CN107686255B - Modified phosphogypsum and phosphogypsum rigid waterproof mortar and preparation method thereof - Google Patents
Modified phosphogypsum and phosphogypsum rigid waterproof mortar and preparation method thereof Download PDFInfo
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- CN107686255B CN107686255B CN201710697996.XA CN201710697996A CN107686255B CN 107686255 B CN107686255 B CN 107686255B CN 201710697996 A CN201710697996 A CN 201710697996A CN 107686255 B CN107686255 B CN 107686255B
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- phosphogypsum
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- waterproof mortar
- rigid waterproof
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Classifications
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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
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/14—Acids or salts thereof containing sulfur in the anion, e.g. sulfides
- C04B22/142—Sulfates
- C04B22/143—Calcium-sulfate
- C04B22/144—Phosphogypsum
-
- 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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
-
- 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
-
- 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
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
Abstract
The invention discloses modified phosphogypsum, phosphogypsum rigid waterproof mortar and a preparation method thereof, wherein the modified phosphogypsum is prepared by the following steps: (1) mixing phosphogypsum and quick lime, and aging to obtain an initial material; (2) uniformly mixing the initial material with water, then adjusting the pH value to 6-8, filtering and drying to obtain the treated phosphogypsum; (3) uniformly mixing the treated phosphogypsum with a reaction liquid A to form a mixed liquid B, wherein the reaction liquid A is an ethanol solution of a modifier; (4) adjusting the pH value of the mixed solution B to 6-8, heating, drying and grinding to obtain modified phosphogypsum; the invention can fully utilize the phosphogypsum waste, solves the problem of treatment of the phosphogypsum and lays a foundation for widening the application of the phosphogypsum.
Description
Technical Field
The invention belongs to the field of building waterproofing, and particularly relates to modified phosphogypsum and phosphogypsum rigid waterproof mortar and a preparation method thereof.
Background
The main cause of the damage of the cement-based structures is the corrosion of the cement-based materials due to external environmental factors. Among them, water is an important factor causing durability problems of cement-based structures. It is known that ordinary concrete or mortar is a heterogeneous and porous composite material in nature, and the main measure for reducing the permeability of concrete (mortar) is to reduce the porosity of the concrete, thereby improving the impermeability and waterproof performance of the concrete. The adoption of waterproof materials is a common main measure for improving the impermeability and the waterproof performance of concrete (mortar). The rigid waterproof material is a door of waterproof materials, and is a material formed by mixing a rigid waterproof agent into a cement-based material, and has good waterproof capability and durability.
Phosphogypsum is solid waste residue produced in phosphoric acid production, and each production is 1t P2O54.25-5.66t of phosphogypsum will be produced. If the phosphogypsum is not treated, not only a large amount of land is occupied, but also P in the phosphogypsum2O5And F etc. can cause serious environmental damage. In the prior art, comprehensive treatment of phosphogypsum is an effective way for the building material industry. The application of the phosphogypsum in the building material industry at present mainly comprises the following steps: phosphogypsum is used as a cement retarder; preparing sulfuric acid by using phosphogypsum; producing building gypsum by using phosphogypsum; preparing aerated blocks from phosphogypsum and the like. These methods open up new ways for the utilization of phosphogypsum, but still cannot meet the current demand of ardealite treatment. The field of preparing rigid waterproof materials by modifying phosphogypsum in an internal mixing mode is not reported.
Disclosure of Invention
The invention aims to provide phosphogypsum rigid waterproof mortar and a preparation method thereof aiming at the defects of the prior art, so as to solve the problem of treatment of solid waste phosphogypsum in phosphoric acid production and open up a new way for utilization of phosphogypsum.
In order to achieve the above object, a first aspect of the present invention provides a modified phosphogypsum, which is prepared according to the following method:
(1) mixing phosphogypsum and quick lime, and aging to obtain an initial material;
(2) uniformly mixing the initial material with water, then adjusting the pH value to 6-8, filtering and drying to obtain the treated phosphogypsum;
(3) uniformly mixing the treated phosphogypsum with a reaction liquid A to form a mixed liquid B, wherein the reaction liquid A is an ethanol solution of a modifier;
(4) and adjusting the pH value of the mixed solution B to 6-8, heating, drying and grinding to obtain the modified phosphogypsum.
The invention provides phosphogypsum rigid waterproof mortar, which is prepared from the following raw materials in parts by weight: 250 parts of cement 200-containing materials, 500 parts of fine sand 350-containing materials, 80-160 parts of water, 5-10 parts of nano magnesium oxide, 5-10 parts of fly ash and 1-5 wt% of modified phosphogypsum, wherein the modified phosphogypsum is the modified phosphogypsum.
