CN108178596B - Method for preparing gypsum-based self-leveling material from glauberite tailings - Google Patents

Method for preparing gypsum-based self-leveling material from glauberite tailings Download PDF

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CN108178596B
CN108178596B CN201711345274.4A CN201711345274A CN108178596B CN 108178596 B CN108178596 B CN 108178596B CN 201711345274 A CN201711345274 A CN 201711345274A CN 108178596 B CN108178596 B CN 108178596B
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parts
gypsum
tailings
based self
leveling material
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CN108178596A (en
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谭琦
赵毅
刘玉林
李一波
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Zhengzhou Institute of Multipurpose Utilization of Mineral Resources CAGS
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Zhengzhou Institute of Multipurpose Utilization of Mineral Resources CAGS
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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
    • C04B28/14—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 calcium sulfate cements
    • C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention provides a method for preparing a gypsum-based self-leveling material from glauber salt tailings, which is used for producing the gypsum-based self-leveling material by a pressurized aqueous solution method, and has the advantages of less additives, wide raw material source and low cost. The invention is carried out according to the following method: putting 450-600 parts of glauber salt tailings into an autoclave, uniformly mixing 0.75-1.5 parts of a crystal modifier, 0.64-1.5 parts of a surfactant and water, pouring into the autoclave, adjusting the pH value to 6-8 by using a pH regulator, tightly covering the autoclave, reacting at 115-130 ℃ for 1-2 h, taking out the solution, filtering in a vacuum filter by using boiling water and absolute ethyl alcohol to remove the reagent, and drying in a drying box. The gypsum-based self-leveling material prepared from the glauber's salt tailings obtained by the invention has the performance exceeding the standard requirement of the national building material industry. And the mirabilite gypsum with low price is used, so the method is easy to popularize and apply.

