CN115466067B - Composite xerogel slow-release chloride ion curing agent and preparation and application thereof - Google Patents

Composite xerogel slow-release chloride ion curing agent and preparation and application thereof Download PDF

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CN115466067B
CN115466067B CN202211170098.6A CN202211170098A CN115466067B CN 115466067 B CN115466067 B CN 115466067B CN 202211170098 A CN202211170098 A CN 202211170098A CN 115466067 B CN115466067 B CN 115466067B
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curing agent
chloride ion
barium
composite xerogel
release
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CN115466067A (en
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刘晓海
潘涵
张美香
罗忠涛
殷昆鹏
弥杰
郭金洋
郅天一
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Zhengzhou University
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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
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/02—Agglomerated materials, e.g. artificial aggregates
    • C04B18/027—Lightweight materials
    • 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
    • C04B20/00—Use 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
    • C04B20/10—Coating or impregnating
    • C04B20/1018—Coating or impregnating with organic materials
    • C04B20/1029—Macromolecular compounds
    • 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
    • C04B20/00—Use 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
    • C04B20/10—Coating or impregnating
    • C04B20/1055—Coating or impregnating with inorganic materials
    • C04B20/1066—Oxides, Hydroxides
    • 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)
  • Civil Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention belongs to the technical field of functional concrete additives, and particularly relates to a composite xerogel slow-release chloride ion curing agent, and preparation and application thereof. The method adopts a cogel method, uses a barium source and a silicon source as precursors, uses propylene oxide as a catalyst, uses a mixed solution of acetonitrile and deionized water as a solvent to prepare barium-containing composite xerogel, uses the composite xerogel as a core material, and uses silica sol/gelatin as a shell material to prepare the slow-release chloride ion curing agent. The curing agent promotes chemical combination of chloride ions and AFm structure of cement hydration products by releasing barium ions in the later stage of hydration, and promotes the curing of chloride ions. The curing agent can obviously improve the durability of the reinforced concrete structure and has excellent social benefit and economic benefit.

