CN111233362A - Preparation method and application of concrete toughening material - Google Patents
Preparation method and application of concrete toughening material Download PDFInfo
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- CN111233362A CN111233362A CN202010219465.1A CN202010219465A CN111233362A CN 111233362 A CN111233362 A CN 111233362A CN 202010219465 A CN202010219465 A CN 202010219465A CN 111233362 A CN111233362 A CN 111233362A
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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
- 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
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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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
- C04B14/00—Use 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
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/10—Clay
- C04B14/106—Kaolin
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
Abstract
The invention discloses a preparation method of a concrete toughening material, which is characterized in that after nano-scale halloysite obtained by short cutting is added with a dispersant to be fully dispersed, the halloysite is sequentially mixed with cyanuric chloride in tetrahydrofuran to react to introduce active chlorine atoms, reacts with 1, 3-propane diamine in an organic solvent to substitute the active chlorine atoms to introduce active amino, reacts with succinic anhydride in the organic solvent to introduce carboxyl groups to generate activated halloysite serving as the concrete toughening material.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method and application of a concrete toughening material.
Background
The conventional concrete has low bending strength, and cracks can be formed in the concrete of special building structures such as tunnel arch walls, viaduct bridge decks and the like under complex stress environments, and can be broken in severe cases, so that the service life of the concrete is greatly reduced, and the safety of buildings is endangered. Therefore, it is necessary to add a toughening material to ordinary concrete in a targeted manner, and to perform toughening and reinforcing treatment on the ordinary concrete so as to meet the use requirements in a special stress environment.
In the prior art, aiming at the problem of insufficient concrete toughness, the strength and toughness of concrete are usually changed by adding materials into the concrete, halloysite is an additive material which is paid attention in recent years and is commonly used for improving the toughness and the strength of the concrete, the halloysite is usually mechanically crushed and modified and then added into the concrete, but the halloysite has a large number of hydroxyl groups on the surface, the hydroxyl groups are tightly attached to the surface of the halloysite in a covalent bond form, and the strong hydrogen bonding between the hydroxyl groups causes poor dispersibility, easy agglomeration and poor toughening effect of the halloysite or kaolin and the like; if only mechanical crushing is carried out or any functional group which cannot overcome the problems of poor dispersibility and the like is combined on the halloysite, the halloysite can still not be fully dispersed after being added into concrete and can be uniformly mixed with other concrete components to achieve the toughening effect.
Disclosure of Invention
The invention aims to provide a preparation method and application of a concrete toughening material aiming at the defects of the prior art, wherein halloysite is modified to obtain activated halloysite with carboxyl on the surface, and the modified activated halloysite has good dispersibility, can be fully dispersed in concrete and endows the concrete with good toughness, isotropy and fatigue resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a concrete toughening material comprises the steps of adding a dispersing agent into nanoscale halloysite obtained by short cutting to fully disperse the halloysite, sequentially mixing the halloysite with cyanuric chloride in tetrahydrofuran to react, introducing active chlorine atoms, reacting with 1, 3-propane diamine in an organic solvent to substitute the active chlorine atoms, introducing active amino, reacting with succinic anhydride in the organic solvent to introduce carboxyl groups, and generating the activated halloysite serving as the concrete toughening material.
Further, the halloysite has an average length of 180-200 nm.
Further, the dispersing agent is Tween-40 aqueous solution.
Further, the organic solvent in the reaction of the halloysite and 1, 3-propane diamine is N-methyl pyrrolidone, and the organic solvent in the reaction of the halloysite and succinic anhydride is N, N' -dimethylformamide.
Further, the preparation method of the concrete toughening material comprises the following specific steps:
(1) chopping: cutting a halloysite tube into short pieces, mechanically crushing to obtain nanoscale halloysite, and screening by a 400-mesh sieve for later use;
(2) dispersing and purifying: adding the halloysite subjected to short-cut treatment into a Tween-40 aqueous solution, performing ultrasonic treatment for 12h for dispersion and purification, filtering, washing the halloysite with water, and performing vacuum drying at 65-67 ℃ for 6h for later use;
(3) mixing halloysite subjected to dispersion purification treatment and cyanuric chloride in tetrahydrofuran, stirring at 2-3 ℃ for 12h, performing ultrasonic treatment at 2-3 ℃ for 2h, reacting at 2-3 ℃ for 36h, washing with tetrahydrofuran, and vacuum drying at 10-12 ℃ for 24 h;
(4) putting the halloysite treated in the step (3) into N-methyl pyrrolidone for 0.5h of ultrasound at 10-12 ℃, slowly dropwise adding 1, 3-propane diamine into a mixed solution of N-methyl pyrrolidone and halloysite at 10-12 ℃ for 1h, stirring for reaction for 1h, heating to 90-92 ℃ under the protection of nitrogen, reacting for 2h at constant temperature, evaporating to remove the solvent, cleaning with anhydrous acetone, and drying in vacuum at 45-50 ℃ for 24 h;
(5) and (3) putting the halloysite treated in the step (4) into N, N '-dimethylformamide, performing ultrasonic treatment at 25-27 ℃ for 0.5h, slowly dropwise adding 0.8mol/L anhydrous ethanol solution of succinic anhydride into the mixed solution of the N, N' -dimethylformamide and the halloysite within 2h at 25-27 ℃, stirring for reaction for 2h, filtering, washing with anhydrous ethanol, and performing vacuum drying at 50-55 ℃ for 24h to obtain the activated halloysite with carboxyl on the surface.
Further, the mass concentration of the Tween-40 aqueous solution in the step (2) is 12%, and the pH value is 8-9.
The invention has the beneficial effects that:
1. according to the invention, the nano-scale halloysite obtained after the short-cut treatment sequentially reacts with cyanuric chloride, 1, 3-propane diamine and succinic anhydride to carry out chemical modification, and finally the activated halloysite with extended surface functional groups and carboxyl groups is prepared; in the preparation process of the activated halloysite, on one hand, the nucleophilic substitution reaction is a method for prolonging the chemical structure of surface molecules, so that groups to be reacted on the surface of the halloysite are prolonged from the outer-layer pipe wall or pipe end of the halloysite, the steric hindrance between molecules is increased, and the dispersibility of the halloysite in a medium (particularly water) is further improved; on the other hand, a carboxyl functional group is introduced to the surface of the finally prepared halloysite, and the carboxyl is a strong hydrophilic group, so that the dispersibility of the halloysite in water is improved; in conclusion, the activated halloysite finally prepared by combining the two modification modes can effectively weaken the agglomeration phenomenon on the surface of the halloysite due to the existence of hydroxyl groups, effectively improve the dispersibility of the halloysite in the medium water used in the concrete preparation process, facilitate the full dispersion of the halloysite in the concrete, and endow the concrete with good toughness, isotropy and fatigue resistance.
2. According to the invention, cyanuric chloride is selected to be used because three chlorine atoms in cyanuric chloride molecules are very active and have different reactivity, the cyanuric chloride can be substituted by a nucleophilic reagent under the condition of controlling the reaction temperature, halloysite and cyanuric chloride are mixed in tetrahydrofuran under the condition of controlling the substitution reaction temperature to be 2-3 ℃, hydroxyl on the surface of the halloysite can generate nucleophilic substitution reaction with the chlorine atoms in the cyanuric chloride, a triazine ring containing two active chlorine atoms is introduced to the surface of the halloysite, and the halloysite with a triazine ring structure containing two active chlorine atoms on the surface obtained through the reaction provides a reactive group for next modification; at the same time, the nucleophilic substitution reaction that occurs lengthens the molecular chemical structure of the halloysite surface.
3. According to the invention, the nucleophilic substitution reaction is carried out again on the 1, 3-propane diamine and two active chlorine atoms on the triazine ring on the surface of the halloysite to obtain the halloysite with the triazine ring structure containing active amino, so that a reaction group is provided for the next step of continuous modification, and meanwhile, the secondary nucleophilic substitution reaction can continuously prolong the molecular chemical structure on the surface of the halloysite.
4. In the invention, succinic anhydride is selected to react with the modified halloysite with active amino on the surface in an N, N' -dimethylformamide organic solvent, the succinic anhydride provides a large amount of carboxyl groups, the succinic anhydride reacts with active amino on a triazine ring structure on the surface of the halloysite after ring opening reaction to generate amido bonds, the ring-opened succinic anhydride molecular structure with carboxyl at the tail end is introduced to the surface of the halloysite through the amido bonds, and finally the halloysite with carboxyl on the surface is obtained, the carboxyl is a strong hydrophilic group, thus the dispersibility of the halloysite in water can be improved, meanwhile, the reaction of the succinic anhydride after ring opening and the active amino on the triazine ring structure on the surface of the halloysite is also a method for prolonging the chemical structure of the surface molecule, which can further prolong the reaction groups from the outer layer or the pipe end of the halloysite, the steric hindrance between molecules can be further increased, and the dispersibility of the halloysite in a medium (particularly water) can be further improved.
5. The Tween-40 is used for dispersing and purifying the nanoscale halloysite, so that the nanoscale halloysite can be effectively dispersed in an aqueous solution, and impurities in the nanoscale halloysite are removed.
6. The toughened material prepared by the method provided by the invention can be quickly and fully mixed with other concrete component materials to be uniformly dispersed, and then the toughened concrete material is obtained after standard curing. Adopts the basic mixture ratio of C40 concrete and 3.9kg/m of water reducing agent3And the toughening material is 1.5Kg/m3The prepared concrete standard sample has the compressive strength improved to 44.6MPa, the flexural strength improved to 8.35MPa and the bending ratio reduced to 5.34, so that the concrete material has high toughness, isotropy, fatigue resistance and other performances.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples.
The halloysite is commercially available, and the main specifications of the halloysite are as follows: the characteristics are as follows: a white powder; density: 2.4-2.5g/cm3(ii) a Comprises the following components: SiO 22：58.23、Al2O3：40.96、Fe2O3：0.34、TiO2：0.15、P2O5: 0.14; the outer diameter of the tube is as follows: 40-60 nm; pipe inner diameter: 15-20 nm; length:<1.1 μm; specific surface area: 52.6m2/g；
The Tween-40(CAS No.9005-66-7) is commercially available, and the main specifications thereof are as follows: the characteristics are as follows: an amber oil-like liquid; acid value (KOHmg/g): less than or equal to 2.0; hydroxyl value (KOHmg/g): 85-100 parts of; HLB value: 15.5; saponification number (KOHmg/g): 40-55; water content (%): less than or equal to 2.5;
the cyanuric chloride, the 1, 3-propane diamine, the succinic anhydride, the anhydrous acetone and the anhydrous ethanol are all commercially available chemical pure reagents.
Example 1
A preparation method of a concrete toughening material comprises the following specific steps:
(1) chopping: cutting a halloysite tube, mechanically crushing to obtain a nanoscale halloysite with the average length of 180nm, and screening by a 400-mesh screen for later use;
(2) dispersing and purifying: adding the halloysite after the short-cut treatment into a Tween-40 aqueous solution with the pH of 8 and the mass concentration of 12% for ultrasonic treatment for 12h for dispersion and purification, filtering, washing the halloysite with water, and drying in vacuum at 67 ℃ for 6h for later use;
wherein, the Tween-40 is a dispersant, and the Tween-40 is used for treating the nanoscale halloysite which has high surface energy and is easy to agglomerate, so that the halloysite can be effectively dispersed in an aqueous solution, and impurities in the halloysite can be removed;
(3) mixing halloysite subjected to dispersion purification treatment and cyanuric chloride in tetrahydrofuran, wherein the tetrahydrofuran is used as an organic solvent, the cyanuric chloride is easily dissolved in the tetrahydrofuran, stirring for 12h at 2 ℃, performing ultrasonic treatment for 2h at 2 ℃, reacting for 36h at 2 ℃, washing with the tetrahydrofuran, and performing vacuum drying for 24h at 10 ℃ to obtain halloysite with a triazine ring structure containing two active chlorine atoms on the surface, so as to provide a reactive group for next modification;
(4) taking halloysite with a triazine ring structure containing two active chlorine atoms on the surface, which is obtained after the treatment in the step (3), placing the halloysite in N-methyl pyrrolidone for 0.5h at 10 ℃, slowly dropwise adding 1, 3-propane diamine at 10 ℃ within 1h, stirring for reaction for 1h, heating to 90 ℃ under the protection of nitrogen for constant-temperature reaction for 2h, evaporating to remove the solvent, washing with anhydrous acetone, and drying in vacuum at 45 ℃ for 24h to obtain the halloysite with the triazine ring structure containing active amino on the surface, and continuously providing a reactive group for the next modification;
(5) and (3) taking halloysite with a triazine ring structure containing active amino on the surface obtained after the treatment in the step (4), placing the halloysite in N, N' -dimethylformamide for 0.5h at 25 ℃, slowly dropwise adding 0.8mol/L anhydrous ethanol solution of succinic anhydride within 2h at 25 ℃, stirring for reaction for 2h, filtering, washing with anhydrous ethanol, and performing vacuum drying at 50 ℃ for 24h to obtain the activated halloysite with carboxyl on the surface.
Example 2
A preparation method of a concrete toughening material comprises the following specific steps:
(1) chopping: cutting a halloysite tube into short pieces, mechanically crushing to obtain halloysite with the average length of 190nm and screening by a 400-mesh sieve for later use;
(2) dispersing and purifying: adding the halloysite after the short-cut treatment into a Tween-40 aqueous solution with the pH of 9 and the mass concentration of 12% for ultrasonic treatment for 12h for dispersion and purification, filtering, washing the halloysite with water, and performing vacuum drying at 65 ℃ for 6h for later use;
wherein, the Tween-40 is a dispersant, and the Tween-40 is used for treating the nanoscale halloysite which has high surface energy and is easy to agglomerate, so that the halloysite can be effectively dispersed in an aqueous solution, and impurities in the halloysite can be removed;
(3) mixing halloysite subjected to dispersion purification treatment and cyanuric chloride in tetrahydrofuran, wherein the tetrahydrofuran is used as an organic solvent, the cyanuric chloride is easily dissolved in the tetrahydrofuran, stirring the mixture at the temperature of 3 ℃ for 12h, performing ultrasonic treatment at the temperature of 3 ℃ for 2h, then reacting at the temperature of 3 ℃ for 36h, washing the mixture by the tetrahydrofuran, and performing vacuum drying at the temperature of 11 ℃ for 24h to obtain halloysite with a triazine ring structure containing two active chlorine atoms on the surface, so as to provide a reactive group for next modification;
(4) taking halloysite with a triazine ring structure containing two active chlorine atoms on the surface, which is obtained after treatment in the step (3), placing the halloysite in N-methyl pyrrolidone for 0.5h under ultrasound at 12 ℃, slowly dropwise adding 1, 3-propane diamine into a mixed solution of N-methyl pyrrolidone and halloysite at 12 ℃ within 1h, stirring for reaction for 1h, heating to 92 ℃ under the protection of nitrogen for constant-temperature reaction for 2h, evaporating to remove a solvent, washing with anhydrous acetone, and vacuum drying at 50 ℃ for 24h to obtain the halloysite with the triazine ring structure containing active amino on the surface, and continuously providing a reactive group for next modification;
(5) and (3) taking halloysite with a triazine ring structure containing active amino on the surface obtained after the treatment in the step (4), placing the halloysite in N, N' -dimethylformamide for 0.5h at 27 ℃, slowly dropwise adding 0.8mol/L anhydrous ethanol solution of succinic anhydride within 2h at 27 ℃, stirring for reaction for 2h, filtering, washing with anhydrous ethanol, and performing vacuum drying at 55 ℃ for 24h to obtain the activated halloysite with carboxyl on the surface.
Example 3
A preparation method of a concrete toughening material comprises the following specific steps:
(1) chopping: cutting a halloysite tube, mechanically crushing to obtain a nanoscale halloysite with the average length of 200nm, and screening by a 400-mesh sieve for later use;
(2) dispersing and purifying: adding the halloysite after the short-cut treatment into a Tween-40 aqueous solution with the pH of 8 and the mass concentration of 12% for ultrasonic treatment for 12h for dispersion and purification, filtering, washing the halloysite with water, and drying in vacuum at 66 ℃ for 6h for later use;
wherein, the Tween-40 is a dispersant, and the Tween-40 is used for treating the nanoscale halloysite which has high surface energy and is easy to agglomerate, so that the halloysite can be effectively dispersed in an aqueous solution, and impurities in the halloysite can be removed;
(3) mixing halloysite subjected to dispersion purification treatment and cyanuric chloride in tetrahydrofuran, wherein the tetrahydrofuran is used as an organic solvent, the cyanuric chloride is easily dissolved in the tetrahydrofuran, stirring the mixture at the temperature of 2 ℃ for 12h, performing ultrasonic treatment at the temperature of 3 ℃ for 2h, then reacting at the temperature of 3 ℃ for 36h, washing the mixture by the tetrahydrofuran, and performing vacuum drying at the temperature of 12 ℃ for 24h to obtain halloysite with a triazine ring structure containing two active chlorine atoms on the surface, so as to provide a reactive group for next modification;
(4) taking halloysite with a triazine ring structure containing two active chlorine atoms on the surface, which is obtained after the treatment in the step (3), placing the halloysite in N-methyl pyrrolidone for 0.5h at 11 ℃, slowly dropwise adding 1, 3-propane diamine at 11 ℃ within 1h, stirring for reaction for 1h, heating to 91 ℃ under the protection of nitrogen for constant-temperature reaction for 2h, evaporating to remove the solvent, washing with anhydrous acetone, and drying in vacuum at 48 ℃ for 24h to obtain the halloysite with the triazine ring structure containing active amino on the surface, and continuously providing a reactive group for the next modification;
(5) and (3) taking halloysite with a triazine ring structure containing active amino on the surface obtained after the treatment in the step (4), placing the halloysite in N, N' -dimethylformamide for ultrasonic treatment at 26 ℃ for 0.5h, slowly dropwise adding 0.8mol/L anhydrous ethanol solution of succinic anhydride at 26 ℃ within 2h, stirring for reaction for 2h, filtering, washing with anhydrous ethanol, and performing vacuum drying at 53 ℃ for 24h to obtain the activated halloysite with carboxyl on the surface.
In summary, the toughening materials prepared by the preparation methods of the embodiments 1 to 3 adopt the basic mixture ratio of C40 concrete and the water reducing agent is 3.9kg/m3And 1.5kg/m3The prepared concrete standard sample is tested, and the following performance indexes are obtained in the following table (1):
TABLE 1 Performance index of concrete with toughening materials prepared according to different embodiments of the present invention
As can be seen from the above Table (1), the compression-fracture ratio of the concrete with the toughening material prepared according to the present invention is significantly reduced compared to the concrete without the toughening material, which indicates that the toughening material prepared according to the present invention can significantly improve the toughness of the concrete.
The toughening material prepared by the preparation method of the embodiment 1 adopts the basic mixture ratio of C40 concrete and the water reducing agent is 3.9kg/m3And toughening materials with different addition amounts are added, and the prepared concrete standard samples are tested to obtain the performance indexes as the following table (2):
TABLE 2 concrete Performance index of different addition amounts of toughening materials in concrete
It can be seen from the above table (2) that the folding ratio of the obtained concrete is 7.12 when the common hydroxyl halloysite is added into the concrete, and the more the modified halloysite prepared by the present invention is added into the concrete as the toughening material, the folding ratio of the obtained concrete is gradually reduced, and obviously, the toughness of the concrete can be obviously improved when the modified halloysite is used as the toughening material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of a concrete toughening material is characterized by comprising the following steps: after a dispersing agent is added into nanoscale halloysite obtained by short cutting to fully disperse the halloysite, the halloysite is sequentially mixed with cyanuric chloride in tetrahydrofuran to react to introduce active chlorine atoms, reacts with 1, 3-propane diamine in an organic solvent to substitute the active chlorine atoms to introduce active amino, reacts with succinic anhydride in the organic solvent to introduce carboxyl groups to generate activated halloysite which is used as a concrete toughening material.
2. The method for preparing a concrete toughening material according to claim 1, wherein: the halloysite has an average length of 180-200 nm.
3. The method for preparing a concrete toughening material according to claim 2, wherein: the dispersant is Tween-40 aqueous solution.
4. A method for preparing a concrete toughening material according to claim 3, wherein: the organic solvent in the reaction of the halloysite and 1, 3-propane diamine is N-methyl pyrrolidone, and the organic solvent in the reaction of the halloysite and succinic anhydride is N, N' -dimethylformamide.
5. The preparation method of the concrete toughening material according to claim 4, characterized by comprising the following steps:
(1) chopping: cutting a halloysite tube into short pieces, mechanically crushing to obtain nanoscale halloysite, and screening by a 400-mesh sieve for later use;
(2) dispersing and purifying: adding the halloysite subjected to short-cut treatment into a Tween-40 aqueous solution, performing ultrasonic treatment for 12h for dispersion and purification, filtering, washing the halloysite with water, and performing vacuum drying at 65-67 ℃ for 6h for later use;
(3) mixing halloysite subjected to dispersion purification treatment and cyanuric chloride in tetrahydrofuran, stirring at 2-3 ℃ for 12h, performing ultrasonic treatment at 2-3 ℃ for 2h, reacting at 2-3 ℃ for 36h, washing with tetrahydrofuran, and vacuum drying at 10-12 ℃ for 24 h;
(4) putting the halloysite treated in the step (3) into N-methyl pyrrolidone for 0.5h of ultrasound at 10-12 ℃, slowly dropwise adding 1, 3-propane diamine into a mixed solution of N-methyl pyrrolidone and halloysite at 10-12 ℃ for 1h, stirring for reaction for 1h, heating to 90-92 ℃ under the protection of nitrogen, reacting for 2h at constant temperature, evaporating to remove the solvent, cleaning with anhydrous acetone, and drying in vacuum at 45-50 ℃ for 24 h;
(5) and (3) putting the halloysite treated in the step (4) into N, N '-dimethylformamide, performing ultrasonic treatment at 25-27 ℃ for 0.5h, slowly dropwise adding 0.8mol/L anhydrous ethanol solution of succinic anhydride into the mixed solution of the N, N' -dimethylformamide and the halloysite within 2h at 25-27 ℃, stirring for reaction for 2h, filtering, washing with anhydrous ethanol, and performing vacuum drying at 50-55 ℃ for 24h to obtain the activated halloysite with carboxyl on the surface.
6. The method for preparing a concrete toughening material according to claim 5, wherein: the mass concentration of the Tween-40 aqueous solution in the step (2) is 12%, and the pH value is 8-9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113073800A (en) * | 2021-03-23 | 2021-07-06 | 江苏苏邑设计集团有限公司 | Waterproof anti-crack outer wall insulation structure of building |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101093559B1 (en) * | 2010-10-28 | 2011-12-13 | 한국지질자원연구원 | Method of preparing halloysite microtubules |
| CN104058398A (en) * | 2014-07-15 | 2014-09-24 | 福建江夏学院 | Modified graphene and preparation method thereof |
| CN106045404A (en) * | 2016-06-08 | 2016-10-26 | 福建江夏学院 | Environment-friendly pervious recycled aggregate concrete and preparation method thereof |
| CN107056123A (en) * | 2017-05-31 | 2017-08-18 | 福建江夏学院 | A kind of concrete activeness and quietness composite and preparation method thereof |
| CN107200491A (en) * | 2017-05-31 | 2017-09-26 | 福建江夏学院 | Concrete toughness reinforcing modified galapectite and preparation method thereof |
| CN109890755A (en) * | 2016-10-25 | 2019-06-14 | 杰富意矿物股份有限公司 | Surface modification galapectite, the manufacturing method of surface modification galapectite and catalysis reaction |
| CN109961962A (en) * | 2017-12-25 | 2019-07-02 | 南京理工大学 | Load the preparation method of the galapectite electrode material of Ni, Mn oxide and curing nickel |
-
2020
- 2020-03-25 CN CN202010219465.1A patent/CN111233362A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101093559B1 (en) * | 2010-10-28 | 2011-12-13 | 한국지질자원연구원 | Method of preparing halloysite microtubules |
| CN104058398A (en) * | 2014-07-15 | 2014-09-24 | 福建江夏学院 | Modified graphene and preparation method thereof |
| CN106045404A (en) * | 2016-06-08 | 2016-10-26 | 福建江夏学院 | Environment-friendly pervious recycled aggregate concrete and preparation method thereof |
| CN109890755A (en) * | 2016-10-25 | 2019-06-14 | 杰富意矿物股份有限公司 | Surface modification galapectite, the manufacturing method of surface modification galapectite and catalysis reaction |
| CN107056123A (en) * | 2017-05-31 | 2017-08-18 | 福建江夏学院 | A kind of concrete activeness and quietness composite and preparation method thereof |
| CN107200491A (en) * | 2017-05-31 | 2017-09-26 | 福建江夏学院 | Concrete toughness reinforcing modified galapectite and preparation method thereof |
| CN109961962A (en) * | 2017-12-25 | 2019-07-02 | 南京理工大学 | Load the preparation method of the galapectite electrode material of Ni, Mn oxide and curing nickel |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113073800A (en) * | 2021-03-23 | 2021-07-06 | 江苏苏邑设计集团有限公司 | Waterproof anti-crack outer wall insulation structure of building |
| CN113073800B (en) * | 2021-03-23 | 2022-03-01 | 苏邑设计集团有限公司 | Waterproof anti-crack outer wall insulation structure of building |
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