CN107935444B - Formula and preparation method of retarder for magnesite cementing material - Google Patents
Formula and preparation method of retarder for magnesite cementing material Download PDFInfo
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- CN107935444B CN107935444B CN201711129326.4A CN201711129326A CN107935444B CN 107935444 B CN107935444 B CN 107935444B CN 201711129326 A CN201711129326 A CN 201711129326A CN 107935444 B CN107935444 B CN 107935444B
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- polysuccinimide
- retarder
- magnesite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention belongs to the technical field of retarders, and provides a retarder for a magnesite cementing material, which comprises the following components in parts by weight: 25-35 parts of N, N-dimethylformamide, 3-7 parts of polysuccinimide, 2-6 parts of glacial acetic acid, 0.5-1.2 parts of sodium citrate, 0.5-1.2 parts of humic acid, 0.5-1.2 parts of ferric chloride, 7-12 parts of 4-zinc hydroxybenzenesulfonate, 0.1-0.5 part of sodium carboxymethylcellulose and 45-50 parts of water, and the technical problem that the conventional coagulant has a poor retarding effect or the strength of a magnesite product is insufficient after being added as an external aid of a cementing material is solved.
Description
Technical Field
The invention belongs to the technical field of retarders, and relates to a formula and a preparation method of a retarder for a magnesite cementing material.
Background
In the production process of the magnesite cementing material, the magnesite slurry has the characteristics of early strength and quick hardening, particularly, in the environment with the air temperature of more than 30 ℃, the magnesite cementing material slurry is hardened too quickly, the problems that the magnesite cementing material slurry is hardened too quickly can exist, the first step is not beneficial to forming operation, the second step is deformation and cracking of the product caused by uneven heat dispersion due to the too quick hardening, but after the existing coagulant is added as an external auxiliary agent of the cementing material, the retarding effect is poor, or the strength of the magnesite product is not enough are solved.
Disclosure of Invention
The invention provides a formula and a preparation method of a retarder for a magnesite cementing material, and solves the technical problems.
The technical scheme of the invention is realized as follows:
the retarder for the magnesite cementing material comprises the following components in parts by weight:
25-35 parts of N, N-Dimethylformamide (DMF), 3-7 parts of polysuccinimide, 2-6 parts of glacial acetic acid, 0.5-1.2 parts of sodium citrate, 0.5-1.2 parts of humic acid, 0.5-1.2 parts of ferric chloride, 7-12 parts of 4-hydroxybenzene sulfonic acid zinc salt, 0.1-0.5 part of sodium carboxymethylcellulose and 45-50 parts of water.
Further, 30 parts of N, N-dimethylformamide, 5 parts of polysuccinimide, 4 parts of glacial acetic acid, 1 part of sodium citrate, 1 part of humic acid, 1 part of ferric chloride, 10 parts of zinc 4-hydroxybenzenesulfonate, 0.2 part of sodium carboxymethylcellulose and 48.8 parts of water.
A preparation method of a retarder for a magnesite cementing material comprises the following steps: :
(1) according to the retarder, weighing DMF, polysuccinimide, glacial acetic acid, sodium citrate, humic acid, ferric chloride, zinc 4-hydroxybenzenesulfonate, sodium hydroxymethyl cellulose and water;
(2) mixing the polysuccinimide in the step (1) with DMF (dimethyl formamide) and stirring under a heating condition until the polysuccinimide is completely dissolved, slowly adding the glacial acetic acid in the step (1) into the mixture, and mixing and stirring to obtain a polysuccinimide solution;
(3) mixing the sodium citrate, humic acid, ferric chloride, 4-zinc hydroxybenzenesulfonate and water weighed in the step (1) to obtain a mixture water solution, heating the mixed water solution, slowly adding the sodium hydroxymethyl cellulose weighed in the step (1) into the mixture water solution under the stirring condition, and stirring to obtain uniform viscous liquid;
(4) and (3) mixing the polysuccinimide solution obtained in the step (2) and the viscous liquid obtained in the step (3) at normal temperature, and uniformly stirring to obtain the magnesite gel material retarder.
Further, the temperature condition of the polysuccinimide and DMF mixing and stirring in the step (2) was 90 ℃, and glacial acetic acid was slowly added while maintaining the temperature, followed by mixing and stirring for 60 minutes.
Further, the mixed aqueous solution in the step (3) is heated to 50 ℃, and is stirred for 20 minutes after the sodium carboxymethyl cellulose is added.
Compared with the prior art, the invention has the working principle and the beneficial effects that:
1. in the invention, researches show that in the production process of the magnesite cementing material, magnesium hydroxide is generated when magnesium oxide is prepared by water, and a large amount of heat is released, so that the magnesite slurry is hardened too fast due to the temperature rise, and the Mg in the magnesite slurry can be effectively combined after the ring-opening product of polysuccinimide and the zinc 4-hydroxybenzenesulfonate are compounded2+The insoluble matter is formed to cover the surface of the magnesium oxide which is not dissolved so as to prevent the magnesium oxide from contacting with water molecules, the reaction speed of the magnesium oxide is reduced, the heat emission in the reaction process is slowed down, the rapid hardening of the magnesite slurry caused by the instantaneous high temperature generated after the heat is concentrated and rapidly emitted is further avoided, the slow setting effect is effectively realized, and after the polysuccinimide and the zinc 4-hydroxybenzenesulfonate are compounded for use, the toughness and the strength of the magnesite gel material are increased by the mutually matched structure of macromolecular chains, so that the magnesite gel material has the excellent slow setting effect and strength, and the technical problem that the slow setting effect and the strength of a magnesite product cannot be combined after the conventional coagulant is added as an external aid of the gel material is solved.
2. Hair brushIn the process of operation, the polysuccinimide is dissolved by taking DMF as a solvent, the DMF has the advantages of high boiling point, good solubility, low price and the like, the polysuccinimide can be better dissolved under the heating condition, and the acetic acid is dripped to promote the polysuccinimide to be hydrolyzed and subjected to ring opening to obtain exposed carboxyl, so that the combination of Mg in magnesite slurry is facilitated2+The reinforcing slow setting effect, 4-hydroxybenzene sulfonic acid zinc solubility is better, direct water is used as the solvent, add humic acid, ferric chloride, sodium citrate is as the auxiliary agent, humic acid, ferric chloride, the pH valve that can effectively adjust the solution is used in the sodium citrate complex formulation, pH to whole solution has the cushioning effect, there is certain inhibitory action to the polyhalogen scumming of magnesite binding material later stage in addition, slowly add the viscidity that carboxymethylcellulose sodium can the limited increase aqueous solution at last, the filling in the later stage of being convenient for, transportation and use, more convenient and even add the retarder to the mud in, in addition, make the polysuccinimide solution of oil phase and viscous liquid alright with the intensive mixing under normal atmospheric temperature.
Detailed Description
The following will clearly and completely describe the technical solutions in 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 embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a formula of a retarder for a magnesite cementing material and a preparation method thereof, wherein the formula comprises the following steps:
the first embodiment is as follows:
(1) weighing 25 parts of DMF, 3 parts of polysuccinimide, 2 parts of glacial acetic acid, 0.5 part of sodium citrate, 0.5 part of humic acid, 0.5 part of ferric chloride, 7 parts of zinc 4-hydroxybenzene sulfonate, 0.1 part of sodium carboxymethylcellulose and 45 parts of water for later use;
(2) mixing and stirring the polysuccinimide in the step (1) and DMF at the temperature of 90 ℃ until the polysuccinimide is completely dissolved, slowly adding the glacial acetic acid in the step (1) into the polysuccinimide, and mixing and stirring for 60 minutes to obtain a polysuccinimide solution;
(3) mixing the sodium citrate, humic acid, ferric chloride, zinc 4-hydroxybenzenesulfonate and water weighed in the step (1) to obtain a mixture aqueous solution, heating the mixture aqueous solution to 50 ℃, slowly adding the sodium carboxymethylcellulose weighed in the step (1) into the mixture aqueous solution under the condition of stirring, and stirring for 20 minutes until the solution becomes uniform viscous liquid;
(4) and (3) mixing the polysuccinimide solution obtained in the step (2) and the viscous liquid obtained in the step (3) at normal temperature, and uniformly stirring to obtain the magnesite gel material retarder.
Example two:
35 parts of DMF, 7 parts of polysuccinimide, 6 parts of glacial acetic acid, 1.2 parts of sodium citrate, 1.2 parts of humic acid, 1.2 parts of ferric chloride, 12 parts of zinc 4-hydroxybenzenesulfonate, 0.5 part of sodium hydroxymethyl cellulose and 50 parts of water are weighed for later use, and other steps are the same as the first embodiment.
Example three:
30 parts of DMF, 5 parts of polysuccinimide, 4 parts of glacial acetic acid, 1 part of sodium citrate, 1 part of humic acid, 1 part of ferric chloride, 10 parts of zinc 4-hydroxybenzenesulfonate, 0.2 part of sodium hydroxymethyl cellulose and 48.8 parts of water are weighed for later use, and other steps are the same as the first embodiment.
The experimental data of the retardation effect and strength of the first, second and third examples are shown in table 1:
TABLE 1 Experimental data for example one, example two and example three
As can be seen from the data in Table 1, the retarders of the first, second and third examples all have better retarding effects when applied to the beauty gel material and also have excellent strength properties, wherein the retarding effect and the strength properties of the third example are the best.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The retarder for the magnesite cementing material is characterized by comprising the following components in parts by weight:
25-35 parts of N, N-dimethylformamide, 3-7 parts of polysuccinimide, 2-6 parts of glacial acetic acid, 0.5-1.2 parts of sodium citrate, 0.5-1.2 parts of humic acid, 0.5-1.2 parts of ferric chloride, 7-12 parts of 4-zinc hydroxybenzenesulfonate, 0.1-0.5 part of sodium carboxymethylcellulose and 45-50 parts of water.
2. The retarder for the magnesite cement material as claimed in claim 1, which is characterized by comprising the following components in parts by weight:
30 parts of N, N-dimethylformamide, 5 parts of polysuccinimide, 4 parts of glacial acetic acid, 1 part of sodium citrate, 1 part of humic acid, 1 part of ferric chloride, 10 parts of zinc 4-hydroxybenzenesulfonate, 0.2 part of sodium carboxymethylcellulose and 48.8 parts of water.
3. The preparation method of the retarder for the magnesite cementing material is characterized by comprising the following steps of:
(1) the retarder according to any one of claims 1 to 2, wherein DMF, polysuccinimide, glacial acetic acid, sodium citrate, humic acid, ferric chloride, zinc 4-hydroxybenzenesulfonate, sodium carboxymethylcellulose and water are weighed;
(2) mixing the polysuccinimide in the step (1) with DMF (dimethyl formamide) and stirring under a heating condition until the polysuccinimide is completely dissolved, slowly adding the glacial acetic acid in the step (1) into the mixture, and mixing and stirring to obtain a polysuccinimide solution;
(3) mixing the sodium citrate, humic acid, ferric chloride, 4-zinc hydroxybenzenesulfonate and water weighed in the step (1) to obtain a mixture water solution, heating the mixed water solution, slowly adding the sodium hydroxymethyl cellulose weighed in the step (1) into the mixture water solution under the stirring condition, and stirring to obtain uniform viscous liquid;
(4) and (3) mixing the polysuccinimide solution obtained in the step (2) and the viscous liquid obtained in the step (3) at normal temperature, and uniformly stirring to obtain the magnesite gel material retarder.
4. The preparation method of the retarder for magnesite cement material as claimed in claim 3, wherein the temperature condition of the polysuccinimide and DMF mixing and stirring in the step (2) is 90 ℃, and glacial acetic acid is slowly added under the condition of keeping the temperature unchanged, and then the mixture is mixed and stirred for 60 minutes.
5. The preparation method of the retarder for magnesite cement as claimed in claim 3, wherein the temperature of the mixed aqueous solution in step (3) is raised to 50 ℃, and the mixture is stirred for 20 minutes after the sodium carboxymethyl cellulose is added.
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CN1118439C (en) * | 2001-09-19 | 2003-08-20 | 山东省建筑科学研究院 | Prepn of retardant for magnesite binding material |
US7091160B2 (en) * | 2004-06-24 | 2006-08-15 | Halliburton Energy Services, Inc. | Methods and compositions for reducing subterranean formation permeabilities |
EP2852487B8 (en) * | 2012-05-22 | 2021-01-20 | Henkel IP & Holding GmbH | Process for binding substrates with a liquid optically clear photo-curable adhesive |
CN102875046B (en) * | 2012-10-24 | 2014-03-19 | 山东建科特种建筑工程技术中心 | Efficient powder type retarder for magnesite cement |
CN102923987A (en) * | 2012-11-23 | 2013-02-13 | 杨益 | Retardant preparation method |
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Address after: 050000 Nanbei Qinghe River, Nanhuan Road, Zanhuang Town, Zanhuang County, Shijiazhuang City, Hebei Province Patentee after: Shijiazhuang chaxiaochuan Technology Co.,Ltd. Address before: 050000 Nanbei Qinghe River, Nanhuan Road, Zanhuang Town, Zanhuang County, Shijiazhuang City, Hebei Province Patentee before: SHIJIAZHUANG JIANHENG NEW MATERIAL TECHNOLOGY CO.,LTD. |