Description

Composite xerogel slow-release chloride ion curing agent and preparation and application thereof
Technical Field
The invention belongs to the technical field of functional concrete additives, and particularly relates to a composite xerogel slow-release chloride ion curing agent, and preparation and application thereof.
Background
Cement materials are widely used in various technical fields, but in a marine environment or under the condition that a large amount of chloride ions exist, free chloride ions can permeate into cement-based materials to damage passivation films on the surfaces of reinforcing steel bars, so that the reinforcing steel bars are rusted, the strength of the reinforcing steel bars is reduced, the binding force between the reinforcing steel bars and concrete is reduced, concrete members are damaged, the durability is poor, the service life is shortened, huge economic loss is caused, and even safety problems are brought in serious cases.
For the problem of reinforcement rust risk caused by high content of endogenous chloride ions in concrete, a plurality of prevention and treatment methods exist, including reinforcement rust inhibitor, coating protection, cathodic protection technology and the like. However, these methods have drawbacks such as local corrosion and accelerated corrosion of a part of the reinforcing steel bar rust inhibitor when the chloride ion concentration is high to a certain extent, and also have disadvantages such as carcinogenesis, alkali aggregate reaction, slump influence, etc. Along with the gradual attention of researchers caused by chloride ion curing, the researchers start to increase the curing capacity of free chloride ions by adding chemical additives, mineral additives and the like into cement-based materials, thereby effectively preventing the reinforcing steel bars from being corroded and prolonging the service life of the reinforced concrete structure.
Disclosure of Invention
In view of the above, the invention aims to provide a composite xerogel sustained-release chloride ion curing agent, and preparation and application thereof.
The technical scheme adopted by the invention is as follows:
the composite xerogel slow-release type chloride ion curing agent comprises the following raw materials in parts by weight: 1-5 parts of barium source, 2-10 parts of organic silicon source, 4-15 parts of catalyst, 15-30 parts of solvent and 2-8 parts of packaging material.
Further preferably, the raw materials used are: 3-5 parts of barium source, 5-10 parts of organic silicon source, 7-15 parts of catalyst, 20-30 parts of solvent and 4-8 parts of packaging material.
The solvent is a mixed solution of acetonitrile and deionized water. The mass ratio of acetonitrile to deionized water is 1:1.
The organic silicon source is one or two of methyl orthosilicate or ethyl orthosilicate; the barium source is one or two of barium acetate and barium nitrate.
The catalyst is propylene oxide; the packaging material is one or two of silica sol and gelatin.
The method for preparing the composite xerogel sustained-release chloride ion curing agent comprises the following steps:
1) Taking the raw materials according to a proportion;
2) Dissolving an organosilicon source in a solvent, and adding a catalyst (30-40% of the total amount) to form a solution A;
3) Dissolving a barium source in a solvent, and stirring to form a solution B;
4) Adding the solution A into the solution B, stirring, and adding the rest catalyst to form a solution C;
5) Drying the solution C, standing, taking out, soaking in absolute ethyl alcohol, taking out, and drying at low temperature and then at high temperature to obtain a composite xerogel;
6) Crushing the composite xerogel to obtain composite xerogel particles;
7) Coating or spraying packaging materials on the surfaces of the composite xerogel particles, and drying to obtain the composite xerogel sustained-release chloride ion curing agent.
The stirring speed in the step 3) is not lower than 500rpm.
The speed of adding the catalyst in the step 4) is not more than 1ml/min.
The drying temperature of the solution C in the step 5) is 30-50 ℃, the soaking time is 2-3d, the temperature during low-temperature drying is 30-50 ℃, and the temperature during high-temperature drying is 100-120 ℃.
The absolute ethyl alcohol is replaced at least 4 times when the absolute ethyl alcohol is soaked in the absolute ethyl alcohol in the step 5).
The particle size of the composite xerogel particles in the step 6) is 0.16-0.30mm.
The temperature during the drying in the step 7) is 40-50 ℃ and the time is 8-10h.
The composite xerogel slow-release type chloride ion curing agent is applied to cement-based materials as a chloride ion curing agent.
The composite xerogel slow-release chloride ion curing agent is added into the cement-based material in an amount which is 1-5% of the total amount of the cementing material.
In the research of the chloride ion curing agent, technicians find that chloride ions in the environment are combined with AFm structures generated by cement hydration reaction through chemical bonds, and are cured to generate hydrated chloroaluminate, including Friedel salt and Kuzel salt, so that corrosion of reinforcing steel bars by the chloride ions in the environment is avoided. But SO4 is present in the environment 2- Can also perform similar binding reaction with AFm structure, SO SO4 2- With Cl - A competing relationship is formed, adversely affecting the curing of chloride ions. The skilled artisan began to consider adding a barium source to first pair SO4 2- Chemical bonding to form stable BaSO 4 Precipitation to reduce SO4 2- For Cl - Competing relationship. The skilled artisan has conceived to add microspheres of a barium source to concrete materials, and has found that the release of barium is indeed comparable to SO4 2- Chemical bonding is carried out to temporarily eliminate SO4 2- But in the environment SO4 2- With Cl - And can not completely disappear, and after a certain time, SO4 in the environment 2- With Cl - The concentration of SO4 will still rise at this time 2- And also form para-Cl - Is to be used in the future). The skilled person considers the need to further investigate how to keep barium ions released for a longer period of time, enabling the elimination of SO4 for a longer period of time 2- For Cl - Is a function of (a) and (b).
