CN114890699B - Cementing material prepared from fluorogypsum and preparation method thereof - Google Patents
Cementing material prepared from fluorogypsum 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
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
- C04B11/266—Chemical 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
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/028—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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Abstract
The invention relates to a cementing material prepared from fluorogypsum and a preparation method thereof, belonging to the technical field of comprehensive utilization of solid wastes. The preparation method of the fluorine gypsum-made cementing material comprises the following steps: a. heating the fluorogypsum to 120-600 ℃ and preheating for 10-25S; b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃; c. and (3) cooling the fluorine gypsum subjected to boiling calcination in the step (b) to 60-100 ℃, mixing with an exciting agent, and grinding to obtain the fluorine gypsum cementing material. The method of the invention prepares the high-quality cementing material by taking the fluorogypsum as the raw material, so that the fluorogypsum is recycled and harmless, and the method is an important way for promoting the comprehensive utilization of industrial solid waste by the fluoride industry, preventing and controlling pollution, protecting the environment and improving the economic benefit.
Description
Technical Field
The invention relates to a cementing material prepared from fluorogypsum and a preparation method thereof, belonging to the technical field of comprehensive utilization of solid wastes.
Background
The fluorogypsum is waste residue generated when fluorite and sulfuric acid are used for preparing hydrofluoric acid. The fluorogypsum is also called as fluorite, white powder, except that part of the fluorogypsum is used as a cement retarder of a cement plant, other market applications are few, and the fluorogypsum is mainly piled up.
The current method for producing hydrogen fluoride mainly uses sulfuric acid to acidolysis fluorite, and can theoretically produce 1t hydrogen fluoride and by-produce 3.4t fluorite, and the emission of fluorite is huge every year. Because the fluorine gypsum contains a small amount of residual sulfuric acid and hydrofluoric acid, the emission is large, and especially the fluorine ions are easy to enter the water body and cause serious environmental pollution. Along with the continuous increase of the emission of the fluorine gypsum, the problems of more impurities, complex components, extremely slow hydration of the main components of the anhydrous gypsum and the like in the fluorine gypsum are added, so that the anhydrous gypsum seriously affects the environment, the utilization difficulty is high, and only the traditional fields of cement retarder and the like are partially studied at present. The pressure for comprehensive utilization of resources is increased. Along with the vigorous development of fluorine chemical industry, a large amount of fluorine gypsum is inevitably generated. How to effectively utilize the industrial waste residue, change waste into valuable and protect the environment is an urgent work. The industrial waste residue is utilized in situ, the recycling of the waste residue is realized, and the method is an advantageous means for saving the cost and improving the economic benefit for enterprises.
In addition to sulfuric acid and hydrofluoric acid, the main component of the fluorogypsum (piled or fresh) is type II anhydrous gypsum, which is insoluble or insoluble, and has potential hydration activity, but the fluorogypsum has slow hydration rate, so that development and utilization are "bottlenecks". The hydrated fluorine gypsum is accelerated to have certain strength by adding the exciting agent, but the due gelatinization performance of the gypsum is not exerted.
CN103130484a discloses a fluorogypsum binding gypsum powder, which comprises the following raw materials in parts by weight: anhydrous fluorine gypsum powder: 68-70 parts of P (phosphogypsum powder): 12-18 parts of neutralizer: 1-6 parts of cement: 7-10 parts of fly ash: 3-10 parts of retarder: 0.05-0.5 part of water-retaining agent: 0.01-0.5 part of adhesive: 0.1-0.5 part, the advantages of the invention are as follows: the fluorine gypsum bonding gypsum powder has the advantages of simple manufacturing process, short period, no toxicity, no smell, environmental protection, no cracking, good fire resistance, high bonding strength, convenient construction and low manufacturing cost, and is suitable for substrates of various different materials. However, the strength is low, the product performance is sensitive to fluorogypsum impurities, and the product performance is unstable.
Disclosure of Invention
It is a first object of the present invention to provide a novel fluorogypsum-made cementitious material.
