CN111484265A - Cement retarder prepared from nickel gypsum waste residues and preparation method thereof - Google Patents
Cement retarder prepared from nickel gypsum waste residues and preparation method thereof Download PDFInfo
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- CN111484265A CN111484265A CN202010323857.2A CN202010323857A CN111484265A CN 111484265 A CN111484265 A CN 111484265A CN 202010323857 A CN202010323857 A CN 202010323857A CN 111484265 A CN111484265 A CN 111484265A
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- gypsum
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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
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a cement retarder prepared from nickel gypsum waste residues and a preparation method thereof. The method comprises the following steps: (1) mixing the waste residue with an inerting agent, and adding water to keep moisture and inerting; (2) and adding the gypsum activity excitant into the inerted mixed material, uniformly mixing, and exciting for a proper time to obtain the cement retarder. Compared with the normal cement sold on the market, the cement prepared by adopting the cement retarder has the advantages that the performance is comparable, and all indexes meet the national standard, namely, the waste residues generated by industrial and mining enterprises can be recycled by adopting the method disclosed by the invention, a cement raw material with excellent performance and low price is obtained, the waste is changed into valuable, and the cement retarder has good environmental benefit and economic benefit.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a cement retarder prepared from nickel gypsum waste residues and a preparation method thereof.
Background
With the continuous progress of society, the demand of various metals is increasing, especially lithium, nickel, manganese, nonferrous metals, and the like. The metals are active and generally exist in the ore in the form of compounds in nature, a series of complicated methods are needed for extracting the metals, and a large amount of waste residues are left after extraction. The waste residues generated by industrial and mining enterprises are various in forms, and one of the waste residues is desulfurized slag. The desulfurization slag is waste slag generated by neutralizing liquid containing sulfuric acid with lime or limestone powder in the production process, and a review report and a detection report during the production process determine that the waste slag is general solid waste, so that the waste slag is mostly and directly stacked in a slag yard, and the stacking of the waste slag is the most painful problem of most industrial and mining enterprises, not only occupies a large amount of land, but also easily causes the problems of environmental pollution and material waste.
At present, the construction industry of China is developing vigorously and rapidly, the cement required in the construction of building engineering is also increased rapidly, but the existing cement formula and production method are various, but the problems of high cost, complex method, substandard cement quality and the like exist, especially the pollution to the environment is large, and the body health of people is seriously influenced.
Disclosure of Invention
Aiming at the prior art, the invention provides a cement retarder prepared from nickel gypsum waste residues and a preparation method thereof, so as to achieve the purposes of recycling the waste residues and reducing the production cost of cement.
In order to achieve the purpose, the invention adopts the technical scheme that: the method for preparing the cement by using the waste residues comprises the following steps:
s1: 60 to 65 weight percent of CaSO4·2H2O and 15-18 wt% of active SiO2The nickel gypsum waste residue is crushed and then mixed with an inerting agent to obtain a mixed material; then adding water, mixing uniformly, and preserving moisture and inerting for 18-25 days at 10-40 ℃;
s2: and adding a gypsum activity excitant into the inerted mixture, uniformly mixing, and exciting for 8-12 days at 20-25 ℃ to obtain the cement retarder.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the mass ratio of the waste residue to the inerting agent in the mixed material is 50: 1-3.
Further, the inerting agent is an agent capable of inerting the active SiO2To render it inactive.
Further, the inerting agent is sodium hydroxide or calcium hydroxide, and the effective content of the inerting agent is not less than 60%.
The invention takes the main mineral as CaSO4·2H2O and active SiO2The waste residue is used as a raw material, and after inerting, activity excitation and other treatments, low-grade gypsum can be prepared and can be used as a cement retarder. The basic principle of the process of the invention is as follows: inerting of SiO with inerting agent2And other impurities are subjected to chemical reaction in the use process of cement, and the CaSO in the waste residue is excited by a gypsum activity excitant4·2H2And the activity of O is used for improving the nucleation and growth rate of dihydrate gypsum crystals, so that the cement material with better strength and water resistance is prepared.
