C of baking oven;It is standby that mortar is levigate;
2. the hydrolysis of silane:The silane coupler that volume fraction is 0.5% is added into 100mL ethanol/waters, and (volume ratio is 9:1) in mixed solution, it is 4-5 to adjust pH value with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension, 70 DEG C of water-baths 4 hours.After reaction terminates, filter, wash to solution in neutrality, be put into baking oven 80 DEG C of dryings 12 hours, mortar It is levigate standby, obtain the black cotton regur soil sample of Silane Grafted.
Free swelling rate is 17% after measured.
Embodiment 5
1. pair black cotton regur soil carries out acidification, the H that volume fraction is 7.5% is added into 15g black cotton regur soil2SO4In solution, The solution configured is put in magnetic agitation 3 hours in 70 DEG C of water-bath;Solution after stirring is washed with deionized, until PH value is neutrality, is put into the drying 12 hours of 105 DEG C of baking oven;It is standby that mortar is levigate;
2. the hydrolysis of silane:The silane coupler that volume fraction is 1% is added to 100mL ethanol/waters (volume ratio 9: 1) in mixed solution, it is 4-5 to adjust pH value with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension. 70 DEG C of water-baths 4 hours.After question response terminates, filter, wash to neutrality, be put into baking oven 80 DEG C of dryings 12 hours, mortar is levigate It is standby, obtain the black cotton regur soil sample of Silane Grafted.
Its free swelling rate is 10% after measured.
Embodiment 6
1. pair black cotton regur soil carries out acidification, the H that volume fraction is 7.5% is added into 15g black cotton regur soil2SO4In solution, The solution configured is put in magnetic agitation 3 hours in 70 DEG C of water-bath;Solution after stirring is washed with deionized, until PH value is neutrality, is put into the drying 12 hours of 105 DEG C of baking oven;It is standby that mortar is levigate;
2. the hydrolysis of silane:The silane coupler that volume fraction is 2% is added to 100mL ethanol/waters (volume ratio 9: 1) in mixed solution, it is 4-5 to adjust pH value with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension. 70 DEG C of water-baths 4 hours.After question response terminates, filter, wash to neutrality, be put into baking oven 80 DEG C of dryings 12 hours, mortar is levigate It is standby, obtain the black cotton regur soil sample of Silane Grafted.
Its free swelling rate is 13% after measured.
Embodiment 7
1. pair black cotton regur soil carries out acidification, the H that volume fraction is 7.5% is added into 15g black cotton regur soil2SO4In solution, The solution configured is put in magnetic agitation 3 hours in 70 DEG C of water-bath;Solution after stirring is washed with deionized, until PH value is neutrality, is put into the drying 12 hours of 105 DEG C of baking oven;It is standby that mortar is levigate;
2. the hydrolysis of silane:The silane coupler that volume fraction is 1% is added to 100mL ethanol/waters (volume ratio 9: 1) in mixed solution, it is 4-5 to adjust pH value with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension. 70 DEG C of water-baths 2 hours.After question response terminates, filter, wash to neutrality, be put into baking oven 80 DEG C of dryings 12 hours, mortar is levigate It is standby, obtain the black cotton regur soil sample of Silane Grafted.
Its free swelling rate is 30% after measured.
Embodiment 8
1. pair black cotton regur soil carries out acidification, the H that volume fraction is 7.5% is added into 15g black cotton regur soil2SO4In solution, The solution configured is put in magnetic agitation 3 hours in 70 DEG C of water-bath;Solution after stirring is washed with deionized, until PH value is neutrality, is put into the drying 12 hours of 105 DEG C of baking oven;It is standby that mortar is levigate;
2. the hydrolysis of silane:The silane coupler that volume fraction is 1% is added to 100mL ethanol/waters (volume ratio 9: 1) in mixed solution, it is 4-5 to adjust pH value with glacial acetic acid, promotes to hydrolyze, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, magnetic agitation in beaker is put in, waits to be uniformly dispersed, stable suspension is formed, solution of silane is slowly dropped into suspension. 70 DEG C of water-baths 8 hours.After question response terminates, filter, wash to neutrality, be put into baking oven 80 DEG C of dryings 12 hours, mortar is levigate It is standby, obtain the black cotton regur soil sample of Silane Grafted.
Its free swelling rate is 13% after measured
Embodiment 9
It is pillared that 1. pair black cotton regur soil carries out sodium:Black cotton regur soil is added in the sodium carbonate liquor that mass fraction is 8%, normal temperature magnetic Power stirs 3 hours;HCl solution is added thereto, removes unnecessary CO3 2-.Suspension is filtered with deionized water, washed, until removing Remove Cl-;105 DEG C of dryings 12 hours in baking oven, buck is standby;
2. the hydrolysis of silane:The silane coupler that volume fraction is 0.5% is added to 100mL ethanol/water (volume ratio For 9:1) it is 4-5 with glacial acetic acid regulation pH value in mixed solution, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, it is put in beaker and stirs, wait to be uniformly dispersed, forms stable suspension, solution of silane is slowly dropped into suspension.70℃ Water-bath 4 hours.After question response terminates, filter, wash to neutrality, 80 DEG C of dryings 12 hours are levigate, obtain the black cotton of Silane Grafted Earth sample.
