CN114085059A - Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof - Google Patents

Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof Download PDF

Info

Publication number
CN114085059A
CN114085059A CN202111491044.5A CN202111491044A CN114085059A CN 114085059 A CN114085059 A CN 114085059A CN 202111491044 A CN202111491044 A CN 202111491044A CN 114085059 A CN114085059 A CN 114085059A
Authority
CN
China
Prior art keywords
wood
cement
nano
grouting material
parts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111491044.5A
Other languages
Chinese (zh)
Other versions
CN114085059B (en
Inventor
吴疆宇
尹乾
刘日成
马丹
蔚立元
姬永生
王逸鸣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China University of Mining and Technology CUMT
Original Assignee
China University of Mining and Technology CUMT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China University of Mining and Technology CUMT filed Critical China University of Mining and Technology CUMT
Priority to CN202111491044.5A priority Critical patent/CN114085059B/en
Publication of CN114085059A publication Critical patent/CN114085059A/en
Application granted granted Critical
Publication of CN114085059B publication Critical patent/CN114085059B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions 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
    • C04B28/04Portland cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/04Silica-rich materials; Silicates
    • C04B14/06Quartz; Sand
    • C04B14/062Microsilica, e.g. colloïdal silica
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/02Treatment
    • C04B20/023Chemical treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2623Polyvinylalcohols; Polyvinylacetates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/38Polysaccharides or derivatives thereof
    • C04B24/383Cellulose or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00008Obtaining or using nanotechnology related materials
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/70Grouts, e.g. injection mixtures for cables for prestressed concrete
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Abstract

The invention discloses a wood nano-cellulose-nano-cement modified grouting material for reinforcing deep-ground engineering surrounding rock and a preparation method thereof, belonging to the technical field of grouting materials. The grouting material comprises the following raw materials in parts by mass: 30-45 parts of cement, 0.1-0.3 part of sodium carbonate, 4-8 parts of fly ash, 0.03-0.07 part of wood nano-cellulose, 10-15 parts of silica gel and 8-13 parts of polyvinyl alcohol. The invention utilizes the interaction between the wood nano-cellulose and the cement, the silica gel and the polyvinyl alcohol and the cement, and the sodium carbonate and the cement to prepare the grouting material with good performance.

