CN105036579A - Beta-phosphorus building plaster preparing method - Google Patents

Beta-phosphorus building plaster preparing method Download PDF

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Publication number
CN105036579A
CN105036579A CN201510436927.4A CN201510436927A CN105036579A CN 105036579 A CN105036579 A CN 105036579A CN 201510436927 A CN201510436927 A CN 201510436927A CN 105036579 A CN105036579 A CN 105036579A
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paris
mixture
beta
phosphorus
leave standstill
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Inventor
杜晨溪
赵志曼
田睿
刘育成
张文佳
姚毅惠
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YUNNAN KUNGANG STEEL STRUCTURE CO Ltd
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YUNNAN KUNGANG STEEL STRUCTURE CO Ltd
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Publication of CN105036579A publication Critical patent/CN105036579A/en
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Abstract

The invention discloses a beta-phosphorus building plaster preparing method. The method comprises the steps of screening ardealite firstly, and then mixing the screened ardealite with water and citric acid in certain proportion to obtain a mixed material; conducting stirring and standing in sequence repeatedly till floating objects on the surface of the mixed material are completely removed; adding Ca(OH)2, conducting stirring and standing till the pH value of the mixed material is 7-10, obtaining a discharged material, conducting heating and drying, and obtaining beta-phosphorus building plaster through secondary screening after the discharged material is naturally cooled to normal temperature. By conducting secondary screening and adding a habit modifier, impurities such as P, F and organic matter can be effectively removed, the crystal shape of the ardealite is converted smoothly, and then the high-strength beta-phosphorus building plaster is obtained. By the adoption of the method, the usage and number of varieties of chemical reagents are reduced, the problems of traditional beta-phosphorus building plaster production methods that a large number of chemical reagents are added, the production process is complicated, and secondary pollution is serious are solved, and production cost is saved.

Description

The preparation method of a kind of β-phosphorus plaster of Paris
Technical field
The present invention relates to the preparation method of a kind of β-phosphorus plaster of Paris, belong to gypsum material technical field.
Background technology
β-phosphorus plaster of Paris refers to and utilizes phosphogypsum waste material to form β-phosphorus plaster of Paris (β-phosphorus semi-hydrated gypsum CaSO through removal of impurities with after turning brilliant process 41/2H 2o).Usually be the β-phosphorus plaster of Paris of waste with phosphogypsum, β-calcium sulphate hemihydrate (β-CaSO in its composition 41/2H 20) content (massfraction) should be not less than 60.0%(standard GB/T/T9776-2008).
Current preparation β-phosphorus plaster of Paris is mainly by washing, flotation, neutralization, calcining four processes.Wherein, not only need to add a large amount of chemical reagent (causing secondary pollution) at the washing of pretreatment stage, flotation, N-process, and its complex process is loaded down with trivial details.Therefore, be necessary to improve the early pre-treatment process of β-phosphorus plaster of Paris, to reach preparation, β-phosphorus plaster of Paris production technique is simple, product cost is high, reduces the object of secondary pollution.
Summary of the invention
For adding the present situations such as a large amount of chemical reagent, complex manufacturing is loaded down with trivial details, secondary pollution is more serious when solving and produce β-phosphorus plaster of Paris at present, the invention provides the preparation method of a kind of β-phosphorus plaster of Paris, simplify β-phosphorus plaster of Paris production technique to reach, reduce the object of secondary pollution.
Technical solution of the present invention and step as follows: the preparation method of a kind of β-phosphorus plaster of Paris, through following each step:
(1) phosphogypsum is sieved;
(2) phosphogypsum after step (1) being sieved and water, citric acid are 150:(70 ~ 80 in mass ratio): (0.45 ~ 0.525) mixes, and obtains mixture;
(3) step (2) gained mixture is stirred 10 ~ 20min and make it even, then leave standstill 30 ~ 40min, to remove the floating matter floated on fluid surface, the operation repeating to stir and leave standstill is until the floaters on surface of mixture is eliminated completely;
(4) mixture after step (3) being processed adds Ca (OH) 2, then stir 10 ~ 20min, leave standstill 30 ~ 40min, pH value determination, repeats to add Ca (OH) 2, stir and leave standstill operation, until the pH value of mixture is 7 ~ 10, obtain discharging;
(5) be 2 ~ 4cm by step (4) gained discharging paving to thickness, then be placed in air blast constant temperature oven and realize dry with 160 DEG C of heating 3h, then naturally cool to normal temperature, after screening again, namely obtain β-phosphorus plaster of Paris.
In described step (2), the particle diameter of citric acid is 1 μm ~ 1mm, and the composition of its mass percent is: C 6h 8o 7h 2o>=99.5%, all the other are impurity.Citric acid, as medium crystallization agent, has and promote that plane of crystal is from discrete piece shape to the effect of short and thick shape future development, and citric acid is cheap.
Screening in described step (1) and step (5) is the square hole sieve of 0.2mm by size of mesh, makes granularity be 100 ~ 200 orders.
In described step (1), the composition of the mass percent of phosphogypsum is:
SO 343.00~46.00%、P 2O 50.50~0.70%、SiO 213.00~16.00%、
CaO19.00~22.00%、Fe 2O 30.30~0.50%、MgO0.03~0.035%、
H 2O4.00~7.00%、F0.11~0.20%、Al 2O 30.50~1.00%、Cl0.011~0.013%。
The composition of the mass percent of described step (5) gained β-phosphorus plaster of Paris is:
SO 350.00~55.00%、P 2O 50.40~0.50%、SiO 212.00~14.00%、
CaO25.00~27.00%、Fe 2O 30.30~0.45%、MgO0.03~0.035%、
H 2O2.00~3.00%、F0.05~0.08%、Al 2O 30.50~1.00%、Cl0.011~0.013%。
The present invention uses material sieving technology twice, and final acquisition meets β-phosphorus plaster of Paris that national standard requires.Can obtain by contrasting above two kinds of components, phosphogypsum after treatment, its main chemical compositions SO 3, CaO content increases, P 2o 5, SiO 2, H 2o, F content reduces to some extent; Fe 2o 3, MgO, Al 2o 3, Cl remains unchanged substantially.Significant contribution of the present invention is physical method (method of sieving) and chemical process to carry out reasonable combination, provides the effective way simplifying production technique, minimizing secondary pollution and attenuating production cost and prepare β-phosphorus plaster of Paris.
Owing to implementing material sieving technology (step 1), greatly reduce number of times and the intensity of washing raw material, and substantially can omit floatation process; Again carry out screening (step 5) to through heat treated phosphogypsum on this basis, just can be met the β-phosphorus plaster of Paris even exceeding national standard and require.Preparating mechanism of the present invention on traditional phosphogypsum treatment process, adds physical treatment method, i.e. regrading method, thus the removal of impurities and the speed of reaction that accelerate phosphogypsum.
The advantage that the present invention possesses and effect are: phosphogypsum is the by product of phosphorus industry, its main component can not have greatly changed along with the change of region, wherein the impurity such as P, F and organism be affect that phosphogypsum is prepared into β-phosphorus plaster of Paris mainly contain harmful substances, wherein P, F impurity forms insoluble Ca in gypsum conversion reaction process 3(PO 4) 2and CaF 2be deposited on CaSO 42H 2o surface, has a strong impact on CaSO 41/2H 2the integrity of O crystal development, causes the strength degradation of phosphorus plaster of Paris.The present invention is by regrading and add medium crystallization agent (citric acid), can effectively remove the impurity such as P, F and organism, make the crystal-type shape of phosphogypsum change (from discrete piece shape to short and thick shape) smoothly as shown in Figure 1, 2, thus obtain the β-phosphorus plaster of Paris of higher-strength.The present invention reduces the consumption of chemical reagent and use kind, use regrading method and citric acid (effective, cheap) process phosphogypsum, the problem such as add a large amount of chemical reagent (as ethylenediamine tetraacetic acid (EDTA) and succinic acid etc.) when overcoming traditional mode of production β-phosphorus plaster of Paris, complex manufacturing is loaded down with trivial details, secondary pollution is serious, has saved production cost simultaneously.
Accompanying drawing explanation
Fig. 1 is the SEM figure of phosphogypsum.
Fig. 2 is the SEM figure of gained of the present invention β-phosphorus plaster of Paris.
Embodiment
Below by example, the present invention will be further described.
Embodiment 1
(1) being carried out by phosphogypsum being sized to granularity is 100 ~ 200 orders, and the composition of its mass percent is: SO 344.58%, P 2o 50.60%, H 2o5.34%, Al 2o 30.76%, SiO 215.68%, CaO21.56%, F0.15%, Cl0.012%, Fe 2o 30.36%, MgO0.03%;
(2) phosphogypsum after step (1) being sieved mixes for 150:75:0.5 in mass ratio with water, citric acid, and obtain mixture, the particle diameter of citric acid is 1 μm ~ 1mm, and the composition of its mass percent is: C 6h 8o 7h 2o>=99.5%, all the other are impurity;
(3) step (2) gained mixture is stirred 20min and make it even, then leave standstill 30min, to remove the floating matter floated on fluid surface, the operation repeating to stir and leave standstill is until the floaters on surface of mixture is eliminated completely;
(4) mixture after step (3) being processed adds Ca (OH) 2, then stir 15min, leave standstill 35min, pH value determination, repeats to add Ca (OH) 2, stir and leave standstill operation, until the pH value of mixture is 7 ~ 10, obtain discharging;
(5) be 2 ~ 4cm by step (4) gained discharging paving to thickness, then be placed in air blast constant temperature oven and realize dry with 160 DEG C of heating 3h, then naturally cooling to normal temperature, namely obtaining β-phosphorus plaster of Paris through being again sized to after granularity is 100 ~ 200 orders.The composition of the mass percent of gained β-phosphorus plaster of Paris is:
SO 350.8%、P 2O 50.45%、SiO 213.68%、
CaO26.3%、Fe 2O 30.35%、MgO0.03%、
H 2O2.1%、F0.06%、Al 2O 30.63%、Cl0.012%。
Embodiment 2
(1) being carried out by phosphogypsum being sized to granularity is 100 ~ 200 orders, its CaSO 42H 2o content is 87.62%, and the composition of mass percent is: SO 345.32%, P 2o 50.51%, H 2o6.54%, Al 2o 30.51%, SiO 214.78%, CaO20.66%, F0.14%, Cl0.011%, Fe 2o 30.46%, MgO0.030%;
(2) phosphogypsum after step (1) being sieved mixes for 150:80:0.525 in mass ratio with water, citric acid, and obtain mixture, the particle diameter of citric acid is 1 μm ~ 1mm, and the composition of its mass percent is: C 6h 8o 7h 2o>=99.5%, all the other are impurity;
(3) step (2) gained mixture is stirred 15min and make it even, then leave standstill 35min, to remove the floating matter floated on fluid surface, the operation repeating to stir and leave standstill is until the floaters on surface of mixture is eliminated completely;
(4) mixture after step (3) being processed adds Ca (OH) 2, then stir 20min, leave standstill 30min, pH value determination, repeats to add Ca (OH) 2, stir and leave standstill operation, until the pH value of mixture is 7 ~ 10, obtain discharging;
(5) be 2 ~ 4cm by step (4) gained discharging paving to thickness, then be placed in air blast constant temperature oven and realize dry with 160 DEG C of heating 3h, then naturally cooling to normal temperature, namely obtaining β-phosphorus plaster of Paris through being again sized to after granularity is 100 ~ 200 orders.The composition of the mass percent of gained β-phosphorus plaster of Paris is:
SO 354.3%、P 2O 50.42%、SiO 212.85%、
CaO25.8%、Fe 2O 30.45%、MgO0.03%、
H 2O2.36%、F0.05%、Al 2O 30.51%、Cl0.011%。
Embodiment 3
(1) being carried out by phosphogypsum being sized to granularity is 100 ~ 200 orders, its CaSO 42H 2o content is 79.56%, and the composition of mass percent is: SO 343.51%, P 2o 50.70%, H 2o4.22%, Al 2o 30.67%SiO 215.18%, CaO19.82%, F0.14%, Cl0.012%, Fe 2o 30.35%, MgO0.03%;
(2) phosphogypsum after step (1) being sieved mixes for 150:70:0.45 in mass ratio with water, citric acid, and obtain mixture, the particle diameter of citric acid is 1 μm ~ 1mm, and the composition of its mass percent is: C 6h 8o 7h 2o>=99.5%, all the other are impurity;
(3) step (2) gained mixture is stirred 10min and make it even, then leave standstill 40min, to remove the floating matter floated on fluid surface, the operation repeating to stir and leave standstill is until the floaters on surface of mixture is eliminated completely;
(4) mixture after step (3) being processed adds Ca (OH) 2, then stir 10min, leave standstill 40min, pH value determination, repeats to add Ca (OH) 2, stir and leave standstill operation, until the pH value of mixture is 7 ~ 10, obtain discharging;
(5) be 2 ~ 4cm by step (4) gained discharging paving to thickness, then be placed in air blast constant temperature oven and realize dry with 160 DEG C of heating 3h, then naturally cooling to normal temperature, namely obtaining β-phosphorus plaster of Paris through being again sized to after granularity is 100 ~ 200 orders.The composition of the mass percent of gained β-phosphorus plaster of Paris is:
SO 355%、P 2O 50.42%、SiO 213.6%、
CaO26.7%、Fe 2O 30.32%、MgO0.03%、
H 2O2%、F0.07%、Al 2O 30.52%、Cl0.011%。
Detect respectively the fineness of example 1,2,3 gained β-phosphorus plaster of Paris, time of coagulation, intensity and coefficient of softening according to plaster of Paris standard (GB/T9776-2008), its result is as shown in table 1.
Test-results shows, β-its fineness of phosphorus plaster of Paris of example 1,2,3, time of coagulation and intensity all meet and even exceedes national standard requirement; Especially its coefficient of softening is greater than 0.80(because of gypsum and belongs to air hardening cementitious materials, and relevant criterion does not generally require the water tolerance of gypsum), this value shows that β-phosphorus plaster of Paris that the present invention develops is regarded as water-resistant material.
The technological property of table 1 gained β-phosphorus plaster of Paris of the present invention

Claims (3)

1. a preparation method for β-phosphorus plaster of Paris, is characterized in that through following each step:
(1) phosphogypsum is sieved;
(2) phosphogypsum after step (1) being sieved and water, citric acid are 150:(70 ~ 80 in mass ratio): (0.45 ~ 0.525) mixes, and obtains mixture;
(3) step (2) gained mixture is stirred 10 ~ 20min, then leave standstill 30 ~ 40min, the operation repeating to stir and leave standstill is until the floaters on surface of mixture is eliminated completely;
(4) mixture after step (3) being processed adds Ca (OH) 2, then stir 10 ~ 20min, leave standstill 30 ~ 40min, pH value determination, repeats to add Ca (OH) 2, stir and leave standstill operation, until the pH value of mixture is 7 ~ 10, obtain discharging;
(5) be 2 ~ 4cm by step (4) gained discharging paving to thickness, then realize dry with 160 DEG C of heating 3h, then naturally cool to normal temperature, after screening again, namely obtain β-phosphorus plaster of Paris.
2. preparation method according to claim 1, is characterized in that: in described step (2), the particle diameter of citric acid is 1 μm ~ 1mm, and the composition of its mass percent is: C 6h 8o 7h 2o>=99.5%, all the other are impurity.
3. preparation method according to claim 1 and 2, is characterized in that: the screening in described step (1) and step (5) is the square hole sieve of 0.2mm by size of mesh, makes granularity be 100 ~ 200 orders.
CN201510436927.4A 2015-07-23 2015-07-23 Beta-phosphorus building plaster preparing method Pending CN105036579A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106630890A (en) * 2016-11-25 2017-05-10 云南昆钢钢结构股份有限公司 A light ardealite-based fireproof non-burned building block and a preparing method thereof
CN106677418A (en) * 2017-01-12 2017-05-17 云南昆钢建设集团有限公司 Cast-in-situ ardealite based early strength fireproof composite wallboard and preparation method thereof
CN106854907A (en) * 2017-02-22 2017-06-16 云南昆钢建设集团有限公司 A kind of cast-in-place ardealite base superelevation combined wall and its construction method
CN107324676A (en) * 2017-07-24 2017-11-07 武汉理工大学 The method that β semi-hydrated gypsums are prepared using low grade coal calcined phosphogypsum and carbide slurry
CN111393052A (en) * 2020-03-06 2020-07-10 三峡大学 Device and method for pretreating phosphogypsum by using magnesium hydroxide
CN111559896A (en) * 2020-05-08 2020-08-21 张延年 Foaming phosphogypsum building block and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
韩松 等: "关于利用云南磷石膏制备磷建筑石膏预处理实验研究", 《科学技术与工程》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106630890A (en) * 2016-11-25 2017-05-10 云南昆钢钢结构股份有限公司 A light ardealite-based fireproof non-burned building block and a preparing method thereof
CN106677418A (en) * 2017-01-12 2017-05-17 云南昆钢建设集团有限公司 Cast-in-situ ardealite based early strength fireproof composite wallboard and preparation method thereof
CN106854907A (en) * 2017-02-22 2017-06-16 云南昆钢建设集团有限公司 A kind of cast-in-place ardealite base superelevation combined wall and its construction method
CN107324676A (en) * 2017-07-24 2017-11-07 武汉理工大学 The method that β semi-hydrated gypsums are prepared using low grade coal calcined phosphogypsum and carbide slurry
CN107324676B (en) * 2017-07-24 2019-11-26 武汉理工大学 β-semi-hydrated gypsum method is prepared using low grade coal calcined phosphogypsum and carbide slurry
CN111393052A (en) * 2020-03-06 2020-07-10 三峡大学 Device and method for pretreating phosphogypsum by using magnesium hydroxide
CN111559896A (en) * 2020-05-08 2020-08-21 张延年 Foaming phosphogypsum building block and preparation method thereof

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