In the invention, the slow-release curing agent is prepared, and long-time release of barium ions can be realized. Thus, SO4 can be eliminated for a long time 2- For Cl - Is a competitive influence of (c). Specifically, the invention adopts a barium source and an organosilicon source as precursors, under the action of a catalyst, a mutual support gel framework which takes silicon gel particles as a main body and barium gel particles as local centers for connection is formed, and the gel framework provides steric hindrance, so that the rest barium gel particles are uniformly dispersed in grid gaps. When the curing agent is added into concrete, through the swelling action, the pore liquid passes through the pores of the packaging material to enter the curing agent after a period of time, and the barium gel particles dispersed in the grid gaps can be firstly mixed with SO4 in the pore liquid 2- Generating robust BaSO 4 After a period of time, calcium hydroxide in the pore liquid reacts with silica gel in the barium silica gel skeleton, so that the gel skeleton and the grid are damaged, barium serving as a local center is released, and the calcium hydroxide reacts with the silica gel relatively slowly, so that the release of the barium is relatively slow, and the curing agent provided by the invention has the function of slowly releasing barium ions through the release of a barium source in two stages.
In this gel-matrix form, to release barium ions into the concrete void solution, the silica gel must be reacted in the concrete void solution to release barium ions.
The silicon source of the invention has special requirements in selection, and the organic silicon source is required to be selected, because the inorganic silicon source has serious shrinkage after forming gel, which can cause structural fracture and is difficult to maintain the stability of the gel skeleton for a long time.
The curing agent disclosed by the invention needs to be added with a catalyst during preparation, the ring-opening addition reaction of propylene oxide is utilized to promote the hydrolysis of an organic silicon source through the catalyst, the hydrolysis speed of the silicon source and the barium source is balanced, and the effect of cogelling the silicon source and the barium source is promoted.
In the selection of the solvent, the hydrolysis speed of the barium source and the silicon source is accelerated and balanced by utilizing the high polarity characteristic of acetonitrile, and barium ions participate in the gel, so that the effects of high content of the barium ions and uniform dispersion are achieved.
The composite xerogel slow-release type chloride ion curing agent has the advantages of low cost of raw materials, readily available raw materials, simple and quick production process, and good social and economic benefits.
Drawings
FIG. 1 is a schematic view showing the appearance of a prepared chloride ion curing agent;
FIG. 2 is a schematic diagram of the gel skeleton of the resulting chloride ion curing agent.
Detailed Description
The following examples are given to illustrate the invention in detail, but are not intended to limit the scope of the invention in any way.
Example 1: a composite xerogel slow-release chloride ion curing agent comprises the following raw materials: 4g of barium acetate, 8g of methyl orthosilicate, 12g of propylene oxide, 25g of solvent and 6g of packaging material.
The preparation method comprises the following steps: after weighing the raw materials, dissolving an organosilicon source in a solvent, and adding 4.5g of propylene oxide to form a solution A; dissolving a barium source in a solvent, and stirring to form a solution B; adding the solution A into the solution B, stirring at 500rpm, and slowly adding 7.5g of propylene oxide at a speed of 0.5ml/min to form a solution C; standing the solution C in a drying oven at 30-50deg.C for 3-5 hours, taking out, soaking in absolute ethanol, taking out, replacing absolute ethanol for at least 4 times, drying at 30-50deg.C for 24 hours, and drying at 100-120deg.C for 10 hours to obtain composite xerogel (0.16-0.30 mm); and coating the surface of the composite xerogel particles with an encapsulating material, and drying at 40-50 ℃ for 8-10 hours to obtain 7g of the composite xerogel sustained-release chloride ion curing agent.
The appearance diagram of the obtained composite xerogel sustained-release type chloride ion curing agent is shown in figure 1, and the microscopic gel skeleton diagram is shown in figure 2.
Example 2: a composite xerogel slow-release chloride ion curing agent comprises the following raw materials: 3g of barium acetate, 5g of methyl orthosilicate, 7g of propylene oxide, 20g of solvent and 4g of packaging material to obtain 4.7g of composite xerogel slow-release chloride ion curing agent.
Example 3: a composite xerogel slow-release chloride ion curing agent comprises the following raw materials: 5g of barium nitrate, 10g of tetraethoxysilane, 15g of propylene oxide, 30g of solvent and 8g of packaging material to obtain 8.9g of composite xerogel sustained-release chloride ion curing agent.
Example 4: a composite xerogel slow-release chloride ion curing agent comprises the following raw materials: 2g of barium nitrate, 4g of methyl orthosilicate, 8g of propylene oxide, 30g of solvent and 6g of packaging material to obtain 5g of composite xerogel slow-release chloride ion curing agent.
Example 5: a composite xerogel slow-release chloride ion curing agent comprises the following raw materials: 3g of barium nitrate, 10g of methyl orthosilicate, 7g of propylene oxide, 30g of solvent and 7g of packaging material to obtain 7.6g of composite xerogel slow-release chloride ion curing agent.
Example 6: a composite xerogel slow-release chloride ion curing agent comprises the following raw materials: 5g of barium acetate, 5g of tetraethoxysilane, 15g of propylene oxide, 20g of solvent and 7g of packaging material to obtain 6.6g of composite xerogel slow-release chloride ion curing agent.
Example 7:
a chloride ion curing agent is prepared from the following raw materials: 4g of barium source, 4g of organosilicon source, 12g of propylene oxide, 25g of solvent and 6g of packaging material to obtain 5g of chloride ion curing agent.
Example 8:
a chloride ion curing agent is prepared from the following raw materials: 2g of barium source, 8g of organosilicon source, 12g of propylene oxide, 25g of solvent and 6g of packaging material to obtain 5.2g of chloride ion curing agent.
Example 9:
a chloride ion curing agent is prepared from the following raw materials: 4g of barium source, 8g of organosilicon source, 6g of propylene oxide, 25g of solvent and 6g of packaging material to obtain 6.2g of chloride ion curing agent.
Example 10:
a chloride ion curing agent is prepared from the following raw materials: 4g of barium source, 8g of organosilicon source, 12g of ethylene oxide, 25g of solvent and 6g of packaging material to obtain 5.8g of chloride ion curing agent.
Example 11:
a chloride ion curing agent is prepared from the following raw materials: 4g of barium source, 8g of inorganic silicon source, 12g of propylene oxide, 25g of solvent and 6g of packaging material to obtain 5.4g of chloride ion curing agent.
Example 12:
a chloride ion curing agent is prepared from the following raw materials: 4g of barium source, 8g of organosilicon source, 12g of propylene oxide, 25g of water and 6g of packaging material to obtain 5g of chloride ion curing agent.
Example 13:
a chloride ion curing agent is prepared from the following raw materials: 4g of barium source, 8g of organosilicon source, 25g of solvent and 6g of packaging material to obtain 5.4g of chloride ion curing agent.
Example 14
A chloride ion curing agent is prepared from the following raw materials: 4g of barium acetate, 0g of tetraethoxysilane, 12g of propylene oxide, 25g of solvent and 6g of packaging material to obtain 3.8g of chloride ion curing agent.
Examples 2-14 were prepared with reference to the preparation method of example 1.
3g of the curing agent prepared in the examples 1-14 are respectively and evenly mixed with 300g of cement, 650g of sand, 135g of deionized water and 3.51g of NaCl, and are respectively recorded as the experimental groups 1-14.
The control group was set to 300g of cement, 650g of sand, 135g of deionized water, and 3.51g of NaCl.
The curing effect of the curing agent prepared in examples 1 to 14 on chloride ions was measured by the following method: 3.51g of sodium chloride was added to each of the test groups 1 to 14, and the chloride ion content was measured at 7 days, 14 days and 28 days, respectively, to calculate the chloride ion curing rate. The results were measured as follows:
the standard for measuring chloride ions adopts JCJT 322-2013 technical procedure for detecting chloride ion content in concrete.
Figure DEST_PATH_IMAGE001
From the above analysis, it can be seen that:
when no silicon source is added, the slow release effect of the curing agent is extremely poor due to no slow release effect of the silica gel, the barium ions are basically released within seven days, the curing rate of the chloride ions reaches 51.46% in 7 days, but the curing rate of the chloride ions is hardly improved in 14 days and 28 days, the slow release effect of the barium ions is poor, the cement is quickly solidified, and the curing agent cannot be applied in practical operation.
When the silicon source amount is less, the silicon gel is worse in wrapping, the barium ion release speed is higher, the chlorine ion curing effect is improved very little in 14 days and 28 days later, the barium ion slow release effect is poor, and the cement setting speed is accelerated.
When inorganic silicon is selected as the silicon source, the structure of the curing agent is damaged due to larger shrinkage, barium ions are quickly released, the curing effect of chlorine ions is not obviously improved in 14 days and 28 days, the barium ions have no slow-release effect, and the setting speed of cement is accelerated.
When no catalyst is added, the silicon source is slow in hydrolysis speed, the co-gelation effect is difficult to achieve, the barium gel is agglomerated, the release speed of barium ions is high, the curing effect of chloride ions is not obviously improved in 14 days and 28 days, the barium ions have no slow release effect, and the cement is quickly coagulated.
When the catalyst amount is insufficient, the hydrolysis speed of the silicon source is slower, so that the complete cogel is not caused, the barium gel is partially agglomerated, the release speed of the barium ions is faster, the curing effect of the chloride ions is not obviously improved in 14 days and 28 days, the slow release effect of the barium ions is not obvious, and the setting speed of the cement is accelerated.
When the solvent is water, the curing agent is difficult to achieve the cogel effect due to no high polarity of acetonitrile to accelerate and balance the hydrolysis speed, so that the barium gel is agglomerated, the release speed of barium ions is high, the curing effect of chloride ions is not obviously improved in 14 days and 28 days, the barium ions have no slow release effect, and the cement is quickly coagulated.
When the amount of the barium source is small, the whole chloride ion curing rate is low because insufficient barium is released into the pore liquid, the chloride ion curing effect is not obviously improved in 14 days and 28 days, the barium ion has no slow release effect, and the curing effect of the curing agent is poor.
When ethylene oxide is selected as the catalyst, the poor balance of hydrolysis speed leads to difficult cogelling, barium ion agglomeration, high release speed of barium ion and curing of chloride ion within 7 days, but causes faster coagulation of cement, and can not be applied in practical operation.
Finally, it is noted that the above-mentioned embodiments are merely for illustrating the technical solution of the present invention, and that other modifications and equivalents thereof by those skilled in the art should be included in the scope of the claims of the present invention without departing from the spirit and scope of the technical solution of the present invention.