The main function of the inerting agent in the present invention is to make the active SiO2To make it inactive, thereby enabling the active SiO2Any inactive reagent is suitable for use in the process of the present invention. In the invention, sodium hydroxide or calcium hydroxide is preferably used as an inerting agent, and in the inerting process, alkali reacts with silicon dioxide to form a cross-linked substance on the surface, so that the chemical reaction of internal silicon dioxide and other impurities in the cement using process is hindered, the stability and the strength of a final product are improved, the final product is used as one of the components in the cement, the performance of the cement is not influenced, a small amount of heavy metal in the nickel gypsum can be effectively solidified, and the use safety of the cement is improved.
Further, the mixed material in the S1 and water are mixed according to the material-liquid ratio of 1: 3-5 g/m L, the inerting temperature is 24-30 ℃, and the inerting time is 20 days.
Further, the mass ratio of the gypsum activity excitant added in the S2 to the inerted mixed material is 1-3: 20.
Further, the gypsum activity excitant comprises the following components in parts by mass:
5-10 parts of sodium oxalate, 2-4 parts of sodium sulfate, 3-6 parts of potassium chloride and 2-4 parts of sodium dodecyl sulfate.
Further, the gypsum activity excitant comprises the following components in parts by mass:
8 parts of sodium oxalate, 3 parts of sodium sulfate, 5 parts of potassium chloride and 3 parts of sodium dodecyl sulfate.
The gypsum powder of the inventionThe sexual excitant is used for exciting the activity of the gypsum, so that reagents capable of improving the activity of the gypsum are all suitable for the process. The gypsum activity excitant in the invention preferably adopts a mixture consisting of sodium oxalate, sodium sulfate, potassium chloride and sodium dodecyl sulfate, and the sodium dodecyl sulfate in the mixture can be used as a surfactant to promote the mutual mixing of the components, so that the prepared low-grade gypsum has uniform texture and can be used as CaSO4·2H2The crystal morphology regulator of O adopts sodium dodecyl sulfate in the invention to regulate the crystal morphology of CaSO4·2H2The crystal morphology of O is adjusted to be regular needle-column-shaped crystals, and the strength of the final product is improved; the potassium chloride in the mixture is a reinforcing agent, so that hydration heat release of a final product can be reduced, the stability of the product is improved, and the strength of the finished cement is improved and is more stable; sodium oxalate and sodium sulfate in the mixture interact to form high SO4 2-The liquid phase with the concentration forms a crystallization supersaturated solution of the dihydrate gypsum, has the conditions of nucleation and growth of the dihydrate gypsum crystal, and improves the crystallization saturation of the dihydrate gypsum and the nucleation and growth rate of the dihydrate gypsum crystal by using sodium oxalate; due to SO4 2-The influence on the nucleation and growth of the dihydrate gypsum crystal is more than that of Ca2+The addition of sodium sulfate breaks the liquid phase SO4 2-With Ca2+The balance relationship of the structure is beneficial to the formation of the polyhedral structure element and the layered structure of the dihydrate gypsum structure, the dihydrate gypsum crystal is promoted to be transformed from a plate shape to a needle-column-shaped crystal shape, and the hydration speed and the strength of the final product are improved.
The invention also claims a cement retarder prepared from the nickel gypsum waste residue, and the cement retarder is prepared by the method.
The invention has the beneficial effects that: the process of the invention prepares the nickel gypsum waste residue into the cement retarder, has simple and convenient preparation process, can effectively solve the problems of land waste and environmental pollution caused by stacking the waste residue, can realize recycling of the waste residue, and has remarkable economic benefit and social benefit. In addition, the product prepared by the method of the invention meets the technical standard of cement retarder materials, can meet various indexes of national standards of cement, is cement with excellent performance, and can be applied to various occasions. Meanwhile, the content of the invention provides reference and reference for the application of the industrial gypsum with similar composition.
Detailed Description
Raw materials
1. Waste residues: the desulfurization slag is stacked in two factory areas of Qinglongzhen forever in Pengshan area in Meishan city by Nippon national Mitsu New Material Co., Sichuan province, and the components of the waste slag are shown in Table 1.
