CN113233449A - Preparation method of modified graphene oxide and formula for preparing slump-retaining mother liquor by using modified graphene oxide - Google Patents

Preparation method of modified graphene oxide and formula for preparing slump-retaining mother liquor by using modified graphene oxide Download PDF

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Publication number
CN113233449A
CN113233449A CN202110543888.3A CN202110543888A CN113233449A CN 113233449 A CN113233449 A CN 113233449A CN 202110543888 A CN202110543888 A CN 202110543888A CN 113233449 A CN113233449 A CN 113233449A
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graphene oxide
preparing
formula
slump
modified graphene
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刘裕
吴健伟
罗帅
王凯
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Shenzhen Gangchuang Building Material Co ltd
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Shenzhen Gangchuang Building Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/194After-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
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F292/00Macromolecular compounds obtained by polymerising monomers on to inorganic 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
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0068Ingredients with a function or property not provided for elsewhere in C04B2103/00

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

The invention discloses a method for preparing modified graphene oxide and a formula for preparing slump-retaining mother liquor by using the modified graphene oxide, which comprises the following steps: s1, taking a proper amount of graphene oxide for modification, preparing 2g/l graphene oxide dispersion liquid, and dispersing for 2h under an ultrasonic condition; s2, weighing 1000g of graphene oxide dispersion liquid, placing the graphene oxide dispersion liquid in a reaction kettle, stirring, and heating in a water bath to 70 ℃; s3, weighing 4g of vinyltriethoxysilane, and adding the vinyltriethoxysilane into the reaction kettle in a dropwise manner for 0.5 hour; s4, continuing the reaction for 0.5 hour after the dropwise addition is finished; according to the method and the formula, the graphene oxide is subjected to certain chemical modification, so that the graphene oxide can participate in the synthesis of the slump-retaining polycarboxylic acid mother liquor, the product can effectively weaken the tackifying effect of the graphene oxide on concrete, the utilization rate of the graphene oxide is improved, and the slump-retaining performance of the graphene modified concrete in a period of time is ensured.