Description

Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof
Technical Field
The invention belongs to the technical field of grouting materials, and particularly relates to a wood nano-cellulose-nano-cement modified grouting material for reinforcing deep-ground engineering surrounding rock and a preparation method thereof.
Background
The cement-based material has unique characteristics such as low manufacturing cost, high pressure resistance, strong durability and the like, and is one of the most widely applied building materials in the current building material industry. The coal mine tunnel is a transportation channel for coal mining, but surrounding rocks of the deep tunnel deform and break under high ground stress and strong mining disturbance, so that a loose broken structure is easily formed, a large number of micron or even nanometer-scale micro cracks develop inside the tunnel, and once slight disturbance occurs, the tunnel can generate disasters such as large deformation caving, roof collapse and the like, so that life and property safety are threatened, and therefore, rock mass containing cracks needs to be reinforced.
The grouting material refers to a main substance which plays a role in filling and consolidating in formation cracks and pores and is key to realizing the water plugging or strengthening effect. Currently, grouting materials can be mainly classified into cement grouting materials and chemical grouting materials. The cement grouting material comprises cement paste, cement clay paste, cement-water glass paste and the like. Although the cement grouting material has the advantages of rich raw material sources, low price, high strength of the stone body and the like, the cement grouting material has the defects of thick particle size, difficulty in injecting micro cracks in the rock body, long initial setting and final setting time, difficulty in accurate control, poor stability, low strength increasing speed, high water precipitation rate and the like, and has the phenomena of poor injectability in a small-pore stratum and the like.
In recent years, in the fields of civil engineering science and application, research work on improving the performance of cement-based grouting materials is always explored, for example, the physical and chemical properties of the cement-based composite grouting materials are intelligently controlled by reinforcing the cement-based composite materials by using nano materials. However, most of the nano materials have the defects of difficult dispersion, easy agglomeration and the like, and a large amount of surfactant or water reducing agent needs to be added in the using process or ultrasonic dispersion treatment is carried out for a long time, so that the cost is continuously increased, the working efficiency is greatly reduced, and even some nano materials easy to agglomerate not only increase the cost input, but also reduce the material strength.
Disclosure of Invention
In view of the above, the invention provides a wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and a preparation method thereof, so as to solve the technical problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the first technical scheme is as follows: a wood nano cellulose-nano cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following raw materials in parts by mass:
30-45 parts of cement, 0.1-0.3 part of sodium carbonate, 4-8 parts of fly ash, 0.03-0.07 part of wood nano-cellulose, 10-15 parts of silica gel and 8-13 parts of polyvinyl alcohol.
Further, the lignocellulose is lignocellulose nano-cellulose filaments with the diameter of 5-20nm, the length of 1-3um and the length-diameter ratio of 50-300; the nano cement is cement particles with the particle size of 10-200 nm.
Further, the raw material of the lignocellulose is lignocellulose, and the preparation method of the lignocellulose comprises the following steps: (1) soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; (2) adding citric acid-sodium citrate buffer solution into the slurry, heating and stirring; (3) then adding enzyme solution for enzymolysis, heating to 95 deg.C for 30min for enzyme deactivation, washing, centrifuging, and balancing water content to obtain lignocellulose.
Further, the waste wood includes wood, straw or pulp; the heating and stirring temperature is 45 ℃, and the stirring speed is 250 r/min.
Further, the enzyme solution is a mixed solution of endoglucanase and laccase, the dosage of the endoglucanase is 10IU/g, and the dosage of the laccase is 20 IU/g.
Further, the mass ratio of the slurry to the enzyme solution is 1: (0.03-0.05).
The second technical scheme is as follows: a preparation method of a wood nanocellulose-nanometer cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following steps:
(1) weighing raw materials according to mass, adding water to dilute lignocellulose, and then carrying out high-pressure homogenization treatment to obtain lignocellulose pulp;
(2) sequentially adding fly ash, sodium carbonate, silica gel, polyvinyl alcohol and wood nano-cellulose slurry into cement, wet grinding, and continuously carrying out high-pressure homogenization treatment to obtain the wood nano-cellulose-nano-cement modified grouting material.
Further, the mass fraction of the wood nano-fibers in the wood nano-cellulose pulp is 0.04-0.08%.
Further, the pressure in the high-pressure homogenizing process is 30-40MPa, and the circulation is carried out for 15-20 times.
