CN114029447A - Hardening accelerator and preparation method thereof - Google Patents

Hardening accelerator and preparation method thereof Download PDF

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Publication number
CN114029447A
CN114029447A CN202111424068.9A CN202111424068A CN114029447A CN 114029447 A CN114029447 A CN 114029447A CN 202111424068 A CN202111424068 A CN 202111424068A CN 114029447 A CN114029447 A CN 114029447A
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Prior art keywords
hardening accelerator
hardening
catalyst
parts
cross
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CN202111424068.9A
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Chinese (zh)
Inventor
陈群
程楠
陈腾飞
宋陶然
马欣
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Jinnaiyuan Henan Industrial Technology Co ltd
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Jinnaiyuan Henan Industrial Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
    • B22C1/02—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by additives for special purposes, e.g. indicators, breakdown additives
    • B22C1/10—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by additives for special purposes, e.g. indicators, breakdown additives for influencing the hardening tendency of the mould material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
    • B22C1/16—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents
    • B22C1/20—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents
    • B22C1/22—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of resins or rosins
    • B22C1/2233—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of organic agents of resins or rosins obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • B22C1/2246—Condensation polymers of aldehydes and ketones
    • B22C1/2253—Condensation polymers of aldehydes and ketones with phenols
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages
    • C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
    • C07F7/1804—Compounds having Si-O-C linkages
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages
    • C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
    • C07F7/1804—Compounds having Si-O-C linkages
    • C07F7/1872—Preparation; Treatments not provided for in C07F7/20
    • C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888

Abstract

The invention discloses a hardening accelerator and a preparation method thereof, relating to the field of hardening accelerators2When the phenolic resin is hardened, the sensitivity is low, the air blowing hardening time is long, and the condensation speed is slow; the hardening accelerator can increase the content of phenolic resin binder CO2The sensitivity of gas hardening is shortened, the blowing hardening time is shortened, the technological strength of the adhesive is greatly improved, the hardening accelerator is added, the effects of heating, reaction crosslinking, dispersion strengthening and the like are achieved, the plasticity of the phenolic resin is increased, the strength is greatly improved, water participates in the hardening acceleration process, and CO is also improved2The moisture absorption of the hardened phenolic resin can reach the initial strengthThe technical level is more than 1.8MPa, the final strength is more than 5.2MPa, and the product is CO2The popularization and application of the gas hardening phenolic resin creates more favorable conditions.

Description

Hardening accelerator and preparation method thereof
Technical Field
The invention relates to the field of hardening accelerator, in particular to a hardening accelerator and a preparation method thereof.
Background
The casting industry is an important component of the mechanical industry, along with the progress of science and technology and the development of society, large-scale, low-energy consumption, high-efficiency and environment-friendly casting is the inevitable requirement of large-scale production in casting socialization, and the traditional small-scale, high-energy consumption, low-efficiency and high-pollution casting production is inevitably eliminated by indiscriminate market competition.
The cold-box method is a generic name of a resin sand core-making process in which a gas or aerosol catalyst is introduced to rapidly harden resin sand blown into a core box at room temperature, such as a triethylamine method and SO2The cold core box method has the advantages of high efficiency, no need of heating the core box, energy conservation, long service life of the core box and the like, is particularly suitable for the requirement of large-scale core making, is a high-efficiency core making method, and has important significance for developing novel cold core box core making materials and processes which are non-toxic or low-toxic to human bodies and have no pollution or little pollution to the environment in the face of stricter and stricter environmental requirements.