The third aspect of the invention provides a preparation method of the phosphogypsum rigid waterproof mortar, which comprises the following steps:
mixing cement, nano magnesium oxide, fly ash and fine sand to obtain mixed powder;
mixing the mixed powder with water, adding the modified phosphogypsum, and stirring to obtain a mixed material;
and pouring, vibrating and maintaining the mixed material to obtain the phosphogypsum rigid waterproof mortar.
Compared with the traditional rigid waterproof material and the phosphogypsum cement-based building material, the technical scheme of the invention has the following advantages:
1) the invention can fully utilize the phosphogypsum waste, solves the problem of treatment of the phosphogypsum and lays a foundation for widening the application of the phosphogypsum;
2) the traditional phosphogypsum has the problem of delaying cement hydration in cement-based application, and the phosphogypsum rigid waterproof mortar provided by the invention has moderate setting time and can meet the actual engineering requirements;
3) according to the preparation method of the modified phosphogypsum, the compatibility of the phosphogypsum and a cement-based material is improved by modifying the phosphogypsum, so that the phosphogypsum and the cement-based material have better compatibility;
4) the maximum seepage resistance pressure of the phosphogypsum rigid waterproof mortar provided by the invention can reach 2.8MPa, and the building material industry standard (JC/T984-2011 standard) of the polymer mortar in China stipulates that the seepage resistance pressure of 28d is not less than 1.5MPa, namely the phosphogypsum rigid waterproof mortar is qualified, so that the seepage resistance pressure of the phosphogypsum rigid waterproof mortar disclosed by the invention far exceeds the industry standard;
5) the preparation method of the phosphogypsum rigid waterproof mortar is simple and easy to popularize.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The first aspect of the invention provides a modified phosphogypsum, which is prepared according to the following method:
(1) mixing phosphogypsum and quick lime, and aging to obtain an initial material;
(2) uniformly mixing the initial material with water, then adjusting the pH value to 6-8, filtering and drying to obtain the treated phosphogypsum;
(3) uniformly mixing the treated phosphogypsum with a reaction liquid A to form a mixed liquid B, wherein the reaction liquid A is an ethanol solution of a modifier;
(4) and adjusting the pH value of the mixed solution B to 6-8, heating, drying and grinding to obtain the modified phosphogypsum.
According to the invention, preferably, the quicklime is 5-20 parts by mass relative to 100 parts of the phosphogypsum.
According to the invention, preferably, the aging time is from 12 to 36 h.
According to the invention, the mass ratio of the initial material to the water is preferably 1: 0.3-0.8.
According to the invention, the pH is preferably adjusted with ammonia.
According to the invention, preferably, the modifier is KH560 in an amount of 2-4 wt% of the weight of the treated phosphogypsum.
According to the present invention, preferably, the method of heat drying includes: and placing the mixed solution B into a microwave reactor, and radiating and heating the mixed solution B to be completely dried by using power of 800-1200W.
According to the present invention, preferably, the method of milling comprises: ball milling is carried out for 20-40min at the rotating speed of 600r/min and the modified phosphogypsum is obtained after being taken out and sieved for 140 meshes and 180 meshes.
The invention provides phosphogypsum rigid waterproof mortar, which is prepared from the following raw materials in parts by weight: 250 parts of cement 200-containing materials, 500 parts of fine sand 350-containing materials, 80-160 parts of water, 5-10 parts of nano magnesium oxide, 5-10 parts of fly ash and 1-5 wt% of modified phosphogypsum, wherein the modified phosphogypsum is the modified phosphogypsum.
The third aspect of the invention provides a preparation method of the phosphogypsum rigid waterproof mortar, which comprises the following steps:
mixing cement, nano magnesium oxide, fly ash and fine sand to obtain mixed powder;
mixing the mixed powder with water, adding the modified phosphogypsum, and stirring to obtain a mixed material;
and pouring, vibrating and maintaining the mixed material to obtain the phosphogypsum rigid waterproof mortar.
Preferably, the materials are mixed by a stirrer, and the stirring time of the mixed powder is 50-80 s; the stirring time of the mixed powder and water is 50-80 s; adding the modified phosphogypsum, and stirring to obtain a mixed material, wherein the stirring time is 60-120 s; the curing time was 28 d.
The raw materials for preparing the phosphogypsum rigid waterproof mortar can be obtained commercially.
The invention is further illustrated by the following examples:
the modifier used in the invention is purchased from the Hubei province and the chemical industry Co., Ltd, and has the model of KH 560.