TABLE 1 chemical composition of the waste residue
XRD analysis shows that the waste slag mainly contains CaSO4·2H2O and active SiO2。
Other materials are derived from commercial industrial grade feedstocks.
The following examples are provided to illustrate specific embodiments of the present invention.
Example 1
A cement retarder prepared from nickel gypsum waste residues is prepared by the following steps:
s1, crushing the nickel gypsum waste residue into particles with the particle size of about 5mm, uniformly mixing the crushed waste residue with NaOH according to the mass ratio of 50:2 to obtain a mixed material, adding water into the mixed material, keeping the mixed material moist at 26 ℃ for 20 days after uniformly mixing, wherein the material-liquid ratio of the mixed material to the added water is 1:4g/m L;
s2: mixing sodium oxalate, sodium sulfate, potassium chloride and sodium dodecyl sulfate according to the mass ratio of 8:3:5:3 to obtain a gypsum activity excitant; adding the gypsum activity excitant into the inerted mixed material, wherein the mass ratio of the added gypsum activity excitant to the inerted mixed material is 1:10, uniformly mixing, exciting for 10 days at 24 ℃, and then grinding into powder to obtain low-grade gypsum powder, wherein CaSO in the low-grade gypsum powder4·2H2The content of O is 62.1 percent, and the low-grade gypsum powder is the cement retarder.
Example 2
A cement retarder prepared from nickel gypsum waste residues is prepared by the following steps:
s1, crushing the nickel gypsum waste residue into particles with the particle size of about 5mm, uniformly mixing the crushed waste residue with NaOH according to the mass ratio of 50:1 to obtain a mixed material, adding water into the mixed material, keeping the mixed material wet at 30 ℃ for 18 days after uniformly mixing, wherein the material-liquid ratio of the mixed material to the added water is 1:3g/m L;
s2: mixing sodium oxalate, sodium sulfate, potassium chloride and sodium dodecyl sulfate according to the mass ratio of 10:2:6:2 to obtain a gypsum activity excitant; adding the gypsum activity excitant into the inerted mixed material, wherein the mass ratio of the added gypsum activity excitant to the inerted mixed material is 1:20, uniformly mixing, exciting for 8 days at 25 ℃, and grinding into powder to obtain low-grade gypsum powder, wherein the low-grade gypsum powder is the cement retarder.
Example 3
A cement retarder prepared from nickel gypsum waste residues is prepared by the following steps:
s1: pulverizing waste residue into particles with particle diameter of about 5mm, mixing with Ca (OH)2Uniformly mixing the materials according to the mass ratio of 50:3 to obtain a mixed material, adding water into the mixed material, wherein the material-liquid ratio of the mixed material to the added water is 1:5g/m L, uniformly mixing, and then preserving moisture at 24 ℃ for 25 days;
s2: mixing sodium oxalate, sodium sulfate, potassium chloride and sodium dodecyl sulfate according to the mass ratio of 5:4:3:4 to obtain a gypsum activity excitant; adding the gypsum activity excitant into the inerted mixed material, wherein the mass ratio of the added gypsum activity excitant to the inerted mixed material is 3:20, uniformly mixing, exciting for 12 days at 20 ℃, and grinding into powder to obtain low-grade gypsum powder, wherein the low-grade gypsum powder is the cement retarder.
Comparative example 1
A cement retarder prepared from nickel gypsum waste residues is prepared by the following steps:
s1: crushing the waste residue into particles with the particle size of about 5 mm;
s2: mixing sodium oxalate, sodium sulfate, potassium chloride and sodium dodecyl sulfate according to the mass ratio of 8:3:5:3 to obtain a gypsum activity excitant; the gypsum activity excitant is added into the particles, the mass ratio of the added gypsum activity excitant to the particles is 1:10, the mixture is evenly mixed and excited for 10 days at 24 ℃, and then the mixture is ground into powder, so that low-grade gypsum powder is obtained and used as a cement retarder for standby.
