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CN114988747A - Dispersing agent for fiber foam concrete - Google Patents

Dispersing agent for fiber foam concrete Download PDF

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Publication number
CN114988747A
CN114988747A CN202210738477.4A CN202210738477A CN114988747A CN 114988747 A CN114988747 A CN 114988747A CN 202210738477 A CN202210738477 A CN 202210738477A CN 114988747 A CN114988747 A CN 114988747A
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Prior art keywords
fiber
foam concrete
anionic clay
hours
dispersant
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Pending
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CN202210738477.4A
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Chinese (zh)
Inventor
王纪缘
朱敏
宋书雨
杨光
张天琪
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Yangzhou Polytechnic Institute
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Yangzhou Polytechnic Institute
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Priority to CN202210738477.4A priority Critical patent/CN114988747A/en
Publication of CN114988747A publication Critical patent/CN114988747A/en
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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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • 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
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/40—Surface-active agents, dispersants
    • C04B2103/408—Dispersants
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a dispersing agent for fiber foam concrete, which belongs to the technical field of concrete and comprises the following raw materials in parts by mass: 50-100 parts of anionic clay, 20-40 parts of hydrophobic modifier and 10-20 parts of surfactant; the using process of the dispersant is as follows: the fiber is first hydrophobically modified with hydrophobic modifier, then modified with surfactant, then loaded with anionic clay, and then mixed with the foam concrete. In the technical scheme of the invention, octadecylamine is used for modifying a fiber material, and then the cationic surfactant cetyl ammonium bromide is used for modifying hydrophobic fibers, so that the hydrophobic fibers are loaded between layers of anionic clay, and the mixing of the anionic clay loaded with the fibers and foam concrete has the following advantages that: anionic clay as a hydrophilic material can be mixed well with the foam concrete, second: the clay has a higher quality than the fibres and can thus be dispersed better.

Description

Dispersing agent for fiber foam concrete
Technical Field
The invention belongs to the technical field of concrete, and particularly relates to a dispersing agent for fiber foam concrete.
Background
The foam concrete is a novel light heat-insulating material containing a large number of closed air holes, which is formed by fully foaming a foaming agent in a mechanical mode through a foaming system of a foaming machine, uniformly mixing foam and cement slurry, then carrying out cast-in-place construction or mould forming through a pumping system of the foaming machine and carrying out natural maintenance. The foam concrete is a lightweight, heat-preservation, heat-insulation, fire-resistant, sound-insulation and frost-resistant concrete material, slurry can automatically level and self-compact, construction workability is good, pumping and leveling are facilitated, the foam concrete almost has good compatibility with other building materials, but the foam concrete has the problems of low strength, easiness in cracking and the like due to the fact that no coarse aggregate and porous structural characteristics exist, and the wide application of the foam concrete is limited.
The problem can be effectively solved by adding the fibers, however, because the density of the fibers is smaller than that of the cement material, the layering and segregation phenomena generally exist in the stirring process, and the dispersion of the fiber materials in the foam concrete is seriously influenced.
Disclosure of Invention
The invention aims to provide a dispersing agent for fiber foam concrete, which is characterized in that fibers are subjected to hydrophobic modification and then are subjected to de-modification by using a cationic surfactant, and the tail end of the cationic surfactant can be inserted into the interlayer of anionic clay, so that the loading of the anionic clay on the fibers is realized.
The technical problems to be solved by the invention are as follows: the dispersant for improving the fiber in the concrete is mainly some surfactants, and the fiber modified by the surfactants can realize the compatibility with the concrete, but the problem of small quality of the fiber cannot be changed.
The purpose of the invention can be realized by the following technical scheme:
a dispersing agent for fiber foam concrete comprises the following raw materials in parts by mass: 50-100 parts of anionic clay, 20-40 parts of hydrophobic modifier and 10-20 parts of surfactant;
the using process of the dispersant is as follows: the fiber is first hydrophobically modified with hydrophobic modifier, then modified with surfactant, then loaded with anionic clay, and then mixed with the foam concrete.