Example 1
The embodiment provides phosphogypsum rigid waterproof mortar, and the preparation method comprises the following steps: pouring 200 parts of cement, 5 parts of nano magnesium oxide, 5 parts of fly ash and 350 parts of fine sand which are weighed into a stirrer in parts by mass, and stirring for 50-80 seconds; then 100 parts of weighed water is poured into the mixture and stirred for 50 to 80 seconds; finally, pouring modified phosphogypsum with the mixing amount of 1 wt% of the cement amount, stirring for 60-120 seconds, pouring, vibrating, and curing for 28 days under standard curing conditions to obtain the phosphogypsum rigid waterproof mortar;
the modified phosphogypsum is prepared by the following steps:
(1) mixing phosphogypsum and quicklime, and aging for 24 hours to obtain an initial material, wherein the parts by mass of the quicklime are 10 parts relative to 100 parts of the phosphogypsum;
(2) pouring the initial material and water into a mixer to be uniformly mixed, then adjusting the pH value to 6-8 by using ammonia water, filtering and drying to obtain the treated phosphogypsum, wherein the mass ratio of the initial material to the water is 1: 0.5;
(3) uniformly mixing the treated phosphogypsum with a reaction liquid A to form a mixed liquid B, wherein the reaction liquid A is an ethanol solution of a modifier, and the dosage of the modifier is 3 wt% of the weight of the treated phosphogypsum;
(4) adjusting the pH value of the mixed solution B to 6-8 by using ammonia water, placing the mixed solution B into a microwave reactor, heating the mixed solution B by radiation with the power of 1000W until the mixed solution B is completely dried, carrying out ball milling for 30min at the rotating speed of 500r/min, taking out the mixed solution, and sieving the mixed solution with a 160-mesh sieve to obtain the modified phosphogypsum.
Example 2
The embodiment provides phosphogypsum rigid waterproof mortar, and the preparation method comprises the following steps: pouring 220 parts of cement, 5 parts of nano magnesium oxide, 10 parts of fly ash and 400 parts of fine sand which are weighed into a stirrer in parts by mass, and stirring for 50-80 seconds; then, adding 80 parts of weighed water and stirring for 50-80 seconds; finally, pouring the modified phosphogypsum with the doping amount of 3 wt% of the cement amount, stirring for 60-120 seconds, pouring, vibrating, and curing for 28 days under standard curing conditions to obtain the phosphogypsum rigid waterproof mortar;
the preparation method, parameters and the use amount of each material of the modified phosphogypsum of the embodiment are the same as those of the embodiment 1.
Example 3
The embodiment provides phosphogypsum rigid waterproof mortar, and the preparation method comprises the following steps: pouring 250 parts of cement, 8 parts of nano magnesium oxide, 5 parts of fly ash and 350 parts of fine sand which are weighed into a stirrer in parts by mass, and stirring for 50-80 seconds; then 100 parts of weighed water is poured into the mixture and stirred for 50 to 80 seconds; finally, pouring modified phosphogypsum with the mixing amount of 5 wt% of the cement amount, stirring for 60-120 seconds, pouring, vibrating, and curing for 28 days under standard curing conditions to obtain the phosphogypsum rigid waterproof mortar;
the preparation method, parameters and the use amount of each material of the modified phosphogypsum of the embodiment are the same as those of the embodiment 1.
Example 4
The embodiment provides phosphogypsum rigid waterproof mortar, and the preparation method comprises the following steps: pouring 250 parts of cement, 10 parts of nano magnesium oxide, 5 parts of fly ash and 500 parts of fine sand into a stirrer, and stirring for 50-80 seconds; then adding 120 parts of weighed water and stirring for 50-80 seconds; finally, pouring the modified phosphogypsum with the doping amount of 3 wt% of the cement amount, stirring for 60-120 seconds, pouring, vibrating, and curing for 28 days under standard curing conditions to obtain the phosphogypsum rigid waterproof mortar;
the preparation method, parameters and the use amount of each material of the modified phosphogypsum of the embodiment are the same as those of the embodiment 1.
Example 5
The embodiment provides phosphogypsum rigid waterproof mortar, and the preparation method comprises the following steps: pouring 220 parts of cement, 8 parts of nano magnesium oxide, 8 parts of fly ash and 500 parts of fine sand which are weighed into a stirrer in parts by mass, and stirring for 50-80 seconds; then, 160 parts of weighed water is poured into the mixture and stirred for 50 to 80 seconds; finally, pouring modified phosphogypsum with the mixing amount of 1 wt% of the cement amount, stirring for 60-120 seconds, pouring, vibrating, and curing for 28 days under standard curing conditions to obtain the phosphogypsum rigid waterproof mortar;
the preparation method, parameters and the use amount of each material of the modified phosphogypsum of the embodiment are the same as those of the embodiment 1.