In order to achieve the first object of the present invention, the preparation method of the fluorogypsum-made cementing material comprises the following steps:
a. heating the fluorogypsum to 120-600 ℃ and preheating for 10-25S;
b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃;
c. and (3) cooling the fluorine gypsum subjected to boiling calcination in the step (b) to 60-100 ℃, mixing with an exciting agent, and grinding to obtain the fluorine gypsum cementing material.
In a specific embodiment, the preheating in step a is a secondary preheating, the primary preheating material is from 120 ℃ to 350 ℃, and the secondary preheating material is from 350 ℃ to 550 ℃.
In a specific embodiment, the particle size range of the fluorogypsum in step a is less than 1mm, preferably less than 0.6 mm.
In a specific embodiment, the fluorogypsum in step a is anhydrous fluorogypsum; the preparation method of the anhydrous fluorine gypsum preferably comprises the following steps: drying the fluorine gypsum containing water at 350-550 ℃; the drying time is preferably 3-5 seconds;
preferably, the temperature of the anhydrous fluorine gypsum before preheating is below 120 ℃.
In one embodiment, the boiling calcination in step b is performed for a period of 10 to 20 seconds.
In a specific embodiment, the cooling in the step c is to cool to below 200 ℃ firstly and then cool to below 100 ℃ by air;
the rotational speed of the grinding powder is 20-30 rpm.
In a specific embodiment, the weight ratio of the calcined fluorogypsum to the exciting agent in the step c is as follows: 94-99:6-1; the exciting agent is preferably a sulfate exciting agent, more preferably a mixture of a component A and a component B, wherein the component A is at least one of potassium sulfate, sodium sulfate and sulfoaluminate cement, the component B is at least one of methylcellulose, fly ash, carboxymethyl cellulose or dextrin water-retaining agent, and the mass ratio of the component A to the component B is 1-3: 2 to 6.
The second aim of the invention is to provide a preparation method of the fluorine gypsum-made cementing material.
In order to achieve the second object of the present invention, the preparation method of the fluorogypsum-made cementing material comprises the following steps:
a. heating the fluorogypsum to 120-600 ℃ and preheating for 10-25S;
b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃, wherein the boiling and calcining time is preferably 10-20 seconds;
c. and (3) cooling the fluorine gypsum subjected to boiling calcination in the step (b) to 60-100 ℃, mixing with an exciting agent, and grinding to obtain the fluorine gypsum cementing material.
In a specific embodiment, the preheating in the step a is a secondary preheating, wherein the first-stage preheating material is from 120 ℃ to 350 ℃, and the second-stage preheating material is from 350 ℃ to 550 ℃;
the particle size range of the fluorine gypsum in the step a is less than 1mm, preferably less than 0.6 mm;
a, the fluorine gypsum in the step a is anhydrous fluorine gypsum; the preparation method of the anhydrous fluorine gypsum preferably comprises the following steps: drying the fluorine gypsum containing water at 350-550 ℃; the drying time is preferably 3-5 seconds;
preferably, the temperature of the anhydrous fluorine gypsum before preheating is below 120 ℃;
c, cooling to 200 ℃ or lower, and then air-cooling to 100 ℃ or lower;
the rotational speed of the grinding powder is 20-30 rpm.
In a specific embodiment, the weight ratio of the calcined fluorogypsum to the exciting agent in the step c is as follows: 94-99:6-1; the exciting agent is preferably a sulfate exciting agent, more preferably a mixture of a component A and a component B, wherein the component A is at least one of potassium sulfate, sodium sulfate and sulfoaluminate cement, the component B is at least one of methylcellulose, fly ash, carboxymethyl cellulose or dextrin water-retaining agent, and the mass ratio of the component A to the component B is 1-3: 2 to 6.