Its free swelling rate is 60% after measured.
Embodiment 10
It is pillared that 1. pair black cotton regur soil carries out sodium:Black cotton regur soil is added in the sodium carbonate liquor that mass fraction is 8%, normal temperature magnetic Power stirs 3 hours;HCl solution is added thereto, removes unnecessary CO3 2-.Suspension is filtered with deionized water, washed, until removing Remove Cl-;105 DEG C of dryings 12 hours in baking oven, buck is standby;
2. the hydrolysis of silane:The silane coupler that volume fraction is 1% is added into 100mL ethanol/water, and (volume ratio is 9:1) it is 4-5 with glacial acetic acid regulation pH value in mixed solution, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, it is put in beaker and stirs, wait to be uniformly dispersed, forms stable suspension, solution of silane is slowly dropped into suspension.70℃ Water-bath 4 hours.After question response terminates, filter, wash to neutrality, 80 DEG C of dryings 12 hours are levigate, obtain the black cotton of Silane Grafted Earth sample.
Its free swelling rate is 38% after measured.
Embodiment 11
It is pillared that 1. pair black cotton regur soil carries out sodium:Black cotton regur soil is added in the sodium carbonate liquor that mass fraction is 8%, normal temperature magnetic Power stirs 3 hours;HCl solution is added thereto, removes unnecessary CO3 2-.Suspension is filtered with deionized water, washed, until removing Remove Cl-;105 DEG C of dryings 12 hours in baking oven, buck is standby;
2. the hydrolysis of silane:The silane coupler that volume fraction is 2% is added into 100mL ethanol/water, and (volume ratio is 9:1) it is 4-5 with glacial acetic acid regulation pH value in mixed solution, magnetic agitation 1 hour under normal temperature.
3. the surface grafting of black cotton regur soil:15g black cotton regur soil is scattered in 100mL ethanol/waters (volume ratio 9:1) mixed solution In, it is put in beaker and stirs, wait to be uniformly dispersed, forms stable suspension, solution of silane is slowly dropped into suspension.70℃ Water-bath 4 hours.After question response terminates, filter, wash to neutrality, 80 DEG C of dryings 12 hours are levigate, obtain the black cotton of Silane Grafted Earth sample.
Its free swelling rate is 40% after measured.
Contrasted by above-described embodiment, in embodiment 1-3, it is pre- without doing that directly former black cotton regur soil carries out Silane Grafted During processing, then after preparing surface progress Silane Grafted of the lower silane hydrolyzate solution to black cotton regur soil based on different condition, black cotton regur soil Expansion rate it is still very high.And after black cotton regur soil is carried out into acidification or the pillared processing of sodium, then to black cotton regur soil after treatment Silane Grafted is carried out, the expansion rate of black cotton regur soil is decreased obviously.
Fig. 2 is the black cotton regur soil sample XRD (X-ray handled by different modes according to the embodiment of the present invention Diffraction, X-ray diffraction) collection of illustrative plates, as shown in Fig. 2 a represents the XRD of undressed black cotton regur soil;B is represented through volume Fraction is the black cotton regur soil sample of 1%Silanes (silane) grafting;It through volume fraction is 7.5%H that c, which is,2SO4Solution acidification, And carry out being grafted black cotton regur soil sample using the silane coupler that volume fraction is 1%;D represent through mass fraction as 8% carbonic acid The pillared processing of sodium solution sodium, and carry out being grafted black cotton regur soil sample using the silane coupler that volume fraction is 1%.Wherein, 1.50nm, 1.64nm, 1.74nm, 1.66nm are the interplanar distance of the first order diffraction maximum of montmorillonite in corresponding sample respectively.
It can be seen that the XRD of modified black cotton regur soil first order diffraction maximum skew, shows that silane molecule enters Clay interlayer.
Table 1 is the FS (free swelling ratio, free swelling rate) of modified black cotton regur soil with the change of modified condition Change.
Table 1
FS (%) BCS+Silanes 8%Na2CO3+Silanes 7.5%H2SO4+Silanes
0.5%Silanes 120 60 17
1%Silanes 61 38 10
2%Silanes 41 40 13
FS represents free swelling rate;Silanes represents silane;BCS represents Black Cotton Soil, i.e. black cotton regur soil;Its In, the water bath time using silane treatment black cotton regur soil is 4 hours.
After measured, former BCS free swelling rates are 160%.
It is observed that from table 1:The expansion rate of black cotton regur soil after acidified processing or the pillared processing of sodium can reduce.
Further, through H2SO4Pretreated black cotton regur soil dilatancy reduces more notable, and its free swelling rate is from original 160% be down to 10%.Using Na2CO3The pillared processing of sodium is carried out to black cotton regur soil, simply Na+By Ca in black cotton regur soil lamella2+Deng from Son cements out, and sulfuric acid treatment can remove the organic matter being distributed in black cotton regur soil;H+Also can be by the Al in octahedron3+Deng from Sub- dissolution, make the more negative electrical charges of clay particle band;Pickling can also produce substantial amounts of scission of link;Increase the reactivity of black cotton regur soil, It is easier to the absorption of silane.Therefore, compared to H2SO4Black cotton regur soil is pre-processed, uses Na2CO3Pretreated black cotton regur soil Dilatancy reduces more notable.