Further, the hydrophobic modification step is as follows:
s1, performing Soxhlet extraction on jute fibers by using benzene/ethanol for 12 hours, and then boiling the jute fibers in distilled water for 3 hours to obtain pretreated fibers, wherein the dosage ratio of the jute fibers to the benzene/ethanol is 0.1-0.3 g: 50-100mL, wherein the benzene/ethanol is composed of benzene and ethanol with the volume ratio of 1-3: 1;
s2, mixing the pretreated fiber with 1.0U/mL laccase, 1.4mg/mL 2,2,6, 6-tetramethyl piperidine-1-oxyl and 10mmol/L octadecylamine in 0.2mol/L acetate buffer solution with pH4.5, reacting at 50 ℃ for 12 hours while stirring with a magnetic rod at the speed of 300r/min, then washing the pretreated fiber with hot water at 80 ℃ for 20 minutes, and extracting with ethanol for 12 hours, wherein the dosage ratio of the pretreated fiber, the laccase, the 2,2,6, 6-tetramethyl piperidine-1-oxyl and the octadecylamine is 0.1-0.5 g: 10-20 mL: 1.3-1.5 mL: 0.2-0.4 g: 5-8 mL.
In the reaction process, C6 primary hydroxyl of glucose unit in jute fiber is oxidized into aldehyde group by laccase/TEMPO system, and in addition, these reaction sites can induce foreign molecules to have nucleophilic addition reaction with electron-donating substituent such as amino group, and imine bond (-C ═ N-) is formed by condensation (Schiff base reaction), so that octadecylamine is grafted to jute fiber, and excellent hydrophobicity is given to them.
Further, the anionic clay is prepared by the following steps:
mixing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 O and (NH) 2 ) 2 Dissolving CO in deionized water to obtain transparent solution, transferring the transparent solution into 100 deg.C oil bath, maintaining for 6-12 hr, stopping stirring when the reaction is over, maintaining for 10 hr, filtering, washing, and freeze drying to obtain anionic clay containing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 O、(NH 2 ) 2 The dosage ratio of CO to deionized water is 70-80 g: 30-40 g: 10-20 g: 700 and 800 mL.
Further, the surfactant is a cationic surfactant, cetyl ammonium bromide.
Further, the specific process of loading the anionic clay is as follows:
dispersing anionic clay into ethanol and deionized water, ultrasonic treating for 20 min, adding ammonium cetyl bromide, stirring at 25 deg.C for 30 min, filtering, washing, and drying in 70 deg.C oven for 5 hr.
The invention has the beneficial effects that:
(1) according to the technical scheme, octadecylamine is used for modifying a fiber material to prepare the hydrophobic fiber, and the hydrophobic fiber is modified by the cationic surfactant cetyl ammonium bromide, wherein a long hydrophobic alkane chain of the cetyl ammonium bromide is adsorbed on the surface of the fiber through hydrophobic interaction, and NH is generated in the fiber 4 + The cationic end can be inserted into the interlayer of the anionic clay, because the interlayer of the anionic clay is filled with anions, thereby realizing that the hydrophobic fiber is loaded into the interlayer of the anionic clay, and the mixing of the anionic clay loaded with the fiber and the foam concrete has the following advantages: anionic clay as a hydrophilic material can be mixed well with the foam concrete, second: the clay has a higher quality than the fibres and can thus be dispersed better.
(2) In the technical scheme of the invention, the anionic clay (LDH) is a non-toxic, smoke-inhibiting and environment-friendly flame retardant, has the function of heat preservation, can also increase the heat preservation performance of the material when added into the foam concrete, and can also permeate into the foam concrete to further increase the mechanical performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The using process of the dispersant is as follows: the fiber is first hydrophobically modified with hydrophobic modifier, then modified with surfactant, then loaded with anionic clay, and then mixed with the foam concrete.
Example 1
The hydrophobic modification steps are as follows:
s1, performing Soxhlet extraction on 0.1g of jute fiber by using 50mL of benzene/ethanol (the volume ratio is 1:1) for 12 hours, and then boiling the jute fiber in distilled water for 3 hours to obtain pretreated fiber;
s2, mixing 0.1g of the pretreated fiber with 1.3mL of 1.0U/mL laccase, 0.2g of 1.4mg/mL of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 5mL of 10mmol/L octadecylamine in 10mL of 0.2mol/L acetate buffer solution with pH4.5, reacting at 50 ℃ for 12 hours while stirring at 300r/min by using a magnetic rod, washing the pretreated fiber with hot water at 80 ℃ for 20 minutes, and extracting with ethanol for 12 hours;
example 2
The hydrophobic modification steps are as follows:
s1, performing Soxhlet extraction on 0.2g of jute fiber by using 80mL of benzene/ethanol (the volume ratio is 2:1) for 12 hours, and then boiling the jute fiber in distilled water for 3 hours to obtain pretreated fiber;
s2, mixing 0.3g of pretreated fiber with 1.4mL of 1.0U/mL laccase, 0.3g of 1.4mg/mL of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 6mL of 10mmol/L octadecylamine in 15mL of 0.2mol/L acetate buffer solution with pH4.5, reacting at 50 ℃ for 12 hours while stirring at 300r/min by using a magnetic rod, washing the pretreated fiber with 80 ℃ hot water for 20 minutes, and extracting with ethanol for 12 hours;
example 3
The hydrophobic modification steps are as follows:
s1, performing Soxhlet extraction on 0.3g of jute fiber by using 100mL of benzene/ethanol (volume ratio is 3:1) for 12 hours, and then boiling the jute fiber in distilled water for 3 hours to obtain pretreated fiber;
s2, mixing 0.5g of pretreated fiber with 1.5mL of 1.0U/mL laccase, 0.4g of 1.4mg/mL of 2,2,6, 6-tetramethylpiperidine-1-oxyl and 8mL of 10mmol/L octadecylamine in 20mL of 0.2mol/L acetate buffer solution with pH4.5, reacting at 50 ℃ for 12 hours while stirring at 300r/min by using a magnetic rod, washing the pretreated fiber with 80 ℃ hot water for 20 minutes, and extracting with ethanol for 12 hours;
the hydrophobic fibers prepared in examples 1 to 3 were now tested, and the surface hydrophobicity of the jute fibers was evaluated by contact angle and wetting time. Before the measurement, the jute fabric samples were moisture equilibrated in a standard atmosphere with a relative humidity of 65% + -5% and a temperature of 21 + -1 ℃. The contact angle was then measured on an OCA50Micro contact angle meter, five points were measured for each sample and the results averaged. The wetting time was measured according to AATCC test method 79-2007. A drop of water was allowed to fall from a height of 10 ± 1mm onto the taut surface of the test fabric. The time required for the specular reflection of the water drop to disappear was measured and recorded as the wetting time, and five readings were taken and averaged for each sample, with the test results shown in table 1 below.
TABLE 1
Item Water contact Angle (°)
Example 1 128.4
Example 2 127.6
Example 3 129.7
Initial 96.5
As can be seen from table 1 above, the jute fiber has increased hydrophobic property after being hydrophobically modified.
Example 4
The anionic clay is prepared by the following steps:
70g of Mg (NO) 3 ) 2 ·6H 2 O and 30g of Al (NO) 3 ) 3 ·9H 2 O and 10g of (NH) 2 ) 2 Dissolving CO in 700mL of deionized water to obtain a transparent solution, transferring the transparent solution into an oil bath at 100 ℃ for 6 hours of reaction time, stopping stirring when the reaction is finished, preserving the temperature for 10 hours, and then filtering, washing and freeze-drying to obtain the anionic clay.
Example 5
The anionic clay is prepared by the following steps:
75g of Mg (NO) 3 ) 2 ·6H 2 O and 35g of Al (NO) 3 ) 3 ·9H 2 O and 15g of (NH) 2 ) 2 Dissolving CO in 750mL of deionized water to obtain a transparent solution, transferring the transparent solution into an oil bath at 100 ℃ for 10 hours of reaction time, stopping stirring when the reaction is finished, preserving the temperature for 10 hours, and then filtering, washing and freeze-drying to obtain the anionic clay.
Example 6
The anionic clay is prepared by the following steps:
80g of Mg (NO) 3 ) 2 ·6H 2 O and 40g of Al (NO) 3 ) 3 ·9H 2 O and 20g of (NH) 2 ) 2 Dissolving CO in 800mL of deionized water to obtain a transparent solution, transferring the transparent solution into an oil bath at 100 ℃ for reaction for 12 hours, stopping stirring when the reaction is finished, preserving the temperature for 10 hours, and then filtering, washing and freeze-drying to obtain the anionic clay.
Example 7
The specific process of loading the anionic clay is as follows:
5g of anionic clay was dispersed in 300mL of ethanol and 300mL of deionized water, sonicated for 20 minutes, 1g of cetylammonium bromide was added and stirring was continued for 30 minutes at 25 deg.C, filtered, washed and dried in an oven at 70 deg.C for 5 hours.
Example 8
The specific process of loading the anionic clay is as follows:
8g of anionic clay was dispersed in 400mL of ethanol and 400mL of deionized water, sonicated for 20 minutes, 1.5g of cetylammonium bromide was added and stirred continuously at 25 ℃ for 30 minutes, filtered, washed and dried in an oven at 70 ℃ for 5 hours.
Example 9
The specific process of loading the anionic clay is as follows:
10g of anionic clay was dispersed in 500mL of ethanol and 500mL of deionized water, sonicated for 20 minutes, 2g of cetylammonium bromide was added and stirring was continued at 25 ℃ for 30 minutes, filtered, washed and dried in an oven at 70 ℃ for 5 hours.
Example 10
A dispersing agent for fiber foam concrete comprises the following raw materials in parts by mass: 50 parts of anionic clay, 20 parts of hydrophobic modifier and 10 parts of surfactant.
Example 11
A dispersing agent for fiber foam concrete comprises the following raw materials in parts by mass: 80 parts of anionic clay, 30 parts of hydrophobic modifier and 15 parts of surfactant.
Example 12
A dispersing agent for fiber foam concrete comprises the following raw materials in parts by mass: 100 parts of anionic clay, 40 parts of hydrophobic modifier and 20 parts of surfactant.
Comparative example 1
This comparative example differs from example 12 in that the anionic clay, hydrophobic modifier and surfactant are conventionally mixed.
The dispersants of examples 10-12 and comparative example 1 were now tested for performance and the results are shown in table 2 below.
TABLE 2
Figure BDA0003716740120000071
As can be seen from table 2 above, in the embodiment of the present invention, the fibers are subjected to hydrophobic modification, and then are subjected to modification by using the cationic surfactant, so that the terminal of the cationic surfactant can be inserted into the interlayer of the anionic clay, thereby realizing the loading of the anionic clay on the fibers, and increasing the mechanical properties and the thermal insulation properties of the fiber foam concrete.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.

Claims (8)

1. The dispersing agent for the fiber foam concrete is characterized by comprising the following raw materials in parts by mass: 50-100 parts of anionic clay, 20-40 parts of hydrophobic modifier and 10-20 parts of surfactant;
the using process of the dispersant is as follows: the fiber is first hydrophobically modified with hydrophobic modifier, then modified with surfactant, then loaded with anionic clay, and then mixed with the foam concrete.
2. The dispersant for fiber foam concrete according to claim 1, wherein the step of hydrophobically modifying is:
s1, performing Soxhlet extraction on jute fibers by using benzene/ethanol for 12 hours, and then boiling the jute fibers in distilled water for 3 hours to obtain pretreated fibers;
s2, mixing the pretreated fiber with laccase, 2,6, 6-tetramethyl piperidine-1-oxyl and octadecylamine in acetate buffer solution, reacting at 50 ℃ for 12 hours while stirring at 300r/min by using a magnetic rod, washing the pretreated fiber with hot water at 80 ℃ for 20 minutes, and extracting with ethanol for 12 hours.
3. The dispersant for fiber foam concrete according to claim 2, wherein in step S1, the dosage ratio of jute fiber and benzene/ethanol is 0.1 to 0.3 g: 50-100mL, benzene/ethanol is composed of benzene and ethanol with the volume ratio of 1-3: 1.
4. The dispersant for fiber foam concrete according to claim 2, wherein in step S2, the amount ratio of the pretreated fiber, laccase, 2,6, 6-tetramethylpiperidine-1-oxyl and octadecylamine is 0.1-0.5 g: 10-20 mL: 1.3-1.5 mL: 0.2-0.4 g: 5-8 mL.
5. A dispersant for fibrous foam concrete according to claim 1 wherein the anionic clay is prepared by the steps of:
mixing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 O and (NH) 2 ) 2 Dissolving CO in deionized water to obtain a transparent solution, transferring the transparent solution into an oil bath at 100 ℃ for 6-12 hours of reaction time, stopping stirring when the reaction is finished, preserving the temperature for 10 hours, and then filtering, washing and freeze-drying to obtain the anionic clay.
6. A dispersant for fibre foam concrete according to claim 5, characterized in that Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 O、(NH 2 ) 2 CO and deionizationThe dosage ratio of water is 70-80 g: 30-40 g: 10-20 g: 700-800 mL.
7. A dispersant for fibrous cellular concrete according to claim 1 wherein the surfactant is a cationic surfactant cetyl ammonium bromide.
8. A dispersant for fibrous foam concrete according to claim 1, characterized in that the specific process of anionic clay loading is as follows:
dispersing anionic clay into ethanol and deionized water, ultrasonic treating for 20 min, adding ammonium cetyl bromide, stirring at 25 deg.C for 30 min, filtering, washing, and drying in 70 deg.C oven for 5 hr.
CN202210738477.4A 2022-06-27 2022-06-27 Dispersing agent for fiber foam concrete Pending CN114988747A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110000632A1 (en) * 2007-12-21 2011-01-06 Auke Gerardus Talma Process to Make a Clay Comprising Charge-Balancing Organic Ions, Clays Thus Obtained, and Nanocomposite Materials Comprising the Same
CN109487545A (en) * 2018-11-06 2019-03-19 绍兴文理学院 A method of improving fiber crops/resin composite materials interface adhesion
CN109487561A (en) * 2017-09-10 2019-03-19 北京林业大学 A kind of hydrophobic bamboo fibre and preparation method thereof based on mussel protein biomimetic modification
CN110606980A (en) * 2019-10-11 2019-12-24 西南石油大学 Preparation method of super-hydrophobic LDH/melamine sponge
CN111333917A (en) * 2020-04-26 2020-06-26 林杨志 Hydrophobic cellulose-chitosan high-barrier composite film and preparation method thereof
CN112442901A (en) * 2020-10-12 2021-03-05 江苏泽昊新材料有限公司 Corrosion-resistant heat-insulating tarpaulin material and production method thereof
CN112723398A (en) * 2020-12-22 2021-04-30 陕西科技大学 Magnesium-aluminum hydrotalcite modified montmorillonite nano material and preparation method thereof
CN113773404A (en) * 2021-07-23 2021-12-10 天津科技大学 Super-hydrophobic modification method of nano-cellulose

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110000632A1 (en) * 2007-12-21 2011-01-06 Auke Gerardus Talma Process to Make a Clay Comprising Charge-Balancing Organic Ions, Clays Thus Obtained, and Nanocomposite Materials Comprising the Same
CN109487561A (en) * 2017-09-10 2019-03-19 北京林业大学 A kind of hydrophobic bamboo fibre and preparation method thereof based on mussel protein biomimetic modification
CN109487545A (en) * 2018-11-06 2019-03-19 绍兴文理学院 A method of improving fiber crops/resin composite materials interface adhesion
CN110606980A (en) * 2019-10-11 2019-12-24 西南石油大学 Preparation method of super-hydrophobic LDH/melamine sponge
CN111333917A (en) * 2020-04-26 2020-06-26 林杨志 Hydrophobic cellulose-chitosan high-barrier composite film and preparation method thereof
CN112442901A (en) * 2020-10-12 2021-03-05 江苏泽昊新材料有限公司 Corrosion-resistant heat-insulating tarpaulin material and production method thereof
CN112723398A (en) * 2020-12-22 2021-04-30 陕西科技大学 Magnesium-aluminum hydrotalcite modified montmorillonite nano material and preparation method thereof
CN113773404A (en) * 2021-07-23 2021-12-10 天津科技大学 Super-hydrophobic modification method of nano-cellulose

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