Further, the wet milling is specifically as follows: grinding for 2-3h at the rotation speed of 2000-. The cement grain size is 10-200nm after two times of wet grinding treatment under high-speed rotation.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the wood nanocellulose and the cement are mixed, the nanocement is coated on the surface of the wood nanocellulose to perform hydration reaction, the large length-diameter ratio of the wood nanocellulose can play a role in bridging micro cracks, the hydration time is short, and the cementing matrix formed by coating staggered wood nanocellulose with a hydration product has high strength, so that the strength of the grouting material is enhanced. The method strictly controls the content of the lignocellulose to ensure the continuous hydration reaction of the cement, and controls the size of the cement to make the lignocellulose and the cement complement each other, so that the defects of monomer raw materials are avoided, and the beneficial effect is maximized.
According to the invention, silica gel and polyvinyl alcohol are added into the grouting material, and the silica gel and polyvinyl alcohol react with cement hydration products to form an interface structure combined by chemical bonds, so that the water-cement ratio is improved, and the compressive strength and durability of the grouting material are improved. The sodium carbonate reacts with calcium ions in the cement to generate calcium carbonate, so that the porosity of the grouting material can be reduced, the compactness is improved, and the mechanical property of the grouting material is further improved.
The method utilizes the combination of endoglucanase and laccase to modify the lignocellulose, promotes the closer combination of hydrogen bonds between the celluloses by reasonably controlling the dosage of enzyme solution and the enzymolysis time, reduces amorphous areas, improves the dispersibility of the lignocellulose, ensures that the lignocellulose is not easy to agglomerate, and reduces the use of dispersing agents and water reducing agents.
The invention uses waste wood as raw material, not only reasonably utilizes resources, but also greatly improves the mechanical property of the original cement after being compounded with the conventional cement and processed by wet grinding and high-pressure homogenization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic diagram of high-speed wet milling of enzyme treated ligno-nanocellulose and cement.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
A wood nano cellulose-nano cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following raw materials in parts by mass:
30-45 parts of cement, 0.1-0.3 part of sodium carbonate, 4-8 parts of fly ash, 0.03-0.07 part of wood nano-cellulose, 10-15 parts of silica gel and 8-13 parts of polyvinyl alcohol.
The wood nanocellulose is wood nanocellulose filaments with the diameter of 5-20nm, the length of 1-3um and the length-diameter ratio of 50-300; the nano cement is cement particles with the particle size of 10-200 nm.
The raw material of the lignocellulose is lignocellulose, and the preparation method of the lignocellulose comprises the following steps: (1) soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; (2) adding citric acid-sodium citrate buffer solution into the slurry, heating and stirring; (3) then adding enzyme solution for enzymolysis, heating to 95 ℃ for enzyme deactivation treatment for 30min, washing, centrifuging, balancing water, and freeze drying to obtain the lignocellulose.
The waste wood comprises wood, straw or pulp; the heating and stirring temperature is 45 ℃, and the stirring speed is 250 r/min.
The enzyme solution is a mixed solution of endoglucanase and laccase, the dosage of the endoglucanase is 10IU/g, and the dosage of the laccase is 20 IU/g.
The mass ratio of the slurry to the enzyme solution is 1: (0.03-0.05).
A preparation method of a wood nanocellulose-nanometer cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following steps:
(1) weighing raw materials according to mass, adding water to dilute lignocellulose, and then carrying out high-pressure homogenization treatment to obtain lignocellulose pulp;
(2) sequentially adding fly ash, sodium carbonate, silica gel, polyvinyl alcohol and wood nano-cellulose slurry into cement, wet grinding, and continuously carrying out high-pressure homogenization treatment to obtain the wood nano-cellulose-nano-cement modified grouting material.
The mass fraction of the wood nano-fiber in the wood nano-cellulose pulp is 0.04-0.08%.
The pressure in the high-pressure homogenizing process is 30-40MPa, and the circulation is carried out for 15-20 times.
The wet milling is specifically as follows: grinding for 2-3h at the rotation speed of 2000-. The cement grain size is 10-200nm after two times of wet grinding treatment under high-speed rotation.
The "parts" described in the following examples are all "parts by mass".
The cement used in the invention comprises the following components in parts by mass: 23-25% SiO2,5-8%Al2O3,54-60%CaO,3-5%Fe2O3And 4-10% of the rest substances.
The cement used in the invention is 32.5 cement.
In the following examples, the diameter of the wood nano-cellulose is 5-20nm, the length is 1-3um, the length-diameter ratio is 50-300, and the particle size of lime is 10-200 nm.
Example 1
