CN115340347B - Phosphogypsum-based NRC strong acid-resistant and freeze-thawing-resistant composite impermeable material and preparation method thereof - Google Patents
Phosphogypsum-based NRC strong acid-resistant and freeze-thawing-resistant composite impermeable material and preparation method thereof Download PDFInfo
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00293—Materials impermeable to liquids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention belongs to the technical field of impermeable materials, and provides an NRC strong acid resistant and freeze-thawing resistant composite impermeable material based on phosphogypsum and a preparation method thereof. The material comprises the following raw materials in percentage by weight: 30-70% of phosphogypsum, 5-10% of PMSB, 1% of high polymer flocculant, 10-35% of graded sand and 14-24% of water. By utilizing the ultra-high expansion performance of PMSB, when percolate passes through, the porous structure in graded sand is expanded and filled, and meanwhile, by utilizing the characteristic that phosphogypsum material has cohesive force, a powerful compact body with a gel structure is formed under the action of a flocculating agent. The composite impermeable material has good acid resistance and freeze-thawing resistance, wide application range and good market prospect.
Description
Technical Field
The invention relates to the technical field of impermeable materials, in particular to an NRC strong acid resistant and freeze-thawing resistant composite impermeable material based on phosphogypsum and a preparation method thereof.
Background
At present, the seepage prevention technologyThe method has wide application in industrial and civil structures such as industrial residue reservoirs, tailing reservoirs containing heavy metals, industrial factories, tank areas, polluted sites, river channels, ponds, reservoirs, dams and the like, and provides reliable long-term protection for groundwater, air and soil. The impermeable material mainly comprises natural clay and HDPE impermeable film. But most clays have a high permeability coefficient (less than 10 -7 cm/s) and degree of compaction>95%) of the natural clay lining layer does not meet the national standard requirements, and moreover, the natural clay lining layer often generates cracks due to uneven sedimentation or drying, so that the seepage-proofing effect of the natural clay lining layer is obviously weakened. Although the HDPE impermeable membrane has good impermeable performance, the HDPE impermeable membrane has the defects of high cost and high construction difficulty.
Phosphogypsum is a waste produced in the phosphorus chemical industry, and 4.5-5.0 tons of phosphogypsum byproducts can be produced by producing 1 ton of phosphoric acid. The rapid development of the phosphorus chemical industry brings huge-magnitude phosphogypsum stockpiling amount which exceeds 6 hundred million tons by 2020, and annual production amount of 7500 ten thousand tons. Occupies a large amount of land, and the soil-water pollution and the environmental problem become a big bottleneck restricting the development of the phosphate fertilizer industry.
Phosphogypsum is currently less studied for use as a barrier material. Chinese patent No. 108751890A discloses a novel environment-friendly impermeable material based on phosphogypsum, which takes phosphogypsum, bentonite and polymer as main raw materials. The impermeable material has poor practical effect on severe environments, especially acidic and extremely cold conditions.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the weather resistance of the seepage-proofing material is not added in the prior art, thereby providing the phosphogypsum-based NRC strong acid-resistant and freeze-thawing-resistant composite seepage-proofing material. The phosphogypsum is used as a base material, and the modified clay material is compounded to form the novel composite impermeable material, and the composite impermeable material can well cope with complex service environments and working conditions such as strong acid, extremely cold, dry and wet circulation and the like, keep extremely low permeability coefficient, and can simultaneously solve the dual environmental problems of the multi-way comprehensive utilization of phosphogypsum and the leakage failure of a solid waste landfill.
The invention provides an phosphogypsum-based NRC strong acid resistant and freeze-thawing resistant composite impermeable material, which comprises the following raw material components in percentage by weight: 30-70% of phosphogypsum, 5-10% of PMSB, 1% of high polymer flocculant, 10-35% of graded sand and 14-24% of water.
It should be noted that the composite impermeable material may also be composed of the above raw material components.
Preferably, the grain diameter of the graded sand is less than or equal to 1mm, and the water content is less than 12%; the dry weight content of the part with the particle size of 0.15-0.7mm is more than 50%.
Preferably, the PMSB has a water content of < 13% and an expansion index of 60mL/2g or more.
The PMSB is polymer modified sand and bentonite material (Polymer modified Sand Bentonite), and the preparation process is ZL202110265306.X.
Preferably, the high molecular polymer flocculant comprises any one of cellulose ether, PVA and PAM.
Preferably, the compactness of the impermeable material is more than or equal to 90%.
The invention also provides a preparation method of the phosphogypsum-based NRC strong acid-resistant and freeze-thawing-resistant composite impermeable material, which comprises the following steps:
(1) Taking PMSB according to weight percentage, drying, grinding, sieving with a 120-mesh sieve, taking clean graded sand, and fully mixing for standby;
(2) Taking phosphogypsum according to the weight percentage, drying, grinding and sieving with a 120-mesh sieve for standby;
(3) Taking a high molecular polymer flocculant according to the weight percentage, and adding the high molecular polymer flocculant into water for full dissolution for standby;
(4) Mixing the raw materials in (1), 2) and (3), and continuously stirring until the raw materials are uniformly mixed;
(5) And compacting the uniformly mixed mixture with the optimal water content to 90% of compactness to obtain the water-based paint.
The invention utilizes the ultra-high expansion performance of PMSB, and expands and fills the pore structure in graded sand when percolate passes through, and simultaneously utilizes the characteristic of the phosphogypsum material having cohesive force to form a powerful compact body with a gel structure under the action of a high polymer flocculant. Meanwhile, because phosphogypsum has acid resistance and PMSB has acid resistance, the phosphogypsum has the following characteristicsThe composite impermeable material has the characteristic of resisting corrosion of strong acid, and the permeability coefficient is kept at 10 under the action of the pH=1 strong acid percolate -8 cm/s, even below 10 -8 cm/s. Due to the water swelling and water loss shrinkage characteristics of PMSB, the composite impermeable material has self-healing characteristics, namely the crack rate is 3.8% -5.27% under the dry condition, and the crack rate is reduced to 0.03% -0.12% under the wet condition because of the self-healing phenomenon of the swelling characteristics. In addition, under the action of the high molecular polymer flocculant, the composite material has freeze-thawing resistance, namely the thawing cycle action after freezing has no influence on the impermeability.
The technical scheme of the invention has the following advantages:
the invention provides an phosphogypsum-based NRC strong acid-resistant and freeze-thawing-resistant composite impermeable material, which utilizes the ultra-high expansion characteristic of PMSB, and hydrophilic functional groups are carried in the impermeable material after meeting water to improve the expansion performance of bentonite, so that a three-dimensional crosslinking effect is generated, and a compact colloid structure and a more tortuous seepage path are formed by combining phosphogypsum fine particles, thereby effectively blocking water infiltration. Permeability coefficient lower than 10 -8 cm/s. Has good self-healing property, and the crack rate is reduced to 0.03-0.12% under the condition of wetting after drying. Meanwhile, the osmotic coefficient of the water-based paint is basically unchanged after 3 times of circulation under the freezing and thawing condition, and the water-based paint also has excellent freezing and thawing resistance after 9 times of circulation.
The composite impermeable material prepared by the invention has wide raw material sources and simple preparation method. The composite material can be used for metal/nonmetal tailing pond seepage prevention, pollutant seepage prevention vertical barriers, refuse landfill seepage prevention, artificial river/pond seepage prevention, roadbed seepage prevention, equalizing basin seepage prevention, top seepage prevention of various solid landfill sites and the like, and has remarkable market popularization value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of the morphology of the composite barrier material prepared in example 1 of the present invention before self-healing (left upper) and after self-healing (right lower) and the fracture rate after self-healing (left lower);
FIG. 2 is a graph of the permeation effects after freeze-thaw cycles of the composite barrier material prepared in example 4 of the present invention.
Detailed Description
Each of the technical solutions defined in the claims is supported.
Examples 1 to 5
The raw material compositions of examples 1-5 and comparative examples 1-5 in weight percent for phosphogypsum-based NRC strong acid and freeze-thaw resistant composite barrier materials are shown in Table 1.