The beneficial effects are that:
1. the method takes the fluorogypsum as the raw material to prepare the high-quality cementing material, wherein the initial setting time is more than or equal to 1.5 hours, and the average time is 3.0 hours; the final setting time is less than or equal to 8 hours, the average compressive strength of the 28d strength is 5.3 hours, the average compressive strength of the 28d strength is 38.5Mpa (the compressive strength of the 28d strength is more than or equal to 30 Mpa), and the softening coefficient is 0.65-0.85, thus being an ideal cementing material. (note: initial and final setting time can be adjusted according to the exciter)
2. The method for producing the high-quality gypsum cementing material by using the fluorine gypsum makes the fluorine gypsum recycled and harmless, and is an important way for fluoride industry to promote the comprehensive utilization of industrial solid wastes, prevent and treat pollution, protect the environment and improve the economic benefit.
3. The method is simple, the calcination intensity in a short time is greatly improved, and the solid waste of the fluorine gypsum can be treated in a large scale to prepare the gypsum cementing material; and the method can also realize large-scale continuous online production, has high efficiency and is beneficial to industrialized popularization and application.
Detailed Description
In order to achieve the first object of the present invention, the preparation method of the fluorogypsum-made cementing material comprises the following steps:
a. heating the fluorogypsum to 120-600 ℃ and preheating for 10-25S;
b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃;
c. and (3) cooling the fluorine gypsum subjected to boiling calcination in the step (b) to 60-100 ℃, mixing with an exciting agent, and grinding to obtain the fluorine gypsum cementing material.
In a specific embodiment, the preheating in step a is a secondary preheating, the primary preheating material is from 120 ℃ to 350 ℃, and the secondary preheating material is from 350 ℃ to 550 ℃.
In a specific embodiment, the particle size range of the fluorogypsum in step a is less than 1mm, preferably less than 0.6 mm.
In a specific embodiment, the fluorogypsum in step a is anhydrous fluorogypsum; the preparation method of the anhydrous fluorine gypsum preferably comprises the following steps: drying the fluorine gypsum containing water at 350-550 ℃; the drying time is preferably 3-5 seconds;
preferably, the temperature of the anhydrous fluorine gypsum before preheating is below 120 ℃.
In one embodiment, the boiling calcination in step b is performed for a period of 10 to 20 seconds.
In a specific embodiment, the cooling in the step c is to cool to below 200 ℃ firstly and then cool to below 100 ℃ by air;
the rotational speed of the grinding powder is 20-30 rpm.
In a specific embodiment, the weight ratio of the calcined fluorogypsum to the exciting agent in the step c is as follows: 94-99:6-1; the exciting agent is preferably a sulfate exciting agent, more preferably a mixture of a component A and a component B, wherein the component A is at least one of potassium sulfate, sodium sulfate and sulfoaluminate cement, the component B is at least one of methylcellulose, fly ash, carboxymethyl cellulose or dextrin water-retaining agent, and the mass ratio of the component A to the component B is 1-3: 2 to 6.
The second object of the invention is to provide a preparation method of the fluorine gypsum-made cementing material.
In order to achieve the second object of the present invention, the preparation method of the fluorogypsum-made cementing material comprises the following steps:
a. heating the fluorogypsum to 120-600 ℃ and preheating for 10-25S;
b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃, wherein the boiling and calcining time is preferably 10-20 seconds;
c. and (3) cooling the fluorine gypsum subjected to boiling calcination in the step (b) to 60-100 ℃, mixing with an exciting agent, and grinding to obtain the fluorine gypsum cementing material.
In a specific embodiment, the preheating in the step a is a secondary preheating, wherein the first-stage preheating material is from 120 ℃ to 350 ℃, and the second-stage preheating material is from 350 ℃ to 550 ℃;
the particle size range of the fluorine gypsum in the step a is less than 1mm, preferably less than 0.6 mm;
a, the fluorine gypsum in the step a is anhydrous fluorine gypsum; the preparation method of the anhydrous fluorine gypsum preferably comprises the following steps: drying the fluorine gypsum containing water at 350-550 ℃; the drying time is preferably 3-5 seconds;
preferably, the temperature of the anhydrous fluorine gypsum before preheating is below 120 ℃;
c, cooling to 200 ℃ or lower, and then air-cooling to 100 ℃ or lower;
the rotational speed of the grinding powder is 20-30 rpm.
