CN111943632B - Magnesium oxychloride cement and preparation method thereof - Google Patents
Magnesium oxychloride cement and preparation method thereof Download PDFInfo
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- CN111943632B CN111943632B CN202010722252.0A CN202010722252A CN111943632B CN 111943632 B CN111943632 B CN 111943632B CN 202010722252 A CN202010722252 A CN 202010722252A CN 111943632 B CN111943632 B CN 111943632B
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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
- C04B28/30—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 containing magnesium cements or similar cements
- C04B28/32—Magnesium oxychloride cements, e.g. Sorel cement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/08—Producing shaped prefabricated articles from the material by vibrating or jolting
- B28B1/087—Producing shaped prefabricated articles from the material by vibrating or jolting by means acting on the mould ; Fixation thereof to the mould
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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Abstract
The invention belongs to the technical field of inorganic cementing materials, and particularly relates to magnesium oxychloride cement and a preparation method thereof. The magnesium oxychloride cement contains a magnesium-ligand complex comprising Mg2+And coordinated to said Mg2+The cyclic ligand of (1) contains at least 2 donor atoms independently selected from phosphorus and oxygen, and is preferably prepared from the following raw materials, by mass, 300-440 parts of light-burned magnesium oxide, 195-210 parts of magnesium chloride hexahydrate, 120-130 parts of water, and 0.6-3.6 parts of phytic acid. The magnesium oxychloride cement provided by the invention has excellent water resistance and strength, and is wide in raw material source and easy for industrial application.
Description
Technical Field
The invention belongs to the technical field of inorganic cementing materials, and particularly relates to magnesium oxychloride cement and a preparation method thereof.
Background
The magnesium oxychloride cement is low-carbon cement, and compared with the silicate cement which is most commonly used in buildings, the magnesium oxychloride cement has the advantages of low alkalinity, high strength, air hardness, environmental protection and the like. In addition, the application of the magnesium oxychloride cement can increase the additional value of the magnesium chloride which is a waste in the potash fertilizer industry and reduce the harm to the environment. With the development of economy and science and technology, the green environment-friendly cement has developed trend. However, magnesium oxychloride cement has poor water resistance, which greatly limits its application.
Magnesium oxychloride cement has poor water resistance and 5-phase crystal (5Mg (OH) of its strength phase2·MgCl2·8H2O) is very easily hydrolyzed into magnesium hydroxide in water or wet environment. In previous studies, various acids and their salts have been commonly used to improve the water resistance of magnesium oxychloride cements. These modifiers reduce the minimum magnesium ion concentration required to form hydrated nuclei by complexing magnesium ions with anions during modification, and convert the rod-like 5 phase to a gelatinous state, thereby improving water resistance. But the internal stress generated after the acid radical ions are added promotes the generation of cracks, thereby causing damage to the mechanical property.
Disclosure of Invention
Aiming at the defects of the existing magnesium oxychloride cement waterproof modification technology, the invention provides a high-performance magnesium oxychloride cement and a preparation method thereof, wherein a cyclic ligand and Mg are constructed2+The complex improves water resistance and reduces crack generation by eliminating stress.
Specifically, the present invention provides the following technical solutions.
A magnesium oxychloride cement comprising a magnesium-ligand complex, said magnesium-ligand complex comprising Mg2+And coordinated to said Mg2+The cyclic ligand of (a), said cyclic ligand comprising at least 2 donor atoms independently selected from phosphorus and oxygen.
Preferably, in the above magnesium oxychloride cement, the cyclic ligand contains at least 4 donor atoms independently selected from phosphorus.
Preferably, in the above magnesium oxychloride cement, the cyclic ligand is phytic acid. The phytic acid is a biomass cyclic polyacid, is derived from plant seeds, and is a renewable material. Multiple phosphate anions on phytic acid can complex with magnesium ions during crystallization of magnesium oxychloride cement to form organic-inorganic complexes. Wherein, the rigid ring in the phytic acid has the capability of resisting internal stress, thereby avoiding the formation of cracks and improving the mechanical property.
Preferably, in the above magnesium oxychloride cement, the magnesium-ligand complex comprises phytic acid and 5mg (oh)2·MgCl2·8H2A complex of O. Acidic group on the phytic acid ring with 5Mg (OH)2·MgCl2·8H2O complexing effective to inhibit 5Mg (OH)2·MgCl2·8H2And O is hydrolyzed, so that the water resistance of the magnesium oxychloride cement is improved.
Preferably, the magnesium oxychloride cement is prepared from the following raw materials: light-burned magnesium oxide, magnesium chloride hexahydrate, phytic acid and water.