TABLE 1
Wherein, the PMSB preparation process is ZL202110265306. X; the water content is less than 13%, and the expansion index is more than or equal to 60mL/2g. The bentonite is common commercial sodium bentonite.
Wherein the high polymer flocculant is selected from any one of cellulose ether, PVA and PAM.
Wherein the grain diameter of the graded sand is less than or equal to 1mm, and the water content is less than 12%; the dry weight content of the part with the particle size of 0.15-0.7mm is more than 50%.
The formulation according to table 1 was prepared according to the following preparation method comprising the steps of:
(1) Taking PMSB according to weight percentage, drying, grinding, sieving with a 120-mesh sieve, taking clean graded sand, and fully mixing for standby;
(2) Taking phosphogypsum according to the weight percentage, drying, grinding and sieving with a 120-mesh sieve for standby;
(3) Taking a high molecular polymer flocculant according to the weight percentage, and adding the high molecular polymer flocculant into water for full dissolution for standby;
(4) Mixing the raw materials in (1), 2) and (3), and continuously stirring until the raw materials are uniformly mixed;
(5) And compacting the uniformly mixed mixture with the optimal water content to 90% of compactness to obtain the water-based paint.
The composite impermeable material prepared in the example was immersed in pure water and ph=1 for one week, and the permeability coefficient was measured, and the results are shown in table 2.
TABLE 2
As can be seen from Table 2, the composite impermeable material prepared by the invention has the characteristic of resisting corrosion of strong acid, and the permeability coefficient is kept at 10 under the action of the pH=1 strong acid percolate -8 cm/s to 10 -9 cm/s scale. Example 1 differs from comparative example 1 in that example 1 uses 10% loading of the modified PMSB material, whereas comparative example 1 uses 10% loading of natural sodium bentonite, as compared to example 2.37X10 in pure water and strong acid -9 cm/s and 7.55X10 -9 The permeability coefficient in cm/s was increased to 3.21X10 for the comparative example -8 cm/s and 1.97X10 -7 cm/s。
The composite impermeable material prepared in the example 4 is subjected to self-healing performance test, a standard sample is firstly placed into a saturated cylinder for air suction in a dry-wet cycle test, water is filled into the cylinder, the sample is saturated for 24 hours after air suction is performed until the sample is completely saturated, and then the saturated sample is placed into an oven for drying until the sample is dried until the quality is not changed, so that the dry-wet cycle is completed. The surface morphology of the sample in the saturated state of the dryer in the dry and wet cycle was recorded by a high resolution camera and analyzed by Image J binarization processing software, and the result is shown in FIG. 1. It should be noted that the crack rate of the composite impermeable material prepared in the other examples is 3.8% -5.27% under the dry condition, and the crack rate is reduced to 0.03% -0.12% under the wet condition because of the self-healing phenomenon of the expansion characteristic of the crack.
The composite impermeable material prepared in the example 4 is compared with the natural sodium bentonite in the comparative example 3 added with a high molecular polymer flocculant and the natural sodium bentonite in the comparative example 4 according to GB/T50123-2019 to respectively carry out permeation tests under the influence of cyclic freeze thawing, and the results are shown in Table 3.
TABLE 3 Table 3
As is clear from Table 3, the invention utilizes the ultra-high expansion property of PMSB, and the porous structure in graded sand is expanded and filled when percolate passes through, and meanwhile, the phosphogypsum material has the characteristic of cohesive force, and forms a strong compact body with a gel structure under the action of the high polymer flocculant, and the high polymer flocculant can protect the compact body from frost heaving damage and crack under the low temperature condition, thereby having better freeze-thawing resistance, and the invention still maintains 10 even after 9 freeze-thawing cycles occur in example 4 -9 Ultra-low permeability coefficient on the order of cm/s. Example 4 shows that the permeability coefficient of the material is basically unchanged after 1 time and 2 times of freeze thawing cycles respectively, and the morphology is basically unchanged after 1 time and 2 times of freeze thawing cycles respectively in fig. 2, which also shows that the material has better freeze thawing resistance. While comparative examples 3 and 4 had an osmotic coefficient increased to 10 after 2 and 1 freeze-thaw cycles, respectively -8 cm/s scale. The osmotic coefficient of the comparative example 3 and the comparative example 4 is increased by 2 orders of magnitude after 9 freeze-thawing cycles, and the freeze-thawing cycle resistance is poor. Compared with comparative example 4, the freezing and thawing resistance of comparative example 3 added with the polymeric flocculant is improved to a very small extent, because the components cannot form a compact body or form a three-dimensional cross-linked and tortuous seepage channel under the condition that only the polymeric flocculant exists, and the freezing and thawing resistance of the comparative example 3 cannot be effectively improved by independently adding the polymeric flocculant.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (5)
1. The phosphogypsum-based NRC strong acid-resistant and freeze-thawing-resistant composite impermeable material is characterized by comprising the following raw material components in percentage by weight: 30-70% of phosphogypsum, 5-10% of PMSB, 1% of high polymer flocculant, 10-35% of graded sand and 14-24% of water; the high polymer flocculant comprises any one of cellulose ether, PVA and PAM; the PMSB is polymer modified sand and bentonite material, and the raw material components of the PMSB comprise, by weight: 70-75% of fine sand, 2-3% of sodium bentonite, 4-5% of high polymer and 15-20% of water;
the high molecular polymer is prepared from methacrylamide, acrylic acid and sodium hydroxide;
the mass ratio of the methacrylamide to the acrylic acid is 1:12-13;
the mass ratio of the acrylic acid to the sodium hydroxide is 1:0.38-0.42;
the preparation method comprises the following steps:
s1, taking clean fine sand and sodium bentonite according to a weight ratio, adding methacrylamide into a container, adding a proper amount of water, and uniformly stirring to obtain a sand-soil mixture;
s2, weighing acrylic acid and sodium hydroxide according to the mass ratio, dissolving the sodium hydroxide in water, and fully cooling to room temperature to obtain a sodium hydroxide solution;
s3, placing the acrylic acid container in a water bath environment, gradually adding sodium hydroxide solution, and continuously stirring the acrylic acid container until the acrylic acid container is cooled to room temperature, wherein the temperature change of the container is kept to be less than 10 ℃ all the time in the adding process;
s4, adding the sodium acrylate monomer solution fully reacted in the S3 into the sand mixture prepared in the S1, continuously stirring until the whole soil body is sticky, and continuously stirring for 3-5min to obtain slurry;
s5, taking out the slurry uniformly stirred in the step S4, and placing the slurry in a constant-temperature 75 ℃ environment for heat preservation treatment, thus obtaining the composite material.
2. The phosphogypsum-based NRC strong acid and freeze-thawing resistant composite impermeable material according to claim 1, wherein the grain size of the graded sand is less than or equal to 1mm, and the water content is less than 12%; the dry weight content of the part with the particle size of 0.15-0.7mm is more than 50%.
3. The phosphogypsum-based NRC strong acid and freeze-thawing resistant composite impermeable material according to claim 1, wherein the PMSB has a water content of less than 13% and an expansion index of more than or equal to 60mL/2g.
4. The phosphogypsum-based NRC strong acid resistant and freeze thawing resistant composite impermeable material according to any one of claims 1-3, wherein the compaction is not less than 90%.
5. The method for preparing the phosphogypsum-based NRC strong acid resistant and freeze thawing resistant composite impermeable material as claimed in any one of claims 1-4, which is characterized by comprising the following steps:
(1) Taking PMSB according to weight percentage, drying, grinding, sieving with a 120-mesh sieve, taking clean graded sand, and fully mixing for standby;
(2) Taking phosphogypsum according to the weight percentage, drying, grinding and sieving with a 120-mesh sieve for standby;
(3) Taking a high molecular polymer flocculant according to the weight percentage, and adding the high molecular polymer flocculant into water for full dissolution for standby;
(4) Mixing the raw materials in (1), 2) and (3), and continuously stirring until the raw materials are uniformly mixed;
(5) And compacting the uniformly mixed mixture with the optimal water content to 90% of compactness to obtain the water-based paint.
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