Claims (8)

1. A composite xerogel slow-release type chloride ion curing agent is characterized in that, by weight,
the raw materials used are: 3-5 parts of barium source, 5-10 parts of organic silicon source, 7-15 parts of catalyst, 20-30 parts of solvent and 4-8 parts of packaging material;
the solvent is a mixed solution of acetonitrile and deionized water, and the catalyst is propylene oxide.
2. The chloride ion curing agent of claim 1, wherein: the organic silicon source is one or two of methyl orthosilicate or ethyl orthosilicate; the barium source is one or two of barium acetate and barium nitrate.
3. The chloride ion curing agent of claim 1, wherein: the packaging material is one or two of silica sol and gelatin.
4. A method for preparing the composite xerogel sustained-release chloride ion curing agent according to claim 1, which is characterized by comprising the following steps:
1) Taking the raw materials according to a proportion;
2) Dissolving an organosilicon source in a solvent, and adding 30-40% of catalyst to form a solution A;
3) Dissolving a barium source in a solvent to form a solution B;
4) Adding the solution A into the solution B, stirring, and adding the rest catalyst to form a solution C;
5) Drying the solution C, standing, fishing out, soaking in absolute ethyl alcohol, fishing out, and drying at low temperature and then at high temperature to obtain a composite xerogel;
6) Crushing the composite xerogel to obtain composite xerogel particles;
7) Coating or spraying packaging materials on the surfaces of the composite xerogel particles, and drying to obtain the composite xerogel sustained-release chloride ion curing agent.
5. The method of manufacturing according to claim 4, wherein: the drying temperature of the solution C in the step 5) is 30-50 ℃, the soaking time is 2-3d, the temperature during low-temperature drying is 30-50 ℃, and the temperature during high-temperature drying is 100-120 ℃.
6. The method of manufacturing according to claim 4, wherein: the particle size of the composite xerogel particles in the step 6) is 0.16-0.30mm; the temperature during the drying in the step 7) is 40-50 ℃ and the time is 8-10h.
7. The use of the composite xerogel sustained-release chloride ion curing agent of claim 1 as a chloride ion curing agent in cement-based materials.
8. The use according to claim 7, characterized in that: the composite xerogel slow-release chloride ion curing agent is added into the cement-based material in an amount which is 1-5% of the total amount of the cementing material.
CN202211170098.6A 2022-09-26 2022-09-26 Composite xerogel slow-release chloride ion curing agent and preparation and application thereof Active CN115466067B (en)

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CN112125571A (en) * 2020-09-27 2020-12-25 武汉理工大学 Porous ceramic supported chloride ion curing agent and preparation method and application thereof

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WO2015131333A1 (en) * 2014-03-04 2015-09-11 深圳大学 Chlorine ion triggered microcapsule and preparation method thereof
CN110255951B (en) * 2019-04-11 2021-11-02 武汉理工大学 Barium-based chloride ion curing agent and preparation method and application thereof
CN111925157A (en) * 2020-07-08 2020-11-13 中国电力科学研究院有限公司 Chloride ion curing method for concrete
CN112142355B (en) * 2020-09-27 2022-05-06 武汉理工大学 Expanded perlite supported chloride ion curing agent and preparation method and application thereof

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