Description

Method for preparing gypsum-based self-leveling material from glauberite tailings
Technical Field
The invention relates to the technical field of comprehensive utilization of tailings, and particularly relates to a method for preparing a gypsum-based self-leveling material from glauber's salt tailings.
Background
The industrial byproduct gypsum is a byproduct or waste residue which is generated in industrial production due to chemical reaction and takes calcium sulfate as a main component, and mainly comprises desulfurized gypsum, phosphogypsum, titanium gypsum, mirabilite gypsum, salt gypsum, citric acid gypsum and the like. The industrial byproduct gypsum in China has huge discharge amount and low comprehensive utilization rate. In 2013, the total emission amount of the industrial byproduct gypsum is about 1.8 hundred million tons, the comprehensive utilization amount of the industrial byproduct gypsum is about 8660 million tons, and the comprehensive utilization rate is about 48 percent. The stacking of the industrial byproduct gypsum not only occupies a large amount of land, but also causes ecological damage and environmental pollution, and is the industrial solid waste which needs to be solved urgently.
The mirabilite gypsum is obtained by leaching Na from glauber salt2SO4Dihydrate gypsum is produced in the course of the solution. Most of the industrial by-product gypsum is stockpiled, and a small part of the industrial by-product gypsum is used as a cement retarder, so that the added value is low. The gypsum-based self-leveling mortar is a dry powder mortar specially used for ground leveling, which is prepared by uniformly mixing gypsum materials, special aggregates and various building chemical additives, has the advantages of accurate size, extremely high levelness, no hollowing, no cracking, convenient operation, high efficiency, heat preservation, heat insulation, sound absorption, flame retardance and the like, and is particularly superior to the performance of cement mortar in the aspect of ground heating leveling. Because the production cost is higher than that of the cement-based self-leveling mortar, the popularization and the application are blocked, and the development is slow.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing a gypsum-based self-leveling material by glauber's salt tailings, the gypsum-based self-leveling material is produced by the glauber's salt tailings through a pressurized aqueous solution method, and the method has the advantages of few additives, wide raw material source and low cost.
The technical scheme of the invention is realized in the following mode: a method for preparing a gypsum-based self-leveling material from glauber's salt tailings is carried out according to the following steps: putting 450-600 parts of glauber salt tailings into an autoclave, uniformly mixing 0.75-1.5 parts of a crystal modifier, 0.64-1.5 parts of a surfactant and water, pouring into the autoclave, adjusting the pH value to 6-8 by using a pH regulator, tightly covering the autoclave, reacting at 115-130 ℃ for 1-2 h, taking out the solution, filtering in a vacuum filter by using boiling water and absolute ethyl alcohol to remove the reagent, and drying in a drying box.
Preferably, the crystal transforming agent is citrate and aluminum salt.
Preferably, the citrate is sodium citrate or potassium citrate.
Preferably, the aluminum salt is aluminum sulfate or aluminum chloride.
Preferably, the surfactant is sodium dodecyl benzene sulfonate.
Preferably, the drying is carried out in an electrothermal blowing drying oven at 120 ℃.
Preferably, the particle size of the glauberite tailings is below 50 meshes.
The gypsum-based self-leveling material prepared from the glauber's salt tailings obtained by the invention has the performance exceeding the standard requirement of the national building material industry. And the mirabilite gypsum with low price is used, so the method is easy to popularize and apply.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, 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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
The invention discloses a method for preparing a gypsum-based self-leveling material from glauber salt tailings, which is carried out according to the following method (the parts of the gypsum-based self-leveling material refer to parts by weight): putting 450-600 parts of glauber salt tailings into an autoclave, uniformly mixing 0.75-1.5 parts of a crystal modifier, 0.64-1.5 parts of a surfactant and water, pouring into the autoclave, adjusting the pH value to 6-8 with a pH regulator, tightly driving the autoclave, reacting at 115-130 ℃ for 1-2 h, taking out the solution, filtering with boiling water and absolute ethyl alcohol in a vacuum filter, dehydrating to remove the reagent, and drying in a drying oven. The fractions described herein are parts by weight.
The glauberite tailing mainly comprises Ca2SO4·2H250-70 parts of O, 15-20 parts of plaster of paris, 10-12 parts of quartz, 8-10 parts of calcite, 2-5 parts of feldspar and 2-5 parts of mica.
The crystal transformation agent is citrate and aluminum salt. Wherein the citrate is sodium citrate or potassium citrate, and the aluminum salt is aluminum sulfate or aluminum chloride.
The surfactant is sodium dodecyl benzene sulfonate.
The drying is carried out in an electrothermal blowing drying oven at 120 ℃.
The granularity of the glauberite tailings is below 50 meshes.
The following describes embodiments of the present invention with reference to specific examples.
Example 1
Weighing 1.5g of sodium citrate, aluminum sulfate and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1.5:2, uniformly stirring in 450mL of water, putting the mixture and 450g of glauber salt tailings below 50 meshes into an autoclave, dripping 1.5mL of dilute sulfuric acid, reacting for 1.5h at 120 ℃, taking out the solution in the autoclave, quickly filtering the solution in the autoclave in a vacuum filter by using 1L of boiling water and 500mL of absolute ethyl alcohol, and drying in an electrothermal blowing drying box at 120 ℃ to obtain the gypsum-based self-leveling material.
The self-leveling material has the water requirement of 25 percent, the initial setting time of 70min, the absolute dry compressive strength of 30MPa, the absolute dry flexural strength of 10MPa and the shrinkage rate of 0.02 percent, and the performances of the self-leveling material far exceed the requirements in the standard JC/T1023-2007 in the building material industry standard JC/T1023-2007 (the initial setting time is more than or equal to 1h, the absolute dry compressive strength is more than or equal to 20MPa, the absolute dry flexural strength is more than or equal to 7.5MPa and the shrinkage rate is less than or equal to 0.05 percent in JC/T1023-2007 Gypsum-based self-leveling mortar.
In this embodiment, the total amount of sodium citrate, aluminum sulfate, and sodium dodecylbenzenesulfonate may be 1.5g, 2g, or 2.5 g.
Example 2
Weighing 2.0g of potassium citrate, aluminum sulfate and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1:2, uniformly stirring in 500mL of water, putting the mixture and 450g of glauber's salt tailings below 50 meshes into an autoclave, dripping 1.5mL of dilute sulfuric acid, reacting for 1.5h at 120 ℃, taking out the solution in the autoclave, quickly filtering the solution in the autoclave in a vacuum filter by using 1L of boiling water and 500mL of absolute ethyl alcohol, and drying the solution in an electrothermal blowing drying box at 120 ℃ to obtain the gypsum-based self-leveling material. The self-leveling material has the water requirement of 23 percent, the initial setting time of 75min, the absolute dry compressive strength of 29MPa, the absolute dry flexural strength of 9.5MPa and the shrinkage rate of 0.02 percent, and the performances of the self-leveling material far exceed the requirements in the national building material industry standard JC/T1023-2007.
In this embodiment, the total amount of potassium citrate, aluminum sulfate, and sodium dodecylbenzenesulfonate may be 2g, 2.25g, or 2.1 g.
Example 3
Weighing 1.5g of sodium citrate, aluminum chloride and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1.5:2, uniformly stirring in 450mL of water, putting the mixture and 450g of glauberite tailings below 50 meshes into an autoclave, dripping 1.5mL of dilute sulfuric acid, reacting for 2 hours at the temperature of 115 ℃, taking out the solution in the autoclave, quickly filtering the solution in the autoclave in a vacuum filter by using 1L of boiling water and 500mL of absolute ethyl alcohol, and drying the solution in an electrothermal blowing drying box at the temperature of 120 ℃ to obtain the gypsum-based self-leveling material. The self-leveling material has the water requirement of 27 percent, the initial setting time of 80min, the absolute dry compressive strength of 32MPa, the absolute dry flexural strength of 11MPa and the shrinkage rate of 0.02 percent, and the performances of the self-leveling material far exceed the requirements of the national building material industry standard JC/T1023-2007-one-material.
In this example, the amount of sodium citrate, aluminum chloride, sodium dodecylbenzenesulfonate may be 1.5g, 1.75g, 3g, or the like.
Example 4
Weighing 2.5g of potassium citrate, aluminum sulfate and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1.5:2.5, uniformly stirring in 600mL of water, putting the mixture and 600g of glauberite tailings below 50 meshes into an autoclave, dripping 2mL of dilute sulfuric acid, reacting for 2 hours at 120 ℃, taking out the solution in the autoclave, quickly filtering the solution in the autoclave in a vacuum filter by using 1.5L of boiling water and 500mL of absolute ethyl alcohol, and drying in an electrothermal blowing drying box at 120 ℃ to obtain the gypsum-based self-leveling material. The self-leveling material has the water requirement of 26 percent, the initial setting time of 80min, the absolute compressive strength of 35MPa, the absolute flexural strength of 12MPa and the shrinkage rate of 0.01 percent, and the performances of the self-leveling material far exceed the requirements of the national building material industry standard JC/T1023-2007-one-material-adding 2007.
In this embodiment, the amount of potassium citrate, aluminum sulfate, and sodium dodecylbenzenesulfonate may be 2.5g, 3g, or 1.8 g.
Example 5
Weighing 1.5g of potassium citrate, aluminum chloride and sodium dodecyl benzene sulfonate according to the mass ratio of 1:1.5:2, uniformly stirring in 450mL of water, putting the mixture and 450g of glauberite tailings below 50 meshes into an autoclave, dripping 1.5mL of dilute sulfuric acid, reacting for 1h at 130 ℃, taking out the solution in the autoclave, quickly filtering the solution in the autoclave in a vacuum filter by using 1L of boiling water and 500mL of absolute ethyl alcohol, and drying in an electrothermal blowing drying box at 120 ℃ to obtain the gypsum-based self-leveling material. The self-leveling material has the water requirement of 25 percent, the initial setting time of 73min, the absolute compressive strength of 29MPa, the absolute flexural strength of 9.7MPa and the shrinkage rate of 0.02 percent, and the performances of the self-leveling material far exceed the requirements in the national building material industry standard JC/T1023-2007.
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 (6)

1. A method for preparing a gypsum-based self-leveling material from glauber's salt tailings is characterized by comprising the following steps of: putting 450-600 parts of glauber salt tailings into an autoclave, uniformly mixing 0.75-1.5 parts of a crystal modifier, 0.64-1.5 parts of a surfactant and water, pouring into the autoclave, adjusting the pH value to 6-8 by using a pH regulator, tightly covering the autoclave, reacting at 115-130 ℃ for 1-2 hours, taking out the solution, filtering in a vacuum filter by using boiling water and absolute ethyl alcohol to remove a reagent, and drying in a drying box; the parts are parts by weight;
wherein the main component of the glauberite tailings is Ca2SO4•2H250-70 parts of O, 15-20 parts of plaster of paris, 10-12 parts of quartz, 8-10 parts of calcite, 2-5 parts of feldspar and 2-5 parts of mica;
the surfactant is sodium dodecyl benzene sulfonate.
2. The method for preparing the gypsum-based self-leveling material from the glauberite tailings according to claim 1, wherein the method comprises the following steps: the crystal transformation agent is citrate and aluminum salt.
3. The method for preparing the gypsum-based self-leveling material from the glauberite tailings according to claim 2, wherein the method comprises the following steps: the citrate is sodium citrate or potassium citrate.
4. The method for preparing the gypsum-based self-leveling material from the glauberite tailings according to claim 2, wherein the method comprises the following steps: the aluminum salt is aluminum sulfate or aluminum chloride.
5. The method for preparing the gypsum-based self-leveling material from the glauberite tailings according to claim 1, wherein the method comprises the following steps: the drying is carried out in an electrothermal blowing drying oven at 120 ℃.
6. The method for preparing the gypsum-based self-leveling material from the glauberite tailings according to claim 1, wherein the method comprises the following steps: the granularity of the glauberite tailings is below 50 meshes.
CN201711345274.4A 2017-12-15 2017-12-15 Method for preparing gypsum-based self-leveling material from glauberite tailings Active CN108178596B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173621B (en) * 2011-01-31 2013-05-08 上海市建筑科学研究院(集团)有限公司 Short column-shaped high-strength desulfurized alpha-gypsum
CN105174760B (en) * 2015-09-18 2017-03-29 金正大生态工程集团股份有限公司 A kind of method that dihydrate gypsum prepares αsemiwatergypsum

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173621B (en) * 2011-01-31 2013-05-08 上海市建筑科学研究院(集团)有限公司 Short column-shaped high-strength desulfurized alpha-gypsum
CN105174760B (en) * 2015-09-18 2017-03-29 金正大生态工程集团股份有限公司 A kind of method that dihydrate gypsum prepares αsemiwatergypsum

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