A wood nano cellulose-nano cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following raw materials in parts by mass:
40 parts of cement, 0.2 part of sodium carbonate, 6 parts of fly ash, 0.05 part of wood nano-cellulose, 13 parts of silica gel and 10 parts of polyvinyl alcohol.
The preparation method comprises the following steps:
(1) preparing lignocellulose: soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; adding 0.04mol/L citric acid-sodium citrate buffer solution (pH6.2) into the slurry, heating and stirring at 45 deg.C with stirring rate of 250 r/min; then adding a mixed solution of endoglucanase and laccase for enzymolysis for 1.5h (the dosage of the endoglucanase is 10IU/g, the dosage of the laccase is 20IU/g), wherein the mass ratio of the pulp to the enzyme solution is 1: 0.04. heating to 95 deg.C, inactivating enzyme for 30min, washing, centrifuging, and balancing water to obtain lignocellulose.
(2) Diluting lignocellulose with water, performing high-pressure homogenization treatment under the condition that the pressure is 35MPa, and circulating for 18 times to obtain lignocellulose pulp; wherein, the adding amount of the water is based on that the mass fraction of the wood fiber in the wood nano-cellulose pulp is 0.06 percent.
(3) Sequentially adding fly ash, sodium carbonate, silica gel, polyvinyl alcohol and wood nano-cellulose pulp into cement, grinding for 2.5h at the rotating speed of 2200r/min, then grinding for 1.5h at the rotating speed of 2800r/min, finally continuing high-pressure homogenization treatment under the condition of 35MPa of pressure, and circulating for 15 times to obtain the wood nano-cellulose-nano-cement modified grouting material.
Example 2
A wood nano cellulose-nano cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following raw materials in parts by mass:
30 parts of cement, 0.1 part of sodium carbonate, 6 parts of fly ash, 0.03 part of lignocellulose, 15 parts of silica gel and 13 parts of polyvinyl alcohol.
The preparation method comprises the following steps:
(1) preparing lignocellulose: soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; adding 0.04mol/L citric acid-sodium citrate buffer solution (pH6.2) into the slurry, heating and stirring at 45 deg.C with stirring rate of 250 r/min; then adding a mixed solution of endoglucanase and laccase for enzymolysis for 1.5h (the dosage of the endoglucanase is 10IU/g, the dosage of the laccase is 20IU/g), wherein the mass ratio of the pulp to the enzyme solution is 1: 0.03. heating to 95 deg.C, inactivating enzyme for 30min, washing, centrifuging, and balancing water to obtain lignocellulose.
(2) Diluting lignocellulose with water, performing high-pressure homogenization treatment under the pressure of 40MPa, and circulating for 15 times to obtain lignocellulose pulp; wherein the adding amount of the water is based on that the mass fraction of the wood fiber in the wood nano-cellulose pulp is 0.04%.
(3) Sequentially adding fly ash, sodium carbonate, silica gel, polyvinyl alcohol and wood nano-cellulose pulp into cement, grinding for 2h at the rotating speed of 2300r/min, then grinding for 2h at the rotating speed of 2500r/min, finally continuing high-pressure homogenization treatment under the pressure of 40MPa, and circulating for 15 times to obtain the wood nano-cellulose-nano-cement modified grouting material.
Example 3
A wood nano cellulose-nano cement modified grouting material for reinforcing deep-ground engineering surrounding rock comprises the following raw materials in parts by mass:
45 parts of cement, 0.3 part of sodium carbonate, 8 parts of fly ash, 0.07 part of wood nano-cellulose, 10 parts of silica gel and 8 parts of polyvinyl alcohol.
The preparation method comprises the following steps:
(1) preparing lignocellulose: soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; adding 0.04mol/L citric acid-sodium citrate buffer solution (pH6.2) into the slurry, heating and stirring at 45 deg.C with stirring rate of 250 r/min; then adding a mixed solution of endoglucanase and laccase for enzymolysis for 1.5h (the dosage of the endoglucanase is 10IU/g, the dosage of the laccase is 20IU/g), wherein the mass ratio of the pulp to the enzyme solution is 1: 0.05. heating to 95 deg.C, inactivating enzyme for 30min, washing, centrifuging, and balancing water to obtain lignocellulose.
(2) Diluting lignocellulose with water, performing high-pressure homogenization treatment under the pressure of 30MPa, and circulating for 20 times to obtain lignocellulose pulp; wherein, the adding amount of the water is based on that the mass fraction of the wood fiber in the wood nano-cellulose pulp is 0.08%.
(3) Sequentially adding fly ash, sodium carbonate, silica gel, polyvinyl alcohol and wood nano-cellulose pulp into cement, grinding for 2.5h at the rotating speed of 2000r/min, then grinding for 1h at the rotating speed of 3000r/min, finally continuing high-pressure homogenization treatment under the condition that the pressure is 35MPa, and circulating for 18 times to obtain the wood nano-cellulose-nano-cement modified grouting material.
Comparative example 1
The difference from example 1 is that the method for preparing lignocellulose comprises: (1) soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; (2) and adding a citric acid-sodium citrate buffer solution into the slurry, heating and stirring, washing, centrifuging, balancing water, and freeze-drying to obtain the lignocellulose.
Comparative example 2