In the specification that this place provides, numerous specific details are set forth.It is to be appreciated, however, that the implementation of the present invention Example can be put into practice in the case of these no details.In some instances, known method, structure is not been shown in detail And technology, so as not to obscure the understanding of this description.
Similarly, it will be appreciated that in order to simplify the disclosure and help to understand one or more of each inventive aspect, Above in the description to the exemplary embodiment of the present invention, each feature of the invention is grouped together into single implementation sometimes In example, figure or descriptions thereof.However, the method for the disclosure should be construed to reflect following intention:I.e. required guarantor The application claims of shield features more more than the feature being expressly recited in each claim.It is more precisely, such as following Claims reflect as, inventive aspect is all features less than single embodiment disclosed above.Therefore, Thus the claims for following embodiment are expressly incorporated in the embodiment, wherein each claim is in itself Separate embodiments all as the present invention.
In addition, it will be appreciated by those of skill in the art that although some embodiments described herein include other embodiments In included some features rather than further feature, but the combination of the feature of different embodiments means in of the invention Within the scope of and form different embodiments.For example, in detail in the claims, embodiment claimed it is one of any Mode it can use in any combination.
So far, although those skilled in the art will appreciate that detailed herein have shown and described multiple showing for the present invention Example property embodiment, still, still can be direct according to present disclosure without departing from the spirit and scope of the present invention It is determined that or derive many other variations or modifications for meeting the principle of the invention.Therefore, the scope of the present invention is understood that and recognized It is set to and covers other all these variations or modifications.

Claims (10)

1. one kind regulation expansile method of black cotton regur soil, including:
Pretreatment is carried out to black cotton regur soil and obtains black cotton regur soil sample, wherein, the pretreatment includes acidification or the pillared processing of sodium;
Silane is hydrolyzed, obtains silane hydrolyzate solution;
Silane Grafted is carried out to the pretreated black cotton regur soil using the silane hydrolyzate solution, obtains the black cotton of Silane Grafted Earth sample.
2. according to the method for claim 1, wherein, the acidification includes:
The black cotton regur soil is added into H2SO4The first configuration solution, magnetic agitation 3 hours in 70 DEG C of water-bath are obtained in solution;
It is neutral that the first configuration solution after the stirring, which is washed to pH value, with deionized water;
The first configuration solution after deionized water washing is dried 12 hours at 105 DEG C, obtains the examination of the first black cotton regur soil Sample crude product;
The first black cotton regur soil sample crude product is ground, obtains the first black cotton regur soil sample.
3. the method according to claim 11, wherein, the H2SO4The volume fraction of solution is 7.5%.
4. according to the method for claim 1, wherein, the pillared processing of sodium includes:
Black cotton regur soil is added to Na2CO3The second configuration solution, magnetic agitation 3 hours under normal temperature are obtained in solution;
HCl solution is added into the second configuration solution after the stirring;
The second configuration solution of the addition HCl solution is washed with deionized water, until removing Cl ions;
The second configuration solution after the deionized water is washed is dried 12 hours at 105 DEG C, and it is thick to obtain the second black cotton regur soil sample Product;
The second black cotton regur soil sample crude product is ground, obtains the second black cotton regur soil sample.
5. the method according to claim 11, wherein, the Na2CO3The mass fraction of solution is 8%.
6. the method according to claim 11, wherein, it is described that silane is hydrolyzed, silane hydrolyzate solution is obtained, including:
It is 9 to prepare volume ratio:1 ethanol and the first mixed solution of water;
Silane coupler is added into first mixed solution, mixed with glacial acetic acid by the first of the addition silane coupler The pH value for closing solution is adjusted to default pH scopes, is stirred, and obtains silane hydrolyzate solution.
7. according to the method for claim 6, wherein, the default pH value range is 4~5.
8. according to the method for claim 6, wherein, the stirring includes:Magnetic agitation 1 hour at normal temperatures.
9. the method according to claim 11, wherein, it is described that black cotton regur soil progress silane is connect using the silane hydrolyzate solution Branch, including:
It is 9 to prepare volume ratio:1 ethanol and the second mixed solution of water;
The black cotton regur soil sample is placed in second mixed solution and is stirred, forms stable suspension;
The silane hydrolyzate solution is instilled in the suspension, the heating water bath preset time at 70 DEG C;
The suspension that instillation after the heating water bath has the silane hydrolyzate solution is washed to neutrality and is dried, is obtained The black cotton regur soil crude product of Silane Grafted;
The black cotton regur soil crude product of the Silane Grafted is ground, obtains the black cotton regur soil sample of Silane Grafted.
10. according to the method for claim 9, wherein, the default time includes:2 hours, 4 hours, 8 hours or 12 Hour.
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