Description

Preparation method of modified graphene oxide and formula for preparing slump-retaining mother liquor by using modified graphene oxide
Technical Field
The invention relates to the technical field of preparation and application of modified graphene oxide, in particular to a preparation method of modified graphene oxide and a formula for preparing slump-retaining mother liquor by using the modified graphene oxide.
Background
The particle size of cement particles is mostly 7-200 mu m, but most of hydration products C-S-H gel of the cement particles are in a nanometer size, the nanometer materials are doped in the cementing materials, the pore filling effect can be achieved, the high-energy surface of the nanometer materials can also play a crystal nucleus effect, the surface of the nanometer materials can be bonded with the C-S-H gel, ettringite is induced to grow on the accessories of the nanometer materials, and finally a three-dimensional space network structure with the nanometer materials as nodes and the C-S-H gel as a network is formed, so that the physical and mechanical properties and durability of the hardened cement slurry are greatly improved.
A large number of researches show that the graphene oxide serving as a nano material can improve the strength of set cement at a certain doping amount, but the graphene oxide is easy to agglomerate under an alkaline condition, so that the utilization rate of the graphene oxide is low, and meanwhile, the concrete can be remarkably thickened along with the increase of the doping amount, so that the slump loss of the concrete is further accelerated. Therefore, a method for preparing modified graphene oxide and a formula for preparing slump-retaining mother liquor by using the modified graphene oxide are provided.
Disclosure of Invention
The invention aims to provide a method for preparing modified graphene oxide and a formula for preparing slump-retaining mother liquor by using the modified graphene oxide, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing modified graphene oxide comprises the following steps:
s1, taking a proper amount of graphene oxide for modification, preparing 2g/l graphene oxide dispersion liquid, and dispersing for 2h under an ultrasonic condition;
s2, weighing 1000g of graphene oxide dispersion liquid, placing the graphene oxide dispersion liquid in a reaction kettle, stirring, and heating in a water bath to 70 ℃;
s3, weighing 4g of vinyltriethoxysilane, and adding the vinyltriethoxysilane into the reaction kettle in a dropwise manner for 0.5 hour;
and S4, continuing the reaction for 0.5 hour after the dropwise addition is finished, standing and cooling, and ending the test.
A formula for preparing slump-retaining mother liquor by using modified graphene oxide comprises 300g of polycarboxylic acid macromonomer, 240g of modified graphene oxide dispersion liquid, 2.75g of hydrogen peroxide, 69g of A liquid, 112.4g of B liquid, 35g of neutralization liquid and 160g of water.
Preferably, the solution A is made of 11g of acrylic acid and 58g of hydroxyethyl acrylate.
Preferably, the solution B is prepared from 1.0g of ascorbic acid, 1.4g of thioglycolic acid and 110g of water.
Preferably, the neutralization solution is made of 5g NaOH and 30g water.
A formula for preparing slump-retaining mother liquor by using modified graphene oxide comprises 300g of polycarboxylic acid macromonomer, 240g of modified graphene oxide dispersion liquid, 2.75g of hydrogen peroxide, 80g of A liquid, 103.5g of B liquid, 35g of neutralization liquid and 240g of water.
Preferably, the solution A is prepared from 20g of acrylic acid, 55g of hydroxyethyl acrylate and 5g of water.
Preferably, the solution B is prepared from 1.5g of ascorbic acid, 2g of thioglycolic acid and 100g of water.
Preferably, the neutralization solution is made of 5g NaOH and 30g water.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the graphene oxide is subjected to certain chemical modification, so that the graphene oxide can participate in the synthesis of the slump retaining polycarboxylic acid mother liquor, the product can effectively weaken the tackifying effect of the graphene oxide on concrete, the utilization rate of the graphene oxide is improved, and the slump retaining performance of the graphene modified concrete in a period of time is ensured.
Detailed Description
The described embodiments are only some embodiments of the invention, not all 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 invention provides a technical scheme that: a method for preparing modified graphene oxide comprises the following steps:
s1, taking a proper amount of graphene oxide for modification, preparing 2g/l graphene oxide dispersion liquid, and dispersing for 2h under an ultrasonic condition;
s2, weighing 1000g of graphene oxide dispersion liquid, placing the graphene oxide dispersion liquid in a reaction kettle, stirring, and heating in a water bath to 70 ℃;
s3, weighing 4g of vinyltriethoxysilane, and adding the vinyltriethoxysilane into the reaction kettle in a dropwise manner for 0.5 hour;
and S4, continuing the reaction for 0.5 hour after the dropwise addition is finished, standing and cooling, and ending the test.
A formula for preparing slump-retaining mother liquor by using modified graphene oxide comprises 300g of polycarboxylic acid macromonomer, 240g of modified graphene oxide dispersion liquid, 2.75g of hydrogen peroxide, 69g of A liquid, 112.4g of B liquid, 35g of neutralization liquid and 160g of water.
The solution A was made from 11g of acrylic acid and 58g of hydroxyethyl acrylate.
The solution B was prepared from 1.0g ascorbic acid, 1.4g thioglycolic acid and 110g water.
The neutralization solution was made of 5g NaOH and 30g water.
A formula for preparing slump-retaining mother liquor by using modified graphene oxide comprises 300g of polycarboxylic acid macromonomer, 240g of modified graphene oxide dispersion liquid, 2.75g of hydrogen peroxide, 80g of A liquid, 103.5g of B liquid, 35g of neutralization liquid and 240g of water.
The solution A is prepared from 20g of acrylic acid, 55g of hydroxyethyl acrylate and 5g of water.
The solution B is prepared from 1.5g of ascorbic acid, 2g of thioglycolic acid and 100g of water.
The neutralization solution was made of 5g NaOH and 30g water.
Figure BDA0003072802460000031
Figure BDA0003072802460000041
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A method for preparing modified graphene oxide is characterized by comprising the following steps: the method comprises the following steps:
s1, taking a proper amount of graphene oxide for modification, preparing 2g/l graphene oxide dispersion liquid, and dispersing for 2h under an ultrasonic condition;
s2, weighing 1000g of graphene oxide dispersion liquid, placing the graphene oxide dispersion liquid in a reaction kettle, stirring, and heating in a water bath to 70 ℃;
s3, weighing 4g of vinyltriethoxysilane, and adding the vinyltriethoxysilane into the reaction kettle in a dropwise manner for 0.5 hour;
and S4, continuing the reaction for 0.5 hour after the dropwise addition is finished, standing and cooling, and ending the test.
2. A formula for preparing slump-retaining mother liquor by using modified graphene oxide is characterized in that: the graphene oxide dispersion liquid comprises 300g of polycarboxylic acid macromonomer, 240g of modified graphene oxide dispersion liquid, 2.75g of hydrogen peroxide, 69g of A liquid, 112.4g of B liquid, 35g of neutralization liquid and 160g of water.
3. The formula for preparing slump-retaining mother liquor by using modified graphene oxide according to claim 2, wherein the formula comprises the following components in percentage by weight: the solution A was made from 11g of acrylic acid and 58g of hydroxyethyl acrylate.
4. The formula for preparing slump-retaining mother liquor by using modified graphene oxide according to claim 3, wherein the formula comprises the following components in percentage by weight: the solution B was prepared from 1.0g ascorbic acid, 1.4g thioglycolic acid and 110g water.
5. The formula for preparing slump-retaining mother liquor by using modified graphene oxide according to claim 4, wherein the formula comprises the following components in percentage by weight: the neutralization solution was made of 5g NaOH and 30g water.
6. A formula for preparing slump-retaining mother liquor by using modified graphene oxide is characterized in that: the graphene oxide/300 g, 80g, 103.5.5 g, 35g, a neutralizing liquid, 35g, and water/a neutralizing liquid, 35g, and 240g, and water 240 g.
7. The formula for preparing slump-retaining mother liquor by using modified graphene oxide according to claim 6, wherein the formula comprises the following components in percentage by weight: the solution A is prepared from 20g of acrylic acid, 55g of hydroxyethyl acrylate and 5g of water.
8. The formula for preparing slump-retaining mother liquor by using modified graphene oxide according to claim 7, wherein the formula comprises the following components in percentage by weight: the solution B is prepared from 1.5g of ascorbic acid, 2g of thioglycolic acid and 100g of water.
9. The formula for preparing slump-retaining mother liquor by using modified graphene oxide according to claim 8, wherein the formula comprises the following components in percentage by weight: the neutralization solution was made of 5g NaOH and 30g water.
CN202110543888.3A 2021-05-19 2021-05-19 Preparation method of modified graphene oxide and formula for preparing slump-retaining mother liquor by using modified graphene oxide Pending CN113233449A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896453A (en) * 2021-10-27 2022-01-07 北京石墨烯技术研究院有限公司 Modified graphene composite material and preparation method thereof, cement reinforcing agent and application thereof

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN106279580A (en) * 2016-08-08 2017-01-04 北京建筑大学 A kind of poly carboxylic acid modified graphene oxide complex and preparation method and application
CN112759726A (en) * 2021-01-21 2021-05-07 深圳港创建材股份有限公司 Graphene oxide modified slump retaining mother solution, and preparation method and use method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106279580A (en) * 2016-08-08 2017-01-04 北京建筑大学 A kind of poly carboxylic acid modified graphene oxide complex and preparation method and application
CN112759726A (en) * 2021-01-21 2021-05-07 深圳港创建材股份有限公司 Graphene oxide modified slump retaining mother solution, and preparation method and use method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896453A (en) * 2021-10-27 2022-01-07 北京石墨烯技术研究院有限公司 Modified graphene composite material and preparation method thereof, cement reinforcing agent and application thereof
CN113896453B (en) * 2021-10-27 2022-11-29 北京石墨烯技术研究院有限公司 Modified graphene composite material and preparation method thereof, cement reinforcing agent and application thereof

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