The difference from example 1 is that the step (3) is eliminated, and all the raw materials are directly mixed and stirred uniformly.
Comparative example 3
The difference from example 1 is that the complex enzyme in step (1) is replaced by a mixture of endoglucanase and xylanase.
Comparative example 4
The difference from example 1 is that a grouting material which is arbitrarily purchased in the market comprises 18 parts of cement, 6 parts of clay, 6 parts of class F class ii fly ash, 1.5 parts of a curing agent, 2 parts of an expanding agent, 0.2 part of a water reducing agent and 20 parts of water by mass.
Comparative example 5
The difference from example 1 is that no silica gel and no polyvinyl alcohol are added.
Test example 1
The grouting materials prepared in examples 1 to 3 and comparative examples 1 to 5 were made into cuboids of 100mm × 20mm × 25mm for performance testing. The results are shown in Table 1.
TABLE 1
Figure BDA0003399361340000111
As can be seen from Table 1, the grouting material prepared by the invention has low water precipitation rate, high viscosity, short initial setting and final setting time and high compressive strength, and compared with a comparative example, the grouting material is found to have a downward trend in all properties without setting according to the preparation method or raw materials of the invention, which indicates that the raw materials of the invention have complementary functions, mutually promote, enhance the beneficial part effect and avoid the defects of monomer raw materials, thereby preparing the grouting material capable of filling micro cracks.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The wood nano-cellulose-nano-cement modified grouting material for reinforcing the deep-ground engineering surrounding rock is characterized by comprising the following raw materials in parts by mass:
30-45 parts of cement, 0.1-0.3 part of sodium carbonate, 4-8 parts of fly ash, 0.03-0.07 part of wood nano-cellulose, 10-15 parts of silica gel and 8-13 parts of polyvinyl alcohol.
2. The wood nanocellulose-nanocement modified grouting material for deep ground engineering surrounding rock reinforcement as claimed in claim 1, wherein the wood nanocellulose is wood nanocellulose filaments with a diameter of 5-20nm, a length of 1-3um, and an aspect ratio of 50-300; the nano cement is cement particles with the particle size of 10-200 nm.
3. The lignocelluloses-nanometer cement modified grouting material for deep ground engineering surrounding rock reinforcement according to claim 2, characterized in that the raw material of lignocelluloses is lignocelluloses, and the preparation method of lignocelluloses is as follows: (1) soaking waste wood in deionized water for 24 hours, pulping, and centrifugally dewatering to obtain pulp; (2) adding citric acid-sodium citrate buffer solution into the slurry, heating and stirring; (3) then adding enzyme solution for enzymolysis, heating to 95 deg.C for 30min for enzyme deactivation, washing, centrifuging, and balancing water content to obtain lignocellulose.
4. The lignocelluloses-nanocement modified grouting material for deep ground engineering surrounding rock reinforcement of claim 3, wherein the waste wood comprises wood, straw or pulp; the heating and stirring temperature is 45 ℃, and the stirring speed is 250 r/min.
5. The wood nano-cellulose-nano-cement modified grouting material for deep engineering surrounding rock reinforcement according to claim 3, characterized in that the enzyme solution is a mixed solution of endoglucanase and laccase, the amount of endoglucanase is 10IU/g, and the amount of laccase is 20 IU/g.
6. The lignocelluloses-nanometer cement modified grouting material for deep ground engineering surrounding rock reinforcement according to claim 3, characterized in that the mass ratio of the slurry to the enzyme solution is 1: (0.03-0.05).
7. The preparation method of the lignocelluloses-nanometer cement modified grouting material for deep ground engineering surrounding rock reinforcement according to any one of claims 1-6, characterized by comprising the following steps:
(1) weighing raw materials according to mass, adding water to dilute lignocellulose, and then carrying out high-pressure homogenization treatment to obtain lignocellulose pulp;
(2) sequentially adding fly ash, sodium carbonate, silica gel, polyvinyl alcohol and wood nano-cellulose slurry into cement, wet grinding, and continuously carrying out high-pressure homogenization treatment to obtain the wood nano-cellulose-nano-cement modified grouting material.
8. The method according to claim 7, wherein the mass fraction of the wood fiber in the nano-sized cellulose pulp is 0.04 to 0.08%.
9. The method according to claim 7, wherein the pressure during the high-pressure homogenization is 30-40MPa, and the cycle is 15-20 times.
10. The preparation method according to claim 7, wherein the wet milling is specifically: grinding for 2-3h at the rotation speed of 2000-.
CN202111491044.5A 2021-12-08 2021-12-08 Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof Active CN114085059B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111491044.5A CN114085059B (en) 2021-12-08 2021-12-08 Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111491044.5A CN114085059B (en) 2021-12-08 2021-12-08 Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114085059A true CN114085059A (en) 2022-02-25
CN114085059B CN114085059B (en) 2023-03-03