Comparative example 2
A cement retarder prepared from nickel gypsum waste residues is prepared by the following steps:
s1, crushing the waste residues into particles with the particle size of about 5mm, uniformly mixing the crushed waste residues with NaOH according to the mass ratio of 50:2 to obtain a mixed material, adding water into the mixed material, keeping the mixed material moist at 26 ℃ for 20 days after uniformly mixing, wherein the material-liquid ratio of the mixed material to the added water is 1:4g/m L;
s2: grinding the inerted particles into powder to obtain low-waste-residue powder which is used as a cement retarder for later use.
Analysis of results
The performance of the cement retarders prepared in the above experimental examples is inspected and compared with that of a normal dihydrate gypsum retarder, the cement retarders prepared in the above experimental examples are prepared by using the same cement clinker as a raw material and adding a mixed material with the same components and composition by a national standard method, and a cement sample is prepared and subjected to standardized detection, and the results are listed in table 2.
Table 2 comparative cement test data for each group
As can be seen from Table 2, the cement prepared by the process of the present invention has comparable effects with the existing dihydrate gypsum coagulant sold in the market, and all indexes meet the national standard, i.e., the waste residues generated by industrial and mining enterprises can be recycled by the process of the present invention.
Comparative example 1 compared to example 1, the inerting was not carried out, and the subsequent chemical reaction of silica and the remaining impurities during the cement application could not be prevented, adversely affecting the setting time and strength. Comparative example 2 compared to example 1, the absence of calcium sulfate activation affects the crystal morphology during subsequent use of the cement, as well as adversely affecting setting time and strength.
In addition, the cement retarder prepared by the invention is detected for the content of soluble heavy metals, and the results are listed in table 3.
TABLE 3 soluble heavy metals test results (mg/kg)
Note: no description is found: the content of soluble lead (Pb) is less than 5 mg/kg; the content of soluble chromium (Cr) is less than 5 mg/kg; the content of soluble cadmium (Cd) is less than 2 mg/kg; soluble mercury (Hg) content less than 0.5mg/kg
As can be seen from table 3, the cement retarder prepared by the method of the present invention has a heavy metal content below the national standard, can be directly added into cement for use, does not cause secondary environmental pollution, and is environment-friendly.
While the present invention has been described in detail with reference to the embodiments, it should not be construed as limited to the scope of the patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (9)
1. A method for preparing a cement retarder by using nickel gypsum waste residues is characterized by comprising the following steps:
s1: 60 to 65 weight percent of CaSO4·2H2O and 15-18 wt% of active SiO2The nickel gypsum waste residue is crushed and then mixed with an inerting agent to obtain a mixed material; then adding water, mixing uniformly, and preserving moisture and inerting for 18-25 days at 10-40 ℃;
s2: and adding a gypsum activity excitant into the inerted mixture, uniformly mixing, and exciting for 8-12 days at 20-25 ℃ to obtain the cement retarder.
2. The method of claim 1, wherein: the mass ratio of the waste residue to the inerting agent in the mixed material is 50: 1-3.
3. The method according to claim 1 or 2, characterized in that: the inerting agent is capable of inerting the active SiO2To render it inactive.
4. The method of claim 3, wherein: the inerting agent is sodium hydroxide or calcium hydroxide.
5. The method according to claim 1, wherein the mixture obtained in S1 is mixed with water at a ratio of 1: 3-5 g/m L, and the inerting temperature is 24-30 ℃ and the inerting time is 20 days.
6. The method of claim 1, wherein: the mass ratio of the gypsum activity excitant added in the S2 to the inerted mixed material is 1-3: 20.
7. The method according to claim 1 or 6, wherein the gypsum activity excitant comprises the following components in parts by mass:
5-10 parts of sodium oxalate, 2-4 parts of sodium sulfate, 3-6 parts of potassium chloride and 2-4 parts of sodium dodecyl sulfate.
8. The method according to claim 7, wherein the gypsum activity excitant comprises the following components in parts by mass:
8 parts of sodium oxalate, 3 parts of sodium sulfate, 5 parts of potassium chloride and 3 parts of sodium dodecyl sulfate.
9. The cement retarder prepared by the method for preparing the cement retarder from the nickel gypsum waste residue according to any one of claims 1 to 8.
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