In a specific embodiment, the weight ratio of the calcined fluorogypsum to the exciting agent in the step c is as follows: 94-99:6-1; the exciting agent is preferably a sulfate exciting agent, more preferably a mixture of a component A and a component B, wherein the component A is at least one of potassium sulfate, sodium sulfate and sulfoaluminate cement, the component B is at least one of methylcellulose, fly ash, carboxymethyl cellulose or dextrin water-retaining agent, and the mass ratio of the component A to the component B is 1-3: 2 to 6.
The following describes the invention in more detail with reference to examples, which are not intended to limit the invention thereto.
Example 1
(1) The fluorine gypsum which is taken from Fujian and piled up for 6 months and contains 3% of free water is dried for 4 seconds at 450 ℃ after being metered, the fluorine gypsum is crushed while being dried, and a coarse particle sedimentation device is arranged at a crushing outlet after crushing, so that the particle size of the fluorine gypsum particles at the outlet is ensured to meet the requirement below 1 mm.
(2) The temperature of the crushed fluorogypsum with the particle size meeting the requirement is about 120 ℃, the dried fluorogypsum is preheated for 15S from 120 ℃ to 550 ℃, the first-stage preheating material is preheated from 120 ℃ to 350 ℃ through the second-stage preheating, and the second-stage preheating material is preheated from 350 ℃ to 550 ℃.
(3) The preheated material enters a calciner to be calcined at 800 ℃ for 12 seconds. Cooling to 180 deg.c, further air cooling to 80 deg.c, mixing with potassium sulfate activator in the rotation speed of 22 rpm, and storing.
Example 2
(1) Fresh fluorogypsum taken from an inner Mongolia production line is metered and then dried at 480 ℃ for 3.5 seconds, the fluorogypsum is crushed while being dried, and a coarse particle sedimentation device is arranged at a crushing outlet after crushing, so that the particle size of the fluorogypsum particles at the outlet is ensured to meet the requirement below 1 mm.
(2) The temperature of the crushed fluorogypsum with the particle size meeting the requirement is about 120 ℃, the dried fluorogypsum is heated to 120-550 ℃ and preheated for 16S, the first-stage preheated material is from 120-350 ℃ and the second-stage preheated material is from 350-550 ℃ through the second-stage preheating.
(3) The preheated material enters a calciner to be calcined at 850 ℃ for 12 seconds. Cooling to 180 deg.c, further air cooling to 80 deg.c, mixing with potassium sulfate activator in the rotation speed of 22 rpm, and storing.
Comparative example 1
Otherwise in accordance with example 1, except for example 1, the stacked fluorogypsum was directly dried, crushed, preheated and then calcined at a temperature of 650 ℃. Cooling to 180 deg.c, further air cooling to 80 deg.c, mixing with potassium sulfate activator in the ratio of 97 to 3, and grinding at speed of 22 rpm.
Table 1 results of the tests of examples 1 and 2, comparative example 1
Project | Initial setting time | Final setting time | 28d Strength compression Strength | Softening coefficient |
Example 1 | 3.8 | 5.7 | 41.0 | 0.80 |
Example 2 | 3.2 | 4.6 | 42.5 | 0.81 |
Comparative example 1 | 1.4 | 2.2 | 35.1 | 0.61 |
The gypsum cementing material is produced by detecting the fluorine gypsum through multiple experiments, wherein the initial setting time (more than or equal to 1.5 h) is 3.0h on average, the final setting time (less than or equal to 8 h) is 5.3h on average, the 28d strength compressive strength is 38.5MPa on average, and the softening coefficient is 0.65-0.85, thus being an ideal cementing material.