Family

ID=80306865

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111491044.5A Active CN114085059B (en) 2021-12-08 2021-12-08 Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114085059B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115286305A (en) * 2022-08-15 2022-11-04 龙岩学院 Soil cave or karst cave filling grouting material and preparation method thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012019364A1 (en) * 2010-08-13 2012-02-16 北新集团建材股份有限公司 Modified wood fiber-reinforced cement external wall panel and producing method therefor
CN103833294A (en) * 2013-11-07 2014-06-04 北京中煤矿山工程有限公司 Single-liquid-stabilized cement-based slurry for surrounding rock consolidation of 1000-meter-depth horizontal roadway
CN105174768A (en) * 2015-08-31 2015-12-23 南京林业大学 Nanometer cellulose fiber reinforced cement-based material
CN105198333A (en) * 2015-10-30 2015-12-30 王璐 Modified grouting material
CN105272085A (en) * 2015-10-30 2016-01-27 王璐 Novel grouting material
CN105272086A (en) * 2015-10-30 2016-01-27 王璐 Double-doped grouting material
CN112252068A (en) * 2020-09-01 2021-01-22 华南理工大学 Lignocellulose nanofibrils as well as preparation method and application thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012019364A1 (en) * 2010-08-13 2012-02-16 北新集团建材股份有限公司 Modified wood fiber-reinforced cement external wall panel and producing method therefor
CN103833294A (en) * 2013-11-07 2014-06-04 北京中煤矿山工程有限公司 Single-liquid-stabilized cement-based slurry for surrounding rock consolidation of 1000-meter-depth horizontal roadway
CN105174768A (en) * 2015-08-31 2015-12-23 南京林业大学 Nanometer cellulose fiber reinforced cement-based material
CN105198333A (en) * 2015-10-30 2015-12-30 王璐 Modified grouting material
CN105272085A (en) * 2015-10-30 2016-01-27 王璐 Novel grouting material
CN105272086A (en) * 2015-10-30 2016-01-27 王璐 Double-doped grouting material
CN112252068A (en) * 2020-09-01 2021-01-22 华南理工大学 Lignocellulose nanofibrils as well as preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115286305A (en) * 2022-08-15 2022-11-04 龙岩学院 Soil cave or karst cave filling grouting material and preparation method thereof

Also Published As

Publication number Publication date
CN114085059B (en) 2023-03-03

Similar Documents

Publication Publication Date Title
CN105294027B (en) Graphene oxide modified cement-based composite material and preparation method thereof
CN104030634A (en) High-strength and high-toughness reactive powder concrete of carbon doped nano-tube and preparation method of high-strength and high-toughness reactive powder concrete
CN110510943A (en) A kind of impervious corrosion resistance of chloride ion concrete and preparation method thereof
CN111807790B (en) Rubber powder ultrahigh-ductility mortar for building 3D printing and preparation
CN113772987B (en) Modification method of fly ash and prepared modified fly ash
CN114085059B (en) Wood nanocellulose-nanometer cement modified grouting material for deep-ground engineering surrounding rock reinforcement and preparation method thereof
CN101891417A (en) High-toughness polypropylene fiber reinforced cement-based composite material and preparation method thereof
CN112608052A (en) Dry-mixed masonry mortar prepared from recycled aggregate and preparation method thereof
CN110143791A (en) A kind of preparation process of high-strength concrete
CN107601977B (en) Cellulose nanocrystal reinforced cement paste material and preparation method thereof
Correia et al. Utilization of vegetable fibers for production of reinforced cementitious materials
CN112592109B (en) Recycled concrete with excellent performance
CN108483978B (en) Cementing agent for regenerated pervious concrete and preparation method and application thereof
CN115477495B (en) Plastering mortar plasticizer and preparation method thereof
CN116375421A (en) Dry-mixed thin-layer masonry mortar and preparation method thereof
CN110498629B (en) Application of ECC material in recycled aggregate reinforcement, recycled reinforced aggregate and preparation method and application thereof
CN114988796A (en) Recycled broken brick concrete based on interface enhancement and preparation method thereof
CN114772985A (en) High-strength anti-crack concrete and preparation method thereof
CN113620660A (en) High-strength aerated reproducible concrete and preparation method thereof
CN105693132A (en) Preparation method of special grinding aid for silver grey rock powder
CN112500115A (en) Building thermal insulation mortar material taking gold tailings and oil sand tailings as raw materials and preparation method and application thereof
CN109553324A (en) A kind of strong concrete accelerator and preparation method thereof
CN111499289A (en) High-strength heat-insulating concrete and preparation method thereof
CN117819926B (en) Potassium titanate whisker reinforced ultra-high performance recycled concrete and preparation method thereof
CN116283201A (en) Modified rice hull fiber toughening grouting material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant