CN111792862A - Method for improving phosphogypsum gelling activity - Google Patents

Method for improving phosphogypsum gelling activity Download PDF

Info

Publication number
CN111792862A
CN111792862A CN202010663619.6A CN202010663619A CN111792862A CN 111792862 A CN111792862 A CN 111792862A CN 202010663619 A CN202010663619 A CN 202010663619A CN 111792862 A CN111792862 A CN 111792862A
Authority
CN
China
Prior art keywords
phosphogypsum
wet
gelling activity
medicament
aqueous solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010663619.6A
Other languages
Chinese (zh)
Inventor
王家伟
王海峰
陈雁冰
龙召凤
李仕玉
曾庆果
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guizhou University
Original Assignee
Guizhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guizhou University filed Critical Guizhou University
Priority to CN202010663619.6A priority Critical patent/CN111792862A/en
Publication of CN111792862A publication Critical patent/CN111792862A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B11/00Calcium sulfate cements
    • C04B11/26Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B11/00Calcium sulfate cements
    • C04B11/005Preparing or treating the raw materials

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a method for improving the gelling activity of phosphogypsum. The method comprises the following steps: (1) aging phosphogypsum by water to obtain aged phosphogypsum; (2) wet grinding the aged phosphogypsum to obtain the wet-ground phosphogypsum; (3) roasting and cooling the wet-milled phosphogypsum to obtain roasted phosphogypsum; (4) and (3) respectively carrying out two-stage heap leaching on the calcined phosphogypsum by using a medicament 1 and a medicament 2 to obtain the phosphogypsum with improved gelling activity. The invention has simple process and lower cost, can greatly improve the gelling activity of the phosphogypsum, and the building material prepared from the treated phosphogypsum has high strength and strong water-soaking resistance, and the doping amount can be more than 70 percent, thereby providing a way for the mass use and the comprehensive utilization of the phosphogypsum.

Description

Method for improving phosphogypsum gelling activity
Technical Field
The invention relates to the field of chemical industry, in particular to a method for improving the gelling activity of phosphogypsum.
Background
China is the country with the most population in the world and is also a large country for agricultural production, the phenomenon of 'phosphorus and potassium deficiency' generally exists in agricultural cultivated land, a large amount of phosphorus chemical fertilizer is needed for agricultural production, the demand of phosphate fertilizer is increased year by year along with the rapid development of agricultural production in China, and a large amount of phosphoric acid is needed for phosphate fertilizer production. The main production method of the existing phosphoric acid is a wet-process phosphoric acid production technology, a large amount of phosphogypsum is generated in the production process, obviously along with the rapid development of the phosphorus chemical industry, the emission of the phosphogypsum discharged by the wet-process phosphoric acid industry is increased year by year, the emission of the phosphogypsum discharged by the world is about 3 hundred million tons per year, the annual emission of the phosphogypsum discharged by China is about 7000 million tons, the total amount of the phosphogypsum which is stockpiled currently exceeds 5 million tons, the yield of the phosphate fertilizer in Guizhou province accounts for about 16 percent of the whole country, the emission of the phosphogypsum is about 1000 million tons. Because the water-soluble phosphorus-fluorine-free acid composite material contains harmful substances such as water-soluble phosphorus, water-soluble fluorine, free acid and the like, a great deal of utilization technology is not well dealt with so far, so that the resource utilization rate is low and is only about 10%.
At present, researchers at home and abroad carry out a great deal of research on the comprehensive utilization of the phosphogypsum. There are several main aspects: 1. the phosphogypsum is used for preparing building materials such as various bricks, building blocks and the like, but the doping amount is not large and is generally less than 30 percent; 2. the phosphogypsum is applied to the traffic field, but the doping amount is only 2.8 percent; 3. the technical process for preparing sulfuric acid and co-producing cement by using phosphogypsum has the advantages of long process, more equipment, high energy consumption, large investment and large technical difficulty; 3. the ardealite is used for producing the gypsum plaster boards, the technology needs to calcine gypsum, the estimated ardealite consumption of the current technology industrialization does not exceed 1000 ten thousand tons, and compared with the annual 7000 ten thousand ton increment in China, a larger gap exists.
Therefore, improvements and innovations are still needed to increase the usage amount or the incorporation amount of the phosphogypsum in various fields.
Disclosure of Invention
The invention aims to provide a method for improving the gelling activity of phosphogypsum. The invention has simple process and lower cost, can greatly improve the gelling activity of the phosphogypsum, and the building material prepared from the treated phosphogypsum has high strength and strong water-soaking resistance, and the doping amount is more than 70 percent, thereby providing a new way for the comprehensive utilization of the phosphogypsum.
The technical scheme of the invention is as follows: a method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) aging phosphogypsum by water to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum to obtain the wet-ground phosphogypsum;
(3) roasting and cooling the wet-milled phosphogypsum to obtain roasted phosphogypsum;
(4) and (3) respectively carrying out two-stage heap leaching on the calcined phosphogypsum by using a medicament 1 and a medicament 2 to obtain the phosphogypsum with improved gelling activity.
In the method for improving the gelling activity of the phosphogypsum, in the step (1), the phosphogypsum is aged for 24-48h by using tap water, and the water content is 30-50% during aging, so that the aged phosphogypsum is obtained.
In the method for improving the gelling activity of the phosphogypsum, in the step (2), the phosphogypsum after aging is subjected to wet grinding for 20-50min to obtain the phosphogypsum after wet grinding.
In the method for improving the gelling activity of the phosphogypsum, the step (3) is to roast the phosphogypsum after wet grinding to 400-600 ℃, preserve heat for 2-5h and then naturally cool to obtain the roasted phosphogypsum.
In the method for improving the gelling activity of the phosphogypsum, the medicament 1 is an aqueous solution prepared from one or more of potassium oxide, sodium carbonate, calcium oxide and magnesium carbonate.
In the method for improving the gelling activity of the phosphogypsum, the medicament 1 is an aqueous solution prepared from one or more of potassium oxide, sodium carbonate, calcium oxide and magnesium carbonate; in the prepared aqueous solution, the total mass fraction of potassium oxide, sodium carbonate, calcium oxide and magnesium carbonate is 3-6%.
In the method for improving the gelling activity of the phosphogypsum, the dosage of the medicament 1 is 200-500ml of the medicament 1 per 100g of calcined phosphogypsum.
In the method for improving the gelling activity of the phosphogypsum, the medicament 2 is an aqueous solution prepared from one or more of sodium sulfate, potassium sulfate and sulfuric acid; in the prepared water solution, the mass fraction of sulfate radicals is 3-5%.
In the method for improving the gelling activity of the phosphogypsum, the dosage of the reagent 2 is 300-500ml of the reagent 2 per 100g of calcined phosphogypsum.
In the method for improving the gelling activity of the phosphogypsum, in the step (4), the reagent 1 pair of heap leaching is firstly applied to the calcined phosphogypsum for 5-10h, then the reagent 2 is applied for 7-14h, and the heap leaching temperature is 25-50 ℃. Heap leaching is carried out in a heap leaching field, the temperature of the heap leaching long field is controlled, and a greenhouse or a plastic film is laid for heat preservation when necessary.
Compared with the prior art, the invention has the following beneficial effects:
1. the method of the invention treats the phosphogypsum through the steps of aging, wet grinding, low-temperature roasting and two-stage heap leaching, and has simple process and lower cost. In the process, the controlled aging is carried out for 24-48h during aging, the water content is 30-50%, and the complete infiltration of the phosphogypsum can be ensured; after wet grinding and aging, the phosphogypsum can be properly reduced in granularity by 20-50 min; roasting the wet-milled phosphogypsum to 400-.
2. The invention adopts the reagent 1 (aqueous solution prepared by one or more of potassium oxide, sodium carbonate, calcium oxide and magnesium carbonate) and the reagent 2 (aqueous solution prepared by one or more of sodium sulfate, potassium sulfate and sulfuric acid) to carry out heap leaching twice on the aged, wet-milled and roasted phosphogypsum, has simple technical process and is easy to realize automation. The heap leaching of the agent 1 pre-excites the calcined phosphogypsum, the heap leaching of the agent 2 pre-excites the pre-excited phosphogypsum, and the activated phosphogypsum has the advantages of rearrangement of calcium sulfate crystal lattices, increase of crystal lattice defects and increase of specific surface area, thereby improving the gelling activity of the phosphogypsum.
3. The invention specifies heap leaching conditions of the medicament 1 and the medicament 2, wherein the medicament 1 is applied for heap leaching for 5-10h, and then the medicament 2 is applied for heap leaching for 7-14h, and the heap leaching temperature is 25-50 ℃. If the heap leaching time is less than the specified time, the phosphogypsum cannot meet the requirement; if the heap leaching time exceeds the specified time, the problems of overlong heap leaching time and low efficiency can occur; the heap leaching temperature is lower in the specified range, the energy consumption is low, and the automation is easier to realize in the production.
4. After the treated phosphogypsum is prepared into a non-fired building material according to the mixing amount of 75 percent, the compressive strength can reach 18MPa after 28 days, and the compressive strength can reach 11MPa after soaking in water for 24 hours.
In summary, the following steps: the invention has simple process and lower cost, can greatly improve the gelling activity of the phosphogypsum, and the building material prepared from the treated phosphogypsum has high strength and strong water-soaking resistance, and the doping amount can be more than 70 percent, thereby providing a way for the mass use and the comprehensive utilization of the phosphogypsum.
In order to verify the feasibility and the beneficial effects of the invention, the inventor carries out a large number of tests, and partial tests are as follows:
experiment I, the inventor respectively carries out XRD pattern tests on the phosphogypsum and the phosphogypsum treated in the examples 1 to 4, and the results are shown in figures 1 to 5.
As can be seen from FIGS. 1-5, the peaks of secondary and tertiary intensities of calcium sulfate in phosphogypsum after treatment in example 1 are obviously reduced; in example 2, the first and third intensity peaks of calcium sulfate in phosphogypsum after treatment are obviously reduced; example 3 the second and third intensity peaks of calcium sulfate in phosphogypsum after treatment are obviously reduced; the second and third intensity peaks of calcium sulfate in phosphogypsum after the treatment of example 2 are obviously reduced.
In the second test, the inventor carries out the test on the phosphogypsum and the phosphogypsum treated in the examples 1 to 4 according to the doping amount of 75 percent, adds 25 percent of cement to prepare the baking-free building material according to the traditional baking-free building material process, and carries out the test on the compressive strength of the prepared baking-free building material for 28 days and the test on the strength of the baking-free building material after soaking for 24 hours respectively, and the test results are shown in table 1.
TABLE 1-28 day compressive strength test and 24h soaking test results table
Item 28 day compressive strength/MPa The compressive strength/MPa is obtained after soaking for 24 hours
Untreated phosphogypsum 6 3
Example 1 14 8
Example 2 18.22 11.5
Example 3 18.55 10.6
Example 4 13.65 8.7
As can be seen from Table 1, the compressive strength of the baking-free building material prepared from the treated phosphogypsum can reach 18MPa after 28 days, and is still more than 11MPa after soaking in water for 24 hours.
Drawings
Figure 1 is an XRD pattern of phosphogypsum;
figure 2 is the XRD pattern of phosphogypsum after treatment of example 1;
figure 3 is the XRD pattern of phosphogypsum after treatment of example 2;
figure 4 is the XRD pattern of phosphogypsum after treatment of example 3;
figure 5 is the XRD pattern of phosphogypsum after treatment of example 4.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Example 1. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 24 hours by using tap water, wherein the water content is controlled to be 35% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 30min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-milled phosphogypsum to 400 ℃, preserving heat for 3 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 5h, and then adding a reagent 2 for heap leaching for 10h, wherein the heap leaching temperature is 25-30 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the dosage of 100g of calcined phosphogypsum is 240ml, the mass fraction of potassium oxide in the aqueous solution is 0.5 percent, the mass fraction of sodium carbonate is 0.02 percent, the mass fraction of calcium oxide is 0.05 percent, and the mass fraction of magnesium carbonate is 2 percent; wherein the agent 2 is aqueous solution, the usage amount of 100g of calcined phosphogypsum is 340ml, and the mass ratio of sodium sulfate to sulfuric acid in the agent 2 is 1: and 9, the mass fraction of the total sulfate radicals in the aqueous solution is 3.5%.
Example 2. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, aging phosphogypsum taken back from a storage yard for 30 hours by using tap water, wherein the water content is controlled to be 35% during aging, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 40min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-ground phosphogypsum to 600 ℃, preserving the heat for 5 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 8h, and then adding a reagent 2 for heap leaching for 12h, wherein the heap leaching temperature is 25-30 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, 100g of calcined phosphogypsum is used in an amount of 280ml, the mass fraction of potassium oxide in the aqueous solution is 0.02%, the mass fraction of sodium carbonate is 0.02%, the mass fraction of calcium oxide is 0.1%, and the mass fraction of magnesium carbonate is 0.5%; the reagent 2 is an aqueous solution, the dosage of 100g of calcined phosphogypsum is 400ml, and the mass ratio of potassium sulfate to sulfuric acid in the reagent 2 is 1: 15, the mass fraction of total sulfate in the aqueous solution was 4.7%.
Example 3. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 24 hours by using tap water, wherein the water content is controlled to be 50% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 40min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-milled phosphogypsum to 500 ℃, preserving the heat for 4 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 7 hours, and then adding a reagent 2 for heap leaching for 14 hours, wherein the heap leaching temperature is 25-30 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the dosage of 100g of calcined phosphogypsum is 450ml, the mass fraction of potassium oxide in the aqueous solution is 0.5%, the mass fraction of sodium carbonate is 0.4%, the mass fraction of calcium oxide is 0.1%, and the mass fraction of magnesium carbonate is 0.5%; wherein the medicament 2 is aqueous solution, the dosage of the calcined phosphogypsum of 100g is 420ml, and the mass ratio of potassium sulfate to sulfuric acid in the medicament 2 is 1: 10, the mass fraction of total sulfate groups in the aqueous solution was 3.5%.
Example 4. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, aging phosphogypsum taken back from a storage yard for 30 hours by using tap water, wherein the water content is controlled to be 30% during aging, so as to obtain the aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 40min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-milled phosphogypsum to 450 ℃, preserving the heat for 4 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 8 hours, and then adding a reagent 2 for heap leaching for 10 hours, wherein the heap leaching temperature is 30-40 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 11 is an aqueous solution, 100g of calcined phosphogypsum is used in 290ml of usage amount, the mass fraction of potassium oxide in the aqueous solution is 0.5 percent, the mass fraction of sodium carbonate is 0.4 percent, the mass fraction of calcium oxide is 0.1 percent, and the mass fraction of magnesium carbonate is 0.2 percent; wherein the medicament 2 is an aqueous solution, the dosage of the calcined phosphogypsum is 460ml according to 100g, and the mass ratio of sodium sulfate, potassium sulfate and sulfuric acid in the medicament 2 is 0.5: 0.5: 10, the mass fraction of total sulfate in the aqueous solution was 4.2%.
Example 5. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, aging phosphogypsum taken back from a storage yard for 24 hours by using tap water, wherein the water content is controlled to be 30% during aging, so as to obtain the aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 20min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-milled phosphogypsum to 400 ℃, preserving the heat for 2 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 5h, and then adding a reagent 2 for heap leaching for 7h, wherein the heap leaching temperature is 25 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the dosage of the calcined phosphogypsum is 500ml according to 100g, the mass fraction of potassium oxide in the aqueous solution is 1 percent, the mass fraction of sodium carbonate is 1 percent, the mass fraction of calcium oxide is 1 percent, and the mass fraction of magnesium carbonate is 2 percent; wherein the agent 2 is aqueous solution, the dosage of 100g of calcined phosphogypsum is 300ml, and the mass ratio of sodium sulfate, potassium sulfate and sulfuric acid in the agent 2 is 1: 1: 1, the mass fraction of total sulfate radicals in the aqueous solution is 5%.
Example 6. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 48 hours by using tap water, wherein the water content is controlled to be 50% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 50min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-ground phosphogypsum to 600 ℃, preserving the heat for 5 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for 10 hours of heap leaching, and then adding a reagent 2 for 14 hours of heap leaching, wherein the heap leaching temperature is 50 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the dosage of 100g of calcined phosphogypsum is 200ml, the mass fraction of potassium oxide in the aqueous solution is 0.5 percent, the mass fraction of sodium carbonate is 0.5 percent, the mass fraction of calcium oxide is 1 percent, and the mass fraction of magnesium carbonate is 2 percent; wherein the medicament 2 is aqueous solution, the dosage of 100g of calcined phosphogypsum is 350ml, and the mass ratio of sodium sulfate, potassium sulfate and sulfuric acid in the medicament 2 is 1: 1: 1, the mass fraction of total sulfate radicals in the aqueous solution was 3%.
Example 7. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 36 hours by using tap water, wherein the water content is controlled to be 40% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 35min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-ground phosphogypsum to 500 ℃, preserving heat for 3.5 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 7.5h, and then adding a reagent 2 for heap leaching for 10.5h, wherein the heap leaching temperature is 37 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, 100g of calcined phosphogypsum is used in an amount of 280ml, the mass fraction of potassium oxide in the aqueous solution is 3%, and the mass fraction of sodium carbonate is 2%; the reagent 2 is an aqueous solution, 100g of calcined phosphogypsum is used in 380ml of usage amount, and the mass ratio of sodium sulfate to potassium sulfate in the reagent 2 is 1: 3, the mass fraction of total sulfate radicals in the aqueous solution is 3%.
Example 8. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 36 hours by using tap water, wherein the water content is controlled to be 40% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 35min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-ground phosphogypsum to 500 ℃, preserving heat for 3.5 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 7.5h, and then adding a reagent 2 for heap leaching for 10.5h, wherein the heap leaching temperature is 37 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the usage amount of 100g of calcined phosphogypsum is 480ml, the mass fraction of sodium carbonate in the aqueous solution is 0.2%, the mass fraction of calcium oxide is 0.5%, and the mass fraction of magnesium carbonate is 2.5%; wherein the agent 2 is an aqueous solution, 100g of calcined phosphogypsum is used in 380ml of usage amount, and the mass fraction of sulfate radicals provided by potassium sulfate in the agent 2 is 3.5%.
Example 9. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 36 hours by using tap water, wherein the water content is controlled to be 40% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 35min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-ground phosphogypsum to 500 ℃, preserving heat for 3.5 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 7.5h, and then adding a reagent 2 for heap leaching for 10.5h, wherein the heap leaching temperature is 37 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the using amount of 100g of calcined phosphogypsum is 480ml, the mass fraction of calcium oxide in the aqueous solution is 3 percent, and the mass fraction of magnesium carbonate is 3 percent; wherein the agent 2 is an aqueous solution, the dosage of 100g of calcined phosphogypsum is 410ml, and the mass fraction of sulfate radicals provided by sulfuric acid in the agent 2 is 4%.
Example 10. A method for improving the gelling activity of phosphogypsum comprises the following steps:
(1) firstly, ageing phosphogypsum taken back from a storage yard for 36 hours by using tap water, wherein the water content is controlled to be 40% during ageing, so as to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum for 35min by using a ball mill to obtain the wet-ground phosphogypsum;
(3) roasting the wet-ground phosphogypsum to 500 ℃, preserving heat for 3.5 hours, and then naturally cooling to obtain the roasted phosphogypsum;
(4) firstly, adding a reagent 1 pair into calcined phosphogypsum for heap leaching for 7.5h, and then adding a reagent 2 for heap leaching for 10.5h, wherein the heap leaching temperature is 37 ℃, so as to obtain the phosphogypsum with improved gelling activity; wherein the medicament 1 is an aqueous solution, the dosage of 100g of calcined phosphogypsum is 340ml, the mass fraction of potassium oxide in the aqueous solution is 0.5 percent, the mass fraction of sodium carbonate is 0.5 percent, the mass fraction of calcium oxide is 0.5 percent, and the mass fraction of magnesium carbonate is 1.5 percent; wherein the medicament 2 is aqueous solution, the dosage of 100g of calcined phosphogypsum is 440ml, and the mass ratio of sodium sulfate to sulfuric acid in the medicament 2 is 2: and 5, the mass fraction of the total sulfate radicals in the aqueous solution is 3.1 percent.

Claims (9)

1. A method for improving the gelling activity of phosphogypsum is characterized by comprising the following steps: the method comprises the following steps:
(1) aging phosphogypsum by water to obtain aged phosphogypsum;
(2) wet grinding the aged phosphogypsum to obtain the wet-ground phosphogypsum;
(3) roasting and cooling the wet-milled phosphogypsum to obtain roasted phosphogypsum;
(4) and (3) respectively carrying out two-stage heap leaching on the calcined phosphogypsum by using a medicament 1 and a medicament 2 to obtain the phosphogypsum with improved gelling activity.
2. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: in the step (1), running water is used for aging the phosphogypsum for 24-48h, and the water content is 30-50% during aging, so that the aged phosphogypsum is obtained.
3. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: and (2) wet-grinding the aged phosphogypsum for 20-50min to obtain the wet-ground phosphogypsum.
4. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: and (3) roasting the wet-ground phosphogypsum to 400-600 ℃, preserving the heat for 2-5h, and naturally cooling to obtain the roasted phosphogypsum.
5. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: the medicament 1 is an aqueous solution prepared from one or more of potassium oxide, sodium carbonate, calcium oxide and magnesium carbonate; in the prepared aqueous solution, the total mass fraction of potassium oxide, sodium carbonate, calcium oxide and magnesium carbonate is 3-6%.
6. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: the dosage of the medicament 1 is 200-500ml of the medicament 1 for every 100g of calcined phosphogypsum.
7. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: the medicament 2 is an aqueous solution prepared from one or more of sodium sulfate, potassium sulfate and sulfuric acid; in the prepared water solution, the mass fraction of sulfate radicals is 3-5%.
8. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: the dosage of the reagent 2 is 300-500ml of the reagent 2 for every 100g of calcined phosphogypsum.
9. The method for increasing the gelling activity of phosphogypsum according to claim 1, characterized in that: in the step (4), firstly, the agent 1 pair of heap leaching is applied to the calcined phosphogypsum for 5-10h, then the agent 2 is applied for 7-14h, and the heap leaching temperature is 25-50 ℃.
CN202010663619.6A 2020-07-10 2020-07-10 Method for improving phosphogypsum gelling activity Pending CN111792862A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010663619.6A CN111792862A (en) 2020-07-10 2020-07-10 Method for improving phosphogypsum gelling activity

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010663619.6A CN111792862A (en) 2020-07-10 2020-07-10 Method for improving phosphogypsum gelling activity

Publications (1)

Publication Number Publication Date
CN111792862A true CN111792862A (en) 2020-10-20

Family

ID=72806922

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010663619.6A Pending CN111792862A (en) 2020-07-10 2020-07-10 Method for improving phosphogypsum gelling activity

Country Status (1)

Country Link
CN (1) CN111792862A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115677247A (en) * 2022-11-07 2023-02-03 中化学生态环境有限公司 Method for modifying phosphogypsum by alkaline oxide

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515681A (en) * 2011-12-12 2012-06-27 昆明理工大学 Method for producing aerated building block with phosphogypsum as main raw material
CN102745926A (en) * 2012-07-13 2012-10-24 武汉亿胜科技有限公司 Modified phosphogypsum and preparation method thereof
CN106517978A (en) * 2016-10-31 2017-03-22 同济大学 Light-weight thermal mortar taking ardealite hydraulic compound gel material as principal material
CN106630882A (en) * 2015-11-04 2017-05-10 北京高能时代环境技术股份有限公司 Medium/high-strength concrete prepared from modified phosphogypsum based binding material and manufacturing method of concrete
CN110627391A (en) * 2019-10-25 2019-12-31 湖北工业大学 High-activity anhydrous phosphogypsum cementing material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515681A (en) * 2011-12-12 2012-06-27 昆明理工大学 Method for producing aerated building block with phosphogypsum as main raw material
CN102745926A (en) * 2012-07-13 2012-10-24 武汉亿胜科技有限公司 Modified phosphogypsum and preparation method thereof
CN106630882A (en) * 2015-11-04 2017-05-10 北京高能时代环境技术股份有限公司 Medium/high-strength concrete prepared from modified phosphogypsum based binding material and manufacturing method of concrete
CN106517978A (en) * 2016-10-31 2017-03-22 同济大学 Light-weight thermal mortar taking ardealite hydraulic compound gel material as principal material
CN110627391A (en) * 2019-10-25 2019-12-31 湖北工业大学 High-activity anhydrous phosphogypsum cementing material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
安艳玲等: "《磷石膏、脱硫石膏资源化与循环经济》", 31 March 2011, 贵州大学出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115677247A (en) * 2022-11-07 2023-02-03 中化学生态环境有限公司 Method for modifying phosphogypsum by alkaline oxide

Similar Documents

Publication Publication Date Title
CN110627391B (en) High-activity anhydrous phosphogypsum cementing material and preparation method thereof
CN108275992B (en) Wide-temperature low-power-consumption high-magnetic-permeability manganese-zinc ferrite material and preparation method thereof
CN104446841A (en) Special fertilizer for peach trees as well as preparation method and application thereof
CN111792862A (en) Method for improving phosphogypsum gelling activity
CN107056400A (en) One kind is used for Edible Fungi compound water retaining agent and preparation method thereof
CN104607144A (en) Structure self-growing aqueous phase phosphate radical adsorbing material and preparation method and application thereof
CN101712471A (en) Method for producing active carbon from agaric bacteria waste base stock
CN114538884A (en) Quick-setting early-strength formed wooden board and preparation method thereof
CN101921141B (en) Method for preparing mineral potassic fertilizer from potassium-enriched rock
CN105985038B (en) A kind of water-fast and sulfate attack inorganic coagulation material and preparation method thereof
CN102249814A (en) Preparation method of liquid fertilizer with humic acid-urea complex as matrix
CN100545091C (en) A kind of production method of high-purity big particle industrial anhydrous sodium sulfate
CN102924644B (en) A kind of preparation method of vinylformic acid moisturizing matrix material
CN106542880A (en) One kind is conducive to improving photosynthetic high-efficiency sustained-release fertilizer of Flos Tagetis Erectae and preparation method thereof
CN113149469B (en) Method for producing lime by combining waste coal with sintering plant
CN110993230A (en) Rare earth RE applied to low-temperature magnetic refrigeration2MnCuO6Material and preparation method
CN114702963A (en) Method for preparing soil conditioner by self-propagating pyrolysis of phosphogypsum and biomass
CN103641581A (en) An efficient compound fertilizer and a preparation method thereof
CN108975739A (en) A kind of preparation method of modified coal ash
CN115196647A (en) Flaky boric acid and preparation method thereof
CN107384421A (en) A kind of moderate alkaline soil modifier
CN106045448A (en) Production process for phosphogypsum baking-free brick
CN106242738A (en) A kind of selenium-enriched foliage fertilizer material
CN110644242A (en) Preparation method for improving filling power of down feather
CN107973588A (en) A kind of Materials with High Strength

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination