CN108002794B - Method for low-temperature curing of waste gypsum into high-strength building material - Google Patents
Method for low-temperature curing of waste gypsum into high-strength building material Download PDFInfo
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- CN108002794B CN108002794B CN201711292491.1A CN201711292491A CN108002794B CN 108002794 B CN108002794 B CN 108002794B CN 201711292491 A CN201711292491 A CN 201711292491A CN 108002794 B CN108002794 B CN 108002794B
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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
- C04B28/142—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 containing synthetic or waste calcium sulfate cements
- C04B28/143—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 containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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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
- C04B28/142—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 containing synthetic or waste calcium sulfate cements
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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
- C04B28/142—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 containing synthetic or waste calcium sulfate cements
- C04B28/144—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 containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being a flue gas desulfurization product
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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
- C04B40/02—Selection of the hardening environment
- C04B40/024—Steam hardening, e.g. in an autoclave
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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
Abstract
The invention relates to a method for solidifying waste gypsum into a novel high-strength building material at low temperature, belonging to the technical field of recycling of gypsum waste generated in an industrial production process. Firstly, measuring waste gypsum according to mass percent: building sandstone: cement: fly ash: 40-75% of water: 10-20%: 5-25%: 5-30%: 5-25 percent, the sum of the contents of all the components is equal to 100 percent, the mixture is obtained by uniform grinding and stirring, a green body is obtained by pressing and forming under the pressure of 10-40 Mpa, the green body is placed in a hydrothermal kettle after being demoulded, and the curing treatment is carried out for 8-24 hours at the temperature of 120-220 ℃, thus obtaining the high-strength building material. The invention effectively solves the problems of dilemma of recycling the waste gypsum, easy secondary pollution to the environment and the like, improves the utilization rate of the waste gypsum, simultaneously the prepared high-strength building material has flexural strength and compressive strength superior to the use standard of common building materials (such as wall and floor tiles, pavement bricks, footpath bricks, river embankment protection materials and the like), has simple production process, low energy consumption in the production process, short period and lower product cost, and is suitable for large-scale production.
Description
Technical Field
The invention relates to a method for solidifying waste gypsum into a novel high-strength building material at low temperature. Belongs to the technical field of gypsum waste recycling generated in the industrial production process.
Background
Gypsum is a common co-product in industrial processes, and in the phosphoric acid industry for example, producing one ton of phosphoric acid produces 5 tons of phosphogypsum; with the gradual development of the industry in China, the discharge amount of gypsum is increased day by day, the utilization rate of the gypsum is extremely low, a large amount of gypsum generated by a chemical plant is accumulated like a mountain, occupies a fertile farmland, causes serious pollution to the environment, and also influences the life quality of residents around a stacking point. For example, Anhui Xuanchiel specialized fertilizer, Inc. produces nearly million tons of phosphogypsum every year, and two gypsum mountains are piled up at present, and the total amount is nearly million tons. The problem of phosphogypsum in cloud, precious and Sichuan areas is more serious, so that the problem of solving the large-scale utilization of waste gypsum is urgent.
At present, the comprehensive utilization of gypsum at home and abroad mainly comprises the following aspects: the cement retarder is used, but the addition amount of the cement retarder is not more than 5% of the total amount, the utilization efficiency is low, and the utilization range is limited; secondly, the activator is used for exciting the activity of the slag cement with high mixing amount; the utilization means is applied more in the America, Japan and the like at present, and the main limiting factors of the utilization means are that the production cost is higher, the market capacity is small, and secondary pollution such as waste water and waste gas can be generated; and fourthly, as a roadbed material, the gypsum can be foamed and expanded when meeting water, so that the road surface is arched.
In the aspect of brick making, a gypsum brick can be prepared by a steam pressing method, phosphogypsum is mainly utilized, firstly, the phosphogypsum is dehydrated to obtain semi-hydrated gypsum, and then, the semi-hydrated gypsum is cooled and recrystallized to obtain dihydrate gypsum, so that a product with certain strength is obtained, in the process, only one raw material of gypsum is used, and the finally obtained sample is not high in strength and can not meet the national standard requirement (the compressive strength is more than 10 MPa); other methods for calcining dihydrate phosphogypsum into a mixture of semi-hydrated gypsum and anhydrous gypsum, and then matching with other materials for press forming and curing brick making, such as the method disclosed in Chinese patent document CN 100364917C, need to pretreat gypsum raw materials and then make bricks, and the methods are all used for processing the dihydrate gypsum without gelling performance into semi-hydrated gypsum or anhydrous gypsum with certain gelling performance in principle, the processing process is complicated, high-temperature calcination is needed, the energy consumption is high, and the problem of gypsum processing cannot be well solved.