CO is adopted in the prior casting production process2When the phenolic resin is hardened, the sensitivity is low, the air blowing hardening time is long, and the setting speed is slow.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a hardening accelerator and a preparation method thereof:
(1) the calcium hydroxide, the Portland cement, the magnesium oxide and the zinc oxide are weighed and ground into powder, the ground materials are uniformly mixed, and the cross-linking agent is added to obtain the hardening accelerator, so that the problem of adopting CO is solved2When the phenolic resin is hardened, the sensitivity is low, the air blowing hardening time is long, and the condensation speed is slow;
(2) loading an acetic acid solution and chitosan into a three-neck flask, adding a purified and opened carbon nano tube, stirring, refluxing, drying and grinding to obtain a catalyst E, adding a chloroplatinic acid isopropanol solution into absolute ethyl alcohol, mixing catalyst E powder with the absolute ethyl alcohol, then adding ethanol to obtain a catalyst F, placing 9-decene-1-alcohol and the catalyst F into the three-neck flask at the indoor temperature of a fume hood, adding methyl dichlorosilane to obtain an intermediate A, and adding the intermediate A into the intermediate AAdding into a three-neck flask, N2Adding propanol into a three-neck flask under protection to obtain an intermediate B, and adding methacryloyl chloride into the intermediate B to obtain the cross-linking agent, so that the problem of final strength reduction caused by easy generation of cracks during rapid condensation is solved.
The purpose of the invention can be realized by the following technical scheme:
a hardening accelerator comprises the following components in parts by weight:
5-6 parts of calcium hydroxide, 2-3 parts of zinc oxide, 1.5-2 parts of magnesium oxide, 3-4 parts of Portland cement and 1-2 parts of a cross-linking agent;
the hardening accelerator is prepared by the following steps:
s1: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide, and grinding into powder;
s2: uniformly mixing the ground materials, and adding a cross-linking agent to obtain the hardening accelerator;
in CO2The gel formed by the phenolic resin under the action of (1) is a reversible gel, the dissolution can be carried out when the pH value of the solution is increased, the reversible gel molecules are combined by intermolecular force or weaker chemical bonds, the combination capability is not strong, namely, the bonding strength is not high, and the hardening accelerator comprises Ca (OH)2Cement, etc., wherein Ca (OH)2Powder with CO2Gas can generate chemical reaction to generate CaCO3And heat, the heat generated assisting in the dehydration of the gel, allowing a rapid build-up of the green strength of the phenolic resin, Ca (OH)2Generating divalent calcium ions with water, and dissociating Ca from dicalcium silicate, tricalcium silicate, tetracalcium aluminoferrite, etc. in cement2 +And SiO4 -4，Ca2+As a cross-linking bridge with the resin to take part in the subsequent hardening and cross-linking reaction, so that CO2The hardening phenolic resin sand has continuously raised strength and high final strength, and the hardening accelerator has the functions of heating, reaction crosslinking, dispersion strengthening, etc. in the adhesive system and has raised plasticity of phenolic resin, greatly raised strength, water participation in hardening process and greatly improved CO content2Suction of hardened phenolic resinsAnd (4) wetting.
As a further scheme of the invention: the cross-linking agent is prepared by the following steps:
s21: filling acetic acid solution and chitosan into a three-neck flask, stirring and dissolving at 50-60 ℃, adding a purified open-tube carbon nano tube, stirring and refluxing for 45-50min, adding NaOH solution to adjust the pH value to 13, completely depositing the chitosan on the surface of the carbon nano tube, washing precipitates with distilled water until the pH value of filtrate is 8, drying and grinding to obtain a catalyst E;
s22: adding the chloroplatinic acid isopropanol solution into absolute ethyl alcohol to prepare chloroplatinic acid isopropanol-ethanol mixed solution, mixing the catalyst E powder with the mixed solution, adding ethanol, heating and refluxing for 6-7h, and distilling under reduced pressure to obtain a catalyst F;
s23: placing 9-decene-1-alcohol and catalyst F in a three-neck flask at room temperature of 20-25 ℃ in a fume hood, and placing N2Adding methyl dichlorosilane under protection, reacting for 2-4h at normal temperature under magnetic stirring, and sampling after no bubbles are generated to obtain an intermediate A;
the chemical reaction formula is as follows:
Figure BDA0003377553750000031
s24: adding the intermediate A into a three-neck flask, N2Adding propanol into a three-neck flask under protection, heating to 40-50 ℃ under magnetic stirring, reacting for 3-5h, cooling, neutralizing and alcoholyzing by triethylamine until no new precipitate is generated, and filtering to obtain an intermediate B;
the chemical reaction formula is as follows:
Figure BDA0003377553750000041
s25: adding methacryloyl chloride into the intermediate B, reacting for 3-4h at normal temperature under magnetic stirring, neutralizing with triethylamine, and filtering to obtain the cross-linking agent;
the chemical reaction formula is as follows:
Figure BDA0003377553750000051
adding the cross-linking agent to form a stable complex with phenolic resin to generate cross-linking hardening, wherein the silicon-containing cross-linking agent forms a bridge between two benzene rings to form a complex network structure of the whole resin chain and increase the strength of the resin, phenolic hydroxyl in the resin is converted into phenolic hydroxyl negative ions under alkaline conditions to enhance the hydrophilicity of the resin and ensure water solubility, and CO is blown into the resin solution to generate cross-linking hardening2When the alkali content is less than the minimum alkali amount required for stabilizing the resin solution, the stability of the resin solution is damaged, resin molecules are close to each other to be crosslinked with a crosslinking agent and to be coagulated along with the phenolic resin, so that the sand core is hardened to generate certain initial strength, the strength is further strengthened along with continuous gel dehydration of a system, a methacryloxy group is introduced to be polymerized with a resin monomer, a flexible long chain with the main carbon chain length of C9 is added, the chemical bond bonding density of the surface of an adherend can be reduced, the impact energy is well absorbed, the surface energy of the adherend is remarkably reduced, and long-chain silane molecules have the function of interface enhancement and toughening between an organic phase and an inorganic phase.
As a further scheme of the invention: in the step S21, the mass fraction of the acetic acid solution is 1.5%, and the usage ratio of the acetic acid solution, chitosan and carbon nanotubes is 50 mL: 0.8 g: 8.0 g.
As a further scheme of the invention: in the step S22, the concentration of the chloroplatinic acid isopropanol solution is 0.0386mol/L, and the dosage ratio of the chloroplatinic acid isopropanol solution, the absolute ethyl alcohol, the catalyst E and the ethyl alcohol is 3.0 ml: 30.0 ml: 1.0 g: 10 mL.
As a further scheme of the invention: in the step S23, the dosage ratio of the 9-decene-1-ol to the catalyst F to the methyl dichlorosilane is 34 g: 4 g: 27.09 g.
As a further scheme of the invention: the dosage ratio of the intermediate A to the propanol in the step S24 is 57.2 g: 12.8 g.
As a further scheme of the invention: the dosage ratio of the intermediate B to the methacryloyl chloride in the step S25 is 60.8 g: 20.9 g.
A preparation method of a hardening accelerator specifically comprises the following steps:
s81: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide according to the weight parts, and grinding into powder for later use;
s82: uniformly mixing the ground calcium hydroxide, the portland cement, the magnesium oxide and the zinc oxide, and adding a cross-linking agent to obtain the hardening accelerator.
The invention has the beneficial effects that:
(1) the hardening accelerator is prepared by weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide, grinding into powder, uniformly mixing the ground materials, adding a cross-linking agent, and adding a phenolic resin binder CO2The sensitivity of gas hardening is shortened, the air-blowing hardening time is shortened, the technological strength of the adhesive is greatly improved after the air-blowing hardening, the addition of the hardening accelerator can reach the technical level that the initial strength is more than 1.8MPa and the final strength is more than 5.2MPa, and the adhesive strength can also be obviously improved, namely CO2The popularization and application of the gas hardening phenolic resin create more favorable conditions, the hardening accelerator plays roles of heating, reaction crosslinking, dispersion enhancement and the like in a binder system, and increases the plasticity of the phenolic resin, so that the strength of the phenolic resin is greatly improved, and water participates in the hardening acceleration process, thereby greatly improving CO2Moisture absorption of hardened phenolic resin;
(2) loading acetic acid solution and chitosan into a three-mouth flask, adding a carbon nano tube after purification and tube opening to obtain a catalyst E, adding chloroplatinic acid isopropanol solution into absolute ethyl alcohol, mixing catalyst E powder with the absolute ethyl alcohol, then adding ethyl alcohol to obtain a catalyst F, placing 9-decene-1-alcohol and the catalyst F into the three-mouth flask, adding methyl dichlorosilane to obtain an intermediate A, adding the intermediate A into the three-mouth flask, adding propyl alcohol to obtain an intermediate B, adding methacryloyl chloride to the intermediate B to obtain the cross-linking agent, adding the cross-linking agent to form a stable complex with phenolic resin to generate cross-linking and hardening, forming a bridge between two benzene rings by the silicon-containing cross-linking agent to form a complex network structure of the whole resin chain and increase the strength of the resin, when the alkali content is less than the minimum alkali amount required by the stable resin solution, the resin molecules are close to each other to be crosslinked with the crosslinking agent and the phenolic resin is coagulated, so that the sand core is hardened to generate certain initial strength, the strength is further strengthened along with the continuous gel dehydration of the system, a methacryloxy group is introduced to polymerize the methacryloxy group with a resin monomer, and a flexible long chain with the main carbon chain length of C9 has the functions of interface enhancement and toughening between an organic phase and an inorganic phase, so that the chemical bond bonding density of the surface of an adherend can be reduced, the impact energy is well absorbed, and the better final strength is achieved.
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.
Example 1:
the embodiment is a hardening accelerator, which comprises the following components in parts by weight:
5 parts of calcium hydroxide, 2 parts of zinc oxide, 2 parts of magnesium oxide, 4 parts of Portland cement and 2 parts of a cross-linking agent;
the hardening accelerator is prepared by the following steps:
s1: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide, and grinding into powder;
s2: uniformly mixing the ground materials, and adding a cross-linking agent to obtain the hardening accelerator;
the cross-linking agent is prepared by the following steps:
s21: filling acetic acid solution and chitosan into a three-neck flask, stirring and dissolving at 50 ℃, adding a purified and opened carbon nano tube, stirring and refluxing for 45min, adding NaOH solution to adjust the pH value to 13 so that the chitosan is completely deposited on the surface of the carbon nano tube, washing precipitates with distilled water until the pH value of filtrate is 8, drying and grinding to obtain a catalyst E;
s22: adding the chloroplatinic acid isopropanol solution into absolute ethyl alcohol to prepare chloroplatinic acid isopropanol-ethanol mixed solution, mixing the catalyst E powder with the mixed solution, adding ethanol, heating and refluxing for 6 hours, and distilling under reduced pressure to obtain a catalyst F;
s23: placing 9-decene-1-alcohol and catalyst F in a three-neck flask at room temperature of 20 ℃ in a fume hood, and placing N2Adding methyl dichlorosilane under protection, reacting for 2 hours at normal temperature under magnetic stirring, and sampling after no bubbles are generated to obtain an intermediate A;
s24: adding the intermediate A into a three-neck flask, N2Adding propanol into a three-neck flask under protection, heating to 40 ℃ under magnetic stirring, reacting for 3h, cooling, neutralizing and alcoholyzing by triethylamine until no new precipitate is generated, and filtering to obtain an intermediate B;
s25: and adding methacryloyl chloride into the intermediate B, reacting for 3 hours at normal temperature under magnetic stirring, neutralizing with triethylamine, and filtering to obtain the cross-linking agent.
Example 2:
the embodiment is a hardening accelerator, which comprises the following components in parts by weight:
6 parts of calcium hydroxide, 2 parts of zinc oxide, 1.5 parts of magnesium oxide, 3 parts of Portland cement and 1 part of a cross-linking agent;
the hardening accelerator is prepared by the following steps:
s1: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide, and grinding into powder;
s2: uniformly mixing the ground materials, and adding a cross-linking agent to obtain the hardening accelerator;
the cross-linking agent is prepared by the following steps:
s21: filling acetic acid solution and chitosan into a three-neck flask, stirring and dissolving at 50 ℃, adding a purified and opened carbon nano tube, stirring and refluxing for 45min, adding NaOH solution to adjust the pH value to 13 so that the chitosan is completely deposited on the surface of the carbon nano tube, washing precipitates with distilled water until the pH value of filtrate is 8, drying and grinding to obtain a catalyst E;
s22: adding the chloroplatinic acid isopropanol solution into absolute ethyl alcohol to prepare chloroplatinic acid isopropanol-ethanol mixed solution, mixing the catalyst E powder with the mixed solution, adding ethanol, heating and refluxing for 6 hours, and distilling under reduced pressure to obtain a catalyst F;
s23: placing 9-decene-1-alcohol and catalyst F in a three-neck flask at room temperature of 25 ℃ in a fume hood, and placing N2Adding methyl dichlorosilane under protection, reacting for 4 hours at normal temperature under magnetic stirring, and sampling after no bubbles are generated to obtain an intermediate A;
s24: adding the intermediate A into a three-neck flask, N2Adding propanol into a three-neck flask under protection, heating to 50 ℃ under magnetic stirring, reacting for 5h, cooling, neutralizing and alcoholyzing by triethylamine until no new precipitate is generated, and filtering to obtain an intermediate B;
s25: and adding methacryloyl chloride into the intermediate B, reacting for 4 hours at normal temperature under magnetic stirring, neutralizing with triethylamine, and filtering to obtain the cross-linking agent.
Example 3:
the embodiment is a hardening accelerator, which comprises the following components in parts by weight:
6 parts of calcium hydroxide, 3 parts of zinc oxide, 1.5 parts of magnesium oxide, 4 parts of Portland cement and 2 parts of a cross-linking agent;
the hardening accelerator is prepared by the following steps:
s1: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide, and grinding into powder;
s2: uniformly mixing the ground materials, and adding a cross-linking agent to obtain the hardening accelerator;
the cross-linking agent is prepared by the following steps:
s21: filling acetic acid solution and chitosan into a three-neck flask, stirring and dissolving at 60 ℃, adding a purified and opened carbon nano tube, stirring and refluxing for 50min, adding NaOH solution to adjust the pH value to 13 so that the chitosan is completely deposited on the surface of the carbon nano tube, washing precipitates with distilled water until the pH value of filtrate is 8, drying and grinding to obtain a catalyst E;
s22: adding the chloroplatinic acid isopropanol solution into absolute ethyl alcohol to prepare chloroplatinic acid isopropanol-ethanol mixed solution, mixing the catalyst E powder with the mixed solution, adding ethanol, heating and refluxing for 7 hours, and distilling under reduced pressure to obtain a catalyst F;
s23: placing 9-decene-1-alcohol and catalyst F in a three-neck flask at room temperature of 25 ℃ in a fume hood, and placing N2Adding methyl dichlorosilane under protection, reacting for 4 hours at normal temperature under magnetic stirring, and sampling after no bubbles are generated to obtain an intermediate A;
s24: adding the intermediate A into a three-neck flask, N2Adding propanol into a three-neck flask under protection, heating to 50 ℃ under magnetic stirring, reacting for 5h, cooling, neutralizing and alcoholyzing by triethylamine until no new precipitate is generated, and filtering to obtain an intermediate B;
s25: and adding methacryloyl chloride into the intermediate B, reacting for 4 hours at normal temperature under magnetic stirring, neutralizing with triethylamine, and filtering to obtain the cross-linking agent.
Comparative example 1:
comparative example 1 differs from example 1 in that no crosslinker is added.
Comparative example 2:
comparative example 2 the water glass sand hardening method disclosed in chinese patent CN201911062759.1 was used.
The binders of examples 1 to 3 and comparative examples 1 to 2 were hardened and examined, and CO was measured using a sand strength tester2The standard sample of the hardened phenolic resin sand core is used for testing the compressive strength, and the strength is divided into the instant strength sigma04 hour strength (middle strength) σ4And 24 hours intensity (final intensity) σ24The intensities of the three samples were averaged for each set of samples.
The results are shown in the following table:
sample (I) σ0/MPa σ4/MPa σ24/MPa
Example 1 1.71 2.55 5.23
Example 2 1.95 2.49 5.12
Example 3 1.93 2.67 5.28
Comparative example 1 1.01 1.97 3.89
Comparative example 2 1.21 1.54 4.34
As can be seen from the above table, σ for the examples0Sigma of comparative example 1 reaching 1.71-1.95MPa without addition of cross-linking agent0Is 101MPa, Sigma of comparative example 2 using the Water glass Sand hardening method disclosed in Chinese patent CN201911062759.101.21MPa, σ of example4Sigma of comparative example 1 reaching 2.49-2.67MPa without addition of cross-linking agent4Sigma of 1.97MPa, comparative example 2 using the water glass sand hardening method disclosed in Chinese patent CN201911062759.14Is 1.54MPa, sigma of example24Sigma of comparative example 1 reaching 5.12-5.28MPa without addition of cross-linking agent24Sigma of 3.89MPa, comparative example 2 using the water glass sand hardening method disclosed in Chinese patent CN201911062759.1244.34MPa, the data of comparative example 2 is better than that of comparative example 1, while the data of the example is obviously better than that of comparative example 2, which shows that the hardening accelerator can improve CO2The compression strength of the hardened phenolic resin sand core is superior to that of the prior art.
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 hardening accelerator is characterized by comprising the following components in parts by weight:
5-6 parts of calcium hydroxide, 2-3 parts of zinc oxide, 1.5-2 parts of magnesium oxide, 3-4 parts of Portland cement and 1-2 parts of a cross-linking agent;
the hardening accelerator is prepared by the following steps:
s1: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide, and grinding into powder;
s2: and uniformly mixing the ground materials, and adding a cross-linking agent to obtain the hardening accelerator.
2. A hardening accelerator according to claim 1, wherein the crosslinking agent is prepared by the steps of:
s21: filling acetic acid solution and chitosan into a three-neck flask, adding the purified carbon nano tube after opening the tube, stirring and refluxing, drying and grinding to obtain a catalyst E;
s22: adding the chloroplatinic acid isopropanol solution into absolute ethyl alcohol, mixing the catalyst E powder with the absolute ethyl alcohol, then adding ethyl alcohol, and carrying out reduced pressure distillation to obtain a catalyst F;
s23: placing 9-decene-1-alcohol and catalyst F in a three-neck flask under the indoor temperature of a fume hood, and placing N2Adding methyl dichlorosilane under protection, and reacting at normal temperature under magnetic stirring to obtain an intermediate A;
s24: adding the intermediate A into a three-neck flask, N2Adding propanol into a three-neck flask under protection, heating and reacting under magnetic stirring, cooling and filtering to obtain an intermediate B;
s25: and adding methacryloyl chloride into the intermediate B, reacting at normal temperature under magnetic stirring, and filtering to obtain the cross-linking agent.
3. The hardening accelerator according to claim 2, wherein the mass fraction of the acetic acid solution in step S21 is 1.5%, and the ratio of the acetic acid solution, chitosan and carbon nanotubes is 50 mL: 0.8 g: 8.0 g.
4. The hardening accelerator according to claim 2, wherein the concentration of the chloroplatinic acid isopropanol solution in step S22 is 0.0386mol/L, and the dosage ratio of the chloroplatinic acid isopropanol solution, the absolute ethanol, the catalyst E and the ethanol is 3.0 ml: 30.0 ml: 1.0 g: 10 mL.
5. The hardening accelerator according to claim 2, wherein the dosage ratio of the 9-decen-1-ol, the catalyst F and the methyl dichlorosilane in step S23 is 34 g: 4 g: 27.09 g.
6. A hardening accelerator according to claim 2, wherein the ratio of the intermediate a to propanol in step S24 is 57.2 g: 12.8 g.
7. A hardening accelerator according to claim 2, wherein the ratio of the amount of intermediate B to methacryloyl chloride in step S25 is 60.8 g: 20.9 g.
8. The method for preparing a hardening accelerator according to claim 1, wherein the method for preparing the hardening accelerator comprises the following steps:
s81: respectively weighing calcium hydroxide, portland cement, magnesium oxide and zinc oxide according to the weight parts, and grinding into powder for later use;
s82: uniformly mixing the ground calcium hydroxide, the portland cement, the magnesium oxide and the zinc oxide, and adding a cross-linking agent to obtain the hardening accelerator.
CN202111424068.9A 2021-11-26 2021-11-26 Hardening accelerator and preparation method thereof Withdrawn CN114029447A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115678491A (en) * 2022-11-08 2023-02-03 广州绿腾新材料有限公司 Organosilicon adhesive with good durability and low adhesive content of 107 and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115678491A (en) * 2022-11-08 2023-02-03 广州绿腾新材料有限公司 Organosilicon adhesive with good durability and low adhesive content of 107 and preparation method thereof

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