Example 6
The embodiment provides phosphogypsum rigid waterproof mortar, and the preparation method comprises the following steps: pouring 200 parts of cement, 10 parts of nano-magnesia, 5 parts of fly ash and 500 parts of fine sand into a stirrer, and stirring for 50-80 seconds; then adding 120 parts of weighed water and stirring for 50-80 seconds; finally, pouring modified phosphogypsum with the mixing amount of 5 wt% of the cement amount, stirring for 60-120 seconds, pouring, vibrating, and curing for 28 days under standard curing conditions to obtain the phosphogypsum rigid waterproof mortar;
the preparation method, parameters and the use amount of each material of the modified phosphogypsum of the embodiment are the same as those of the embodiment 1.
Test example
The samples 1-6 of the invention are tested for permeation resistance pressure according to JC/T984-2011 standard, and the samples 1-6 of the invention are tested for cracking resistance according to JC/T951-2005 standard, and the specific test results are shown in Table 1.
TABLE 1 phosphogypsum rigid waterproof mortar performance test results
| Detecting items | The cracking resistance is more than gamma% | Osmotic pressure resistance/MPa |
| EXAMPLE 1 | -4.5 | 2.3 |
| EXAMPLE 2 | -3.8 | 2.1 |
| EXAMPLE 3 | -6.8 | 2.2 |
| EXAMPLE 4 | -4.5 | 2.8 |
| EXAMPLE 5 | -5.2 | 2.6 |
| EXAMPLE 6 | -5.1 | 2.7 |
The test results show that the ardealite rigid waterproof mortar of the examples 1 to 6 has good cracking resistance and seepage pressure resistance; wherein, the comprehensive detection results of the examples 4 to 6 are better than those of the examples 1 to 3; the permeation resistance pressure of the embodiment 4 reaches 2.8MPa, which is far beyond the industry standard of 1.5 MPa.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (8)
1. The phosphogypsum rigid waterproof mortar is characterized by being prepared from the following raw materials in parts by weight: 250 parts of cement 200-doped materials, 500 parts of fine sand 350-doped materials, 80-160 parts of water, 5-10 parts of nano magnesium oxide, 5-10 parts of fly ash and modified phosphogypsum, wherein the doping amount is 1-5 wt% of the using amount of the cement, and the modified phosphogypsum is prepared by the following method:
(1) mixing phosphogypsum and quick lime, and aging to obtain an initial material;
(2) uniformly mixing the initial material with water, then adjusting the pH value to 6-8, filtering and drying to obtain the treated phosphogypsum;
(3) uniformly mixing the treated phosphogypsum with a reaction liquid A to form a mixed liquid B, wherein the reaction liquid A is an ethanol solution of a modifier;
(4) adjusting the pH value of the mixed solution B to 6-8, heating, drying and grinding to obtain modified phosphogypsum;
the modifier is KH560, and the dosage of the modifier is 2-4 wt% of the weight of the treated phosphogypsum.
2. The phosphogypsum rigid waterproof mortar according to claim 1, wherein the quicklime is 5-20 parts by mass relative to 100 parts of phosphogypsum.
3. The phosphogypsum rigid waterproof mortar according to claim 1, wherein the aging time is from 12 to 36 h.
4. The phosphogypsum rigid waterproof mortar according to claim 1, wherein the mass ratio of the initial material to the water is 1: 0.3-0.8.
5. The phosphogypsum rigid waterproof mortar according to claim 1, wherein the PH is adjusted with ammonia.
6. The phosphogypsum rigid waterproof mortar according to claim 1, wherein the method of thermal drying comprises: and placing the mixed solution B into a microwave reactor, and radiating and heating the mixed solution B to be completely dried by using power of 800-1200W.
7. The phosphogypsum rigid waterproof mortar according to claim 1, wherein the method of grinding comprises: ball milling is carried out for 20-40min at the rotating speed of 600r/min and the modified phosphogypsum is obtained after being taken out and sieved for 140 meshes and 180 meshes.
8. The process for the preparation of phosphogypsum rigid waterproof mortar according to claim 1, characterized in that it comprises:
mixing cement, nano magnesium oxide, fly ash and fine sand to obtain mixed powder;
mixing the mixed powder with water, adding the modified phosphogypsum, and stirring to obtain a mixed material;
and pouring, vibrating and maintaining the mixed material to obtain the phosphogypsum rigid waterproof mortar.
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| CN101565293B (en) * | 2009-06-04 | 2012-02-08 | 何昌霖 | modified phosphogypsum and preparation method thereof |
| CN103717548B (en) * | 2011-06-09 | 2016-08-17 | 新泽西州州立大学(拉特格斯) | Synthesis formulation and preparation and application thereof |
| CN105347765A (en) * | 2015-10-23 | 2016-02-24 | 潍坊德霖建材科技有限公司 | Phosphogypsum waterproof dry-mixed mortar |
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