Preferably, the magnesium oxychloride cement is prepared from the following raw materials, by mass, 300-440 parts of light-burned magnesium oxide, 195-210 parts of magnesium chloride hexahydrate, 120-130 parts of water and 0.6-3.6 parts of phytic acid; more preferably, the magnesium oxide material is prepared from the following raw materials, by mass, 300-350 parts of light-burned magnesium oxide, 195-210 parts of magnesium chloride hexahydrate, 120-130 parts of water and 0.6-2.0 parts of phytic acid.
In the preparation of the traditional magnesium oxychloride cement, the light-burned magnesium oxide and the magnesium chloride hexahydrate are subjected to hydration reaction under the action of water to generate 5Mg (OH)2·MgCl2·8H2O、3Mg(OH)2·MgCl2·8H2O and Mg (OH)2. In the invention, the magnesium oxychloride cement is prepared by taking the light-burned magnesium oxide, the magnesium chloride hexahydrate, the phytic acid and the water which are reasonably proportioned as raw materials, and the main strength phase 5Mg (OH) in the magnesium oxychloride cement is further promoted by the unexpected discovery while the phytic acid and the magnesium ions are ensured to form a complex, the water resistance of the cement is improved and the generation of cracks is reduced2·MgCl2·8H2And O is generated, so that the mechanical property is improved.
Preferably, in the magnesium oxychloride cement, the activity index of the light-burned magnesium oxide is 60-70%, and the content of the magnesium oxide is 80-90%.
Preferably, in the above magnesium oxychloride cement, the water is tap water, softened water or deionized water.
The invention also provides a preparation method of the magnesium oxychloride cement, which comprises the following steps:
(1) mixing phytic acid and water to obtain a first solution;
(2) mixing magnesium chloride hexahydrate and the first solution obtained in the step (1) to obtain a second solution;
(3) mixing the light calcined magnesia with the second solution obtained in the step (2) to obtain slurry;
(4) injecting the slurry obtained in the step (3) into a mold for compaction, curing for a period of time, and then demolding;
(5) and (5) placing the demoulded sample in the air for natural curing for a period of time to obtain the product.
Preferably, in the preparation method, in the step (4), the curing temperature is 20-30 ℃ and the curing time is 18-30 hours.
Preferably, in the preparation method, in the step (5), the natural curing temperature is 20-30 ℃ and the natural curing time is 24-32 days.
The invention has the following beneficial effects:
the magnesium oxychloride cement provided by the invention follows the principle of environmental protection sustainable development, has the advantages of simple preparation method, wide raw material source, renewability, excellent water resistance and strength, reduction of crack generation, improvement of mechanical property and easiness in industrial application.
Drawings
FIG. 1 is a graph showing the compressive strength of magnesium oxychloride cements prepared in examples 1 to 4 and comparative examples 1 to 3 by natural curing for 3 days, 7 days, 28 days and 7 days after natural curing for 7 days by soaking in water.
FIG. 2 is a graph showing the strength retention coefficients of the magnesium oxychloride cements prepared in examples 1 to 4 and comparative example 1.
FIG. 3 is a diagram showing the phase composition and content analysis of magnesium oxychloride cement prepared in examples 1 to 4 and comparative example 1 after natural curing for 7 days.
FIG. 4 is an XRD pattern of the magnesium oxychloride cement prepared in examples 1 to 4 and comparative example 1 after 7 days of natural curing for 7 days after being soaked in water for 7 days.
FIG. 5 is a diagram showing the analysis of the phase components and contents of the magnesium oxychloride cement prepared in examples 1 to 4 and comparative example 1 after being naturally cured for 7 days after being soaked in water for 7 days.
FIG. 6 is a SEM image comparison of the surfaces of magnesium oxychloride cements prepared in example 4 and comparative examples 2-3 after natural curing for 28 days.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited thereto.
The experimental procedures used in the following examples are conventional unless otherwise specified. The experimental raw materials and the related equipments used in the following examples are commercially available unless otherwise specified.
The light-burned heavy magnesia used in the following examples was purchased from Guangzhou Danlin trade company, Inc. and had a magnesia content of 85% and an activity of 64%.
Example 1
(1) Dissolving 0.63 mass part of phytic acid in 126 mass parts of water, and uniformly stirring at 25 +/-2 ℃ to form a phytic acid aqueous solution;
(2) adding 205 parts by mass of magnesium chloride hexahydrate into the phytic acid aqueous solution prepared in the step (1), and uniformly stirring;
(3) adding 315 parts by mass of light-burned heavy magnesium oxide into the mixed solution obtained in the step (2), and stirring for 5 minutes to form uniform cement slurry;
(4) pouring into a mold, compacting, curing at 25 +/-2 ℃ for 24 hours, and then demolding;
(5) and curing for 28 days at 25 +/-2 ℃ after demolding to obtain the organic-inorganic hybrid modified high-performance magnesium oxychloride cement.
Example 2
(1) Dissolving 1.26 parts by mass of phytic acid in 126 parts by mass of water, and uniformly stirring at 25 +/-2 ℃ to form a phytic acid aqueous solution;
(2) adding 205 parts by mass of magnesium chloride hexahydrate into the phytic acid aqueous solution prepared in the step (1), and uniformly stirring;
(3) adding 315 parts by mass of light-burned heavy magnesium oxide into the mixed solution obtained in the step (2), and stirring for 5 minutes to form uniform cement slurry;
(4) pouring into a mold, compacting, curing at 25 +/-2 ℃ for 24 hours, and then demolding;
(5) and curing for 28 days at 25 +/-2 ℃ after demolding to obtain the organic-inorganic hybrid modified high-performance magnesium oxychloride cement.
Example 3
(1) Dissolving 1.9 parts by mass of phytic acid in 126 parts by mass of water, and uniformly stirring at room temperature to form a phytic acid aqueous solution;
(2) adding 205 parts by mass of magnesium chloride hexahydrate into the phytic acid aqueous solution prepared in the step (1), and uniformly stirring;
(3) adding 315 parts by mass of light-burned heavy magnesium oxide into the mixed solution obtained in the step (2), and stirring for 5 minutes to form uniform cement slurry;
(4) pouring into a mold, compacting, curing at 25 +/-2 ℃ for 24 hours, and then demolding;
(5) and curing for 28 days at 25 +/-2 ℃ after demolding to obtain the organic-inorganic hybrid modified high-performance magnesium oxychloride cement.
Example 4
(1) Dissolving 2.52 parts by mass of phytic acid in 126 parts by mass of water, and uniformly stirring at room temperature to form a phytic acid aqueous solution;
(2) adding 205 parts by mass of magnesium chloride hexahydrate into the phytic acid aqueous solution prepared in the step (1), and uniformly stirring;
(3) adding 315 parts by mass of light-burned heavy magnesium oxide into the mixed solution obtained in the step (2), and stirring for 5 minutes to form uniform cement slurry;
(4) pouring into a mold, compacting, curing at 25 +/-2 ℃ for 24 hours, and then demolding;
(5) and curing for 28 days at 25 +/-2 ℃ after demolding to obtain the organic-inorganic hybrid modified high-performance magnesium oxychloride cement.
Comparative example 1
(1) Dissolving 205 parts by mass of magnesium chloride hexahydrate in 126 parts by mass of water, and uniformly stirring at 25 +/-2 ℃ to form a magnesium chloride aqueous solution;
(2) adding 315 parts by mass of light-burned heavy magnesium oxide into a magnesium chloride aqueous solution, and stirring for 5 minutes to form uniform cement slurry;
(3) pouring into a mold, compacting, curing at 25 +/-2 ℃ for 24 hours, and then demolding;
(4) and curing for 28 days at 25 +/-2 ℃ after demolding to obtain the magnesium oxychloride cement.
Comparative example 2
Comparative example 2 differs from example 4 only in that: 6 parts by mass of tartaric acid is used instead of phytic acid.
Comparative example 3
Comparative example 3 differs from example 4 only in that: 6 parts by mass of sodium polyacrylate is used instead of phytic acid.
Test examples
1. Compressive strength
FIG. 1 is a graph showing the compressive strength of magnesium oxychloride cements prepared in examples 1 to 4 and comparative examples 1 to 3 by natural curing for 3 days, 7 days, 28 days and 7 days after natural curing for 7 days by soaking in water. The compressive strength test was carried out using a universal mechanical tester (WDW-50) at a loading rate of 5 mm/min. It can be seen that the compressive strength of the magnesium oxychloride cement prepared in examples 1-4 after natural curing for 7 days is higher than that of the cement prepared in comparative examples 1-3.
2. Coefficient of strength retention
FIG. 2 shows the strength retention coefficients of the magnesium oxychloride cements prepared in examples 1 to 4 and comparative examples 1 to 3, in which it can be seen that the water resistance of examples 1 to 4 is higher than that of comparative examples 1 to 2, and is improved by more than 95% compared with comparative example 1, indicating that a small amount of phytic acid added can achieve higher water resistance. The water resistance of comparative example 3 is slightly higher than that of examples 1 to 4, which is associated with the low compressive strength of comparative example 3 before foaming.
The intensity retention coefficient is calculated from the following formula:
4. XRD and phase content
FIG. 3 is a diagram showing the composition and content analysis of each phase of the magnesium oxychloride cement prepared after natural curing for 7 days in examples 1 to 4 and comparative example 1, and it can be seen that the 5-phase crystals (5Mg (OH)) of examples 1 to 3 are formed after adding a small amount of phytic acid2·MgCl2·8H2O) is higher than the comparative content, which shows that the content of 5-phase crystals in the prepared magnesium oxychloride cement can be improved by adding a small amount of phytic acid. The slightly lower 5-phase crystal content of example 4 than in comparative example 1 is associated with retarding the reaction of part of the magnesium oxide with carbon dioxide in the air to magnesium carbonate during cement setting.
FIG. 4 is an XRD pattern of the magnesium oxychloride cement prepared in examples 1 to 4 and comparative example 1 after 7 days of natural curing for 7 days after soaking in water, from which it can be seen that Mg (OH) in comparative example 12The intensity of the characteristic peak is high, the characteristic peak of the 5-phase crystal is weaker, while examples 1 to 4 mainly show the characteristic peak of the 5-phase crystal, Mg (OH)2The characteristic peak is obviously weakened, which shows that the phytic acid is added to form a phytic acid-magnesium complex which can inhibit the 5-phase crystal from decomposing in water.
FIG. 5 is a graph showing the composition and content analysis of the phases after 7 days of soaking of the magnesium oxychloride cements prepared in examples 1 to 4 and comparative example 1 after 7 days of natural curing, and it can be seen that the five-phase structure portion in comparative example 1 is converted into magnesium hydroxide after 7 days of soaking, whereas the five-phase content of all examples is higher, the content of magnesium hydroxide is low, and unreacted magnesium oxide is still contained after soaking, indicating that the prepared magnesium oxychloride cement has better water resistance.
5. SEM characterization
FIG. 6 is a SEM image comparing the surfaces of the magnesium oxychloride cements prepared in example 4 and comparative examples 2 to 3 after natural curing for 28 days, and it can be seen from FIG. 6 that the surface cracks of the phytic acid modified magnesium oxychloride cement are significantly reduced compared with those of other acid modified magnesium oxychloride cements.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. A magnesium oxychloride cement comprising a magnesium-ligand complex, wherein the magnesium-ligand complex comprises phytic acid and 5Mg (OH)2·MgCl2·8H2A complex of O.
2. The magnesium oxychloride cement of claim 1, wherein the magnesium oxychloride cement is prepared from the following raw materials: light-burned magnesium oxide, magnesium chloride hexahydrate, phytic acid and water.
3. The magnesium oxychloride cement of claim 2, which is prepared from the following raw materials, by mass, 300-440 parts of light calcined magnesia, 195-210 parts of magnesium chloride hexahydrate, 120-130 parts of water, and 0.6-3.6 parts of phytic acid.
4. The magnesium oxychloride cement of claim 3, which is prepared from the following raw materials, by mass, 300-350 parts of light calcined magnesia, 195-210 parts of magnesium chloride hexahydrate, 120-130 parts of water, and 0.6-2.0 parts of phytic acid.
5. The magnesium oxychloride cement of any one of claims 2 to 4, wherein the light-burned magnesium oxide has an activity index of 60 to 70% and a magnesium oxide content of 80 to 90%.
6. A process for the preparation of a magnesium oxychloride cement as claimed in any one of claims 1 to 5, which comprises the steps of:
(1) mixing phytic acid and water to obtain a first solution;
(2) mixing magnesium chloride hexahydrate and the first solution obtained in the step (1) to obtain a second solution;
(3) mixing the light calcined magnesia with the second solution obtained in the step (2) to obtain slurry;
(4) injecting the slurry obtained in the step (3) into a mold for compaction, curing for a period of time, and then demolding;
(5) and (5) placing the demoulded sample in the air for natural curing for a period of time to obtain the product.
7. The preparation method according to claim 6, wherein in the step (4), the curing temperature is 20-30 ℃ and the curing time is 18-30 h.
8. The method according to claim 6 or 7, wherein the natural curing in the step (5) is carried out at a temperature of 20 to 30 ℃ for 24 to 32 days.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000818A (en) * | 2015-05-29 | 2015-10-28 | 盐城工学院 | Modifying agent for magnesium oxychloride cement, preparing method thereof and application thereof |
| CN107235701A (en) * | 2017-06-28 | 2017-10-10 | 常州凯恒纺织品有限公司 | A kind of water-resistant type magnesia oxychloride cement material |
| CN110272258A (en) * | 2019-06-15 | 2019-09-24 | 北京林业大学 | A kind of high strong water resistant magnesia oxychloride cement and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000818A (en) * | 2015-05-29 | 2015-10-28 | 盐城工学院 | Modifying agent for magnesium oxychloride cement, preparing method thereof and application thereof |
| CN107235701A (en) * | 2017-06-28 | 2017-10-10 | 常州凯恒纺织品有限公司 | A kind of water-resistant type magnesia oxychloride cement material |
| CN110272258A (en) * | 2019-06-15 | 2019-09-24 | 北京林业大学 | A kind of high strong water resistant magnesia oxychloride cement and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 磷酸根离子对氯氧镁水泥水化物稳定性的影响;邓德华;《建筑材料学报》;20020331;第5卷(第1期);第9-12页 * |
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