Claims (11)
1. The preparation method of the fluorine gypsum cementing material is characterized by comprising the following steps:
a. heating the fluorogypsum to 120-600 ℃ for preheating for 10-25 s, wherein the preheating in the step a is secondary preheating, the first-stage preheating material is from 120 ℃ to 350 ℃, the second-stage preheating material is from 350 ℃ to 550 ℃, and the fluorogypsum in the step a is anhydrous fluorogypsum;
b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃, wherein the boiling and calcining time is 10-20 seconds;
c. cooling the fluorogypsum subjected to boiling calcination in the step b to 60-100 ℃, mixing with an exciting agent, and grinding to obtain a fluorogypsum cementing material; and c, the weight ratio of the calcined fluorogypsum to the exciting agent is as follows: 94-99:6-1; the exciting agent is a mixture of a component A and a component B, wherein the component A is at least one of potassium sulfate, sodium sulfate and sulfoaluminate cement, the component B is at least one of methylcellulose, fly ash, carboxymethyl cellulose or dextrin water-retaining agent, and the mass ratio of the component A to the component B is 1-3: 2 to 6.
2. The fluorogypsum-made cement according to claim 1, wherein the particle size range of the fluorogypsum in the step a is 1mm or less.
3. The fluorogypsum-made cement according to claim 1, wherein the particle size range of the fluorogypsum in the step a is 0.6mm or less.
4. The fluorogypsum-made cement according to claim 1 or 2, wherein the preparation method of the anhydrous fluorogypsum comprises: and drying the fluorine gypsum containing water at 350-550 ℃.
5. The fluorogypsum-made cement according to claim 4, wherein the preparation method of the anhydrous fluorogypsum comprises: the drying time is 3-5 seconds.
6. The fluorogypsum-made binder according to claim 1 or 2, wherein the temperature of the anhydrous fluorogypsum before preheating is 120 ℃ or lower.
7. The fluorogypsum-made binder of claim 1 or 2, wherein the cooling in step c is to cool to below 200 ℃ and then to below 100 ℃;
the rotational speed of the grinding powder is 20-30 rpm.
8. The method for preparing a fluorogypsum-made binder according to any one of claims 1 to 7, comprising the steps of:
a. heating the fluorogypsum to 120-600 ℃ and preheating for 10-25S; the preheating in the step a is secondary preheating, wherein the temperature of the first-stage preheating material is 120-350 ℃, and the temperature of the second-stage preheating material is 350-550 ℃; a, the fluorine gypsum in the step a is anhydrous fluorine gypsum;
b. b, boiling and calcining the fluorine gypsum preheated in the step a at 700-900 ℃, wherein the boiling and calcining time is 10-20 seconds;
c. cooling the fluorogypsum subjected to boiling calcination in the step b to 60-100 ℃, mixing with an exciting agent, and grinding to obtain a fluorogypsum cementing material; and c, the weight ratio of the calcined fluorogypsum to the exciting agent is as follows: 94-99:6-1; the exciting agent is a mixture of a component A and a component B, wherein the component A is at least one of potassium sulfate, sodium sulfate and sulfoaluminate cement, the component B is at least one of methylcellulose, fly ash, carboxymethyl cellulose or dextrin water-retaining agent, and the mass ratio of the component A to the component B is 1-3: 2 to 6.
9. The method for preparing the fluorogypsum-made cementing material of claim 8, wherein,
the granularity range of the fluorine gypsum in the step a is below 1 mm; c, cooling to below 200 ℃ firstly, and then cooling to below 100 ℃ by air cooling;
the rotational speed of the grinding powder is 20-30 rpm.
10. The method for preparing the fluorogypsum-made cementing material of claim 8, wherein,
the preparation method of the anhydrous fluorine gypsum comprises the following steps: drying the fluorine gypsum containing water at 350-550 ℃; the drying time is 3-5 seconds.
11. The method for producing a fluorine gypsum-based binder according to claim 8, wherein the temperature before preheating the anhydrous fluorine gypsum is 120 ℃ or lower.
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