Disclosure of Invention
The invention aims to provide a method for curing waste gypsum into a high-strength building material at low temperature, which is beneficial to solving the problems of stacking of the waste gypsum, environmental pollution and the like.
In order to achieve the purpose, the invention directly cures the waste gypsum and other additives at 120-220 ℃ to obtain the high-strength building material which can be used as wall and floor tiles, square tiles, pavement tiles and the like, thus being a method for efficiently treating the waste gypsum. The method comprises the following specific steps:
firstly, 40-75% of waste gypsum, 10-20% of building gravel, 5-25% of cement, 5-30% of fly ash and 5-25% of water are weighed according to the mass percentage ratio, the sum of the contents of the components is equal to 100%, the mixture is obtained by uniformly grinding and stirring, a green body is obtained by compression molding under the pressure of 10-40 Mpa, the green body is placed in a hydrothermal kettle after being demoulded, curing treatment is carried out for 8-24 hours under the environment of 120-220 ℃ and saturated steam, natural drying is carried out after the treatment is finished, and the product is obtained, wherein the flexural strength of the product can reach more than 15MPa through detection.
The waste gypsum is waste gypsum generated in the industrial production process, comprises one of phosphogypsum waste, boron gypsum waste, desulfurized gypsum waste and the like or more than two gypsum wastes mixed according to any proportion, does not need any treatment, and is directly used as a reaction raw material to be added into a reaction system.
The building sand stone is common sand stone in building application, comprises one or more of mountain sand, river sand, sea sand and machine-made sand, and is about 487.6cm when the volume of the prepared product is less than or equal to 1/3 of the volume of a standard brick3In the process, the powder is ground and sieved by a 100-mesh sieve so as to meet the structural performance requirement.
The cement adopts products with the model no less than 32.5.
The invention has the advantages that:
the waste gypsum of the invention has high utilization rate, large waste gypsum consumption and large market capacity of building materials, and can effectively solve the problems of stacking of waste gypsum, pollution to the environment and the like.
2, the high-strength building material gypsum brick prepared by the method has the average flexural strength of more than 11MPa and the highest flexural strength of 18MPa and the compressive strength of 40MPa, and can meet the requirements of various building materials.
3, compared with the traditional method for preparing the gypsum brick by the steam pressing method, the compression strength is improved by about 4 times; compared with the gypsum brick prepared by the sintering method, the compression strength is improved by about 2 times.
4, the method has simple process, lower production cost, low energy consumption in the production process and short period, and is suitable for large-scale production.
Drawings
Figure 1 is an XRD profile of samples obtained by curing the present invention using different amounts of waste phosphogypsum.
FIG. 2 is SEM photograph of waste phosphogypsum raw material used in the experiment of the invention.
FIG. 3 is an SEM photograph of a sample prepared in example 1 of the present invention.
FIG. 4 is an SEM photograph of a sample prepared in example 4 of the present invention.
FIG. 5 is a graph showing flexural strength curves of samples of high-strength building materials prepared at different reaction temperatures according to the present invention.
FIG. 6 is a plot of flexural strength of samples of high strength building materials made according to the present invention at different reaction times.
Detailed Description
The invention is further illustrated by the following examples.
Example 1:
taking waste gypsum, ground building sand, cement and fly ash as raw materials, weighing 50% of waste gypsum, 20% of building sandstone, 15% of cement, 5% of fly ash and 10% of water according to mass, fully grinding and stirring the raw materials, and then pressing and molding the raw materials in an FW-4 tablet press to obtain a green body, wherein the sample is in a cuboid block shape with the length of about 40mm, the width of about 15mm and the thickness of about 5mm, and the molding pressure is 30 MPa; transferring the formed green body into a closed hydrothermal reaction kettle, adding a certain volume of water into the reaction kettle, wherein the specific addition amount is 15% of the volume of the reaction kettle, and then carrying out heating treatment at the heating temperature of 200 ℃ for 8 hours; and taking out the treated sample, and drying the sample in an oven at 80 ℃ for 24 hours to obtain a product solidified body. The three-point method is used for testing the flexural strength, and the result shows that the flexural strength of the sample can reach 18Mpa, thereby meeting the requirement on the strength of the building material.
Example 2:
the method comprises the following steps of taking waste gypsum, ground building sand, cement and fly ash as raw materials, weighing 40% of waste gypsum, 20% of building gravel, 20% of cement, 10% of fly ash and 10% of water according to mass, fully grinding and stirring the raw materials, and then performing compression molding on the raw materials by using an FW-4 tablet press to obtain a green body, wherein the sample is in a cuboid block shape with the length of about 40mm, the width of about 15mm and the thickness of about 5mm, and the molding pressure is 20 MPa; transferring the formed green body into a closed reaction kettle, adding a certain volume of water into the reaction kettle, wherein the specific addition amount is 15% of the volume of the reaction kettle, and then heating at 160 ℃ for 16 hours; and taking out the treated sample, and drying the sample in an oven at 80 ℃ for 24 hours to obtain a product solidified body. The three-point method is used for testing the flexural strength, and the result shows that the flexural strength of the sample can reach 14Mpa, thereby meeting the requirement on the strength of the building material.
Example 3:
the method comprises the following steps of taking waste gypsum, ground building sand, cement and fly ash as raw materials, weighing 60% of waste gypsum, 10% of building gravel, 12% of cement, 8% of fly ash and 10% of water according to mass, fully grinding and stirring the raw materials, and then performing compression molding on the raw materials by using an FW-4 tablet press to obtain a green body, wherein the sample is in a cuboid block shape with the length of about 40mm, the width of about 15mm and the thickness of about 5mm, and the molding pressure is 30 MPa; transferring the formed green body into a closed reaction kettle, adding a certain volume of water into the reaction kettle, wherein the specific addition amount is 15% of the volume of the reaction kettle, and then heating at 120 ℃ for 24 hours; and taking out the treated sample, and drying the sample in an oven at 80 ℃ for 24 hours to obtain a product solidified body. The three-point method is used for testing the flexural strength, and the result shows that the flexural strength of the sample can reach 11Mpa, thereby meeting the requirement on the strength of the building material.
Example 4:
taking waste gypsum, ground building sand, cement and fly ash as raw materials, weighing 70% of waste gypsum, 10% of building sandstone, 8% of cement, 4% of fly ash and 8% of water according to mass, fully grinding and stirring the raw materials, and then pressing and molding the raw materials in an FW-4 tablet press to obtain a green body, wherein the sample is a round block with the diameter of about 50mm and the thickness of about 10mm, and the molding pressure is 30 MPa; transferring the formed green body into a closed reaction kettle, adding a certain volume of water into the reaction kettle, wherein the specific addition amount is 15% of the volume of the reaction kettle, and then heating at 160 ℃ for 12 hours; and taking out the treated sample, and drying the sample in an oven at 80 ℃ for 24 hours to obtain a product solidified body. The flexural strength of the sample can reach 12Mpa, and the requirement of the strength of the building material is met.
A method for solidifying waste gypsum into high-strength building material at low temperature has the reaction principle of simulating the formation process of rock, accelerating the dissolution-precipitation of raw materials under the production condition, greatly improving the solubility of reaction raw materials, accelerating the generation of calcium silicate hydrate and further improving the density of a sample; as the reaction proceeds, the fibrous or flaky tobermorite is finally generated and interwoven with each other to be filled in the gaps of the raw materials, and the strength of the sample is finally improved.
The waste gypsum comprises one of phosphogypsum waste, boron gypsum waste, desulfurized gypsum waste and the like or more than two gypsum wastes which are mixed according to any proportion, does not need any treatment and is directly used as a reaction raw material to be added into a reaction system.
The building sand stone is common sand stone in building application, comprises one or more of mountain sand, river sand, sea sand and machine-made sand, and has a volume of about 487.6cm when the volume of the prepared product is less than or equal to 1/3 of the volume of a standard brick3In the process, the powder is ground and sieved by a 100-mesh sieve so as to meet the structural performance requirement.
The cement adopts products with the model no less than 32.5.
The invention is further illustrated by the following experiments on phosphogypsum waste discharged by the specialized fertilizer Limited of Xuanchen Seiki, Anhui:
fig. 1 shows XRD curves of samples measured when curing is performed using waste phosphogypsum with different addition amounts, and it can be seen from the graphs that, in a certain range, the smaller the addition amount of the waste phosphogypsum, the more obvious the tobermorite peak at 7-8 degrees, and in combination with examples 1-4, when the addition amount of the waste gypsum is 40%, the highest strength of the obtained sample is 18 MPa. This indicates that tobermorite formation has a critical effect on sample strength.
Fig. 2 shows an SEM photograph of the waste phosphogypsum raw material, which can be seen as a granular material with a relatively loose structure, no close packing and non-uniform pore distribution.
Fig. 3 and 4 show SEM photographs of the samples of example 1 and example 4, respectively, from which it is apparent that there is a morphology pattern of fibrous and lamellar structure, tobermorite.
The effect of the different reaction temperatures on the flexural strength of the samples is shown in FIG. 5, from which it can be seen that the higher the reaction temperature, the higher the final strength of the samples, in particular, the final strength of the samples reached 18MPa at a temperature of 200 ℃.
FIG. 6 shows the effect of different reaction times on the flexural strength of the sample, from which it can be seen that the sample strength increases with increasing reaction time within 24 h; thereafter, the sample strength gradually stabilized with further increase in reaction time.
Claims (5)
1. A method for low-temperature curing of waste gypsum into a high-strength building material is characterized by comprising the following steps: firstly, measuring waste gypsum according to mass percentage: building sandstone: cement: fly ash: 40-75% of water: 10-20%: 5-25%: 5-30%: 5-25 percent, wherein the sum of the contents of all the components is equal to 100 percent, uniformly grinding and stirring to obtain a mixture, pressing and forming under the pressure of 10-40 Mpa to obtain a green body, demolding the green body, placing the green body into a hydrothermal kettle, curing at 120-220 ℃ for 8-24 hours, and naturally drying after the treatment is finished to obtain the high-strength building material product.
2. The method of low temperature curing waste gypsum into high strength building material as claimed in claim 1, wherein: the waste gypsum is waste gypsum generated in the industrial production process, and comprises one of phosphogypsum waste, boron gypsum waste and desulfurized gypsum waste or more than two gypsum wastes mixed according to any proportion.
3. The method of low temperature curing waste gypsum into high strength building material as claimed in claim 1, wherein: the building sandstone is common sandstone in building engineering application, and comprises one or more than two kinds of sandstone in mountain sand, river sand, sea sand and machine-made sand which are mixed according to any proportion, and when the volume of the prepared product is less than or equal to 1/3 of the volume of a standard brick, the prepared product needs to be ground and then screened by a 100-mesh sieve.
4. The method of low temperature curing waste gypsum into high strength building material as claimed in claim 1, wherein: the cement is made of products with the model no less than 32.5.
5. The method of low temperature curing waste gypsum into high strength building material as claimed in claim 1, wherein: the fly ash is calcium type fly ash.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH081641A (en) * | 1994-06-23 | 1996-01-09 | Mitsubishi Materials Corp | Method and device for measuring setting time of hemihydrate gypsum as well as method for managing production process of gypsum building material |
| CN104761223A (en) * | 2015-02-04 | 2015-07-08 | 贵州开磷集团股份有限公司 | Phosphogypsum base material imitation jade board and preparation method thereof |
| CN106316326A (en) * | 2016-08-31 | 2017-01-11 | 韩涛 | Method for preparing building material from desulfurization gypsum |
| CN106365578A (en) * | 2016-08-31 | 2017-02-01 | 韩涛 | Method for preparing building material by using phosphogypsum |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH081641A (en) * | 1994-06-23 | 1996-01-09 | Mitsubishi Materials Corp | Method and device for measuring setting time of hemihydrate gypsum as well as method for managing production process of gypsum building material |
| CN104761223A (en) * | 2015-02-04 | 2015-07-08 | 贵州开磷集团股份有限公司 | Phosphogypsum base material imitation jade board and preparation method thereof |
| CN106316326A (en) * | 2016-08-31 | 2017-01-11 | 韩涛 | Method for preparing building material from desulfurization gypsum |
| CN106365578A (en) * | 2016-08-31 | 2017-02-01 | 韩涛 | Method for preparing building material by using phosphogypsum |
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