CN104176955B - A kind of method of modifying of fluorgypsum - Google Patents
A kind of method of modifying of fluorgypsum Download PDFInfo
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- CN104176955B CN104176955B CN201410390525.0A CN201410390525A CN104176955B CN 104176955 B CN104176955 B CN 104176955B CN 201410390525 A CN201410390525 A CN 201410390525A CN 104176955 B CN104176955 B CN 104176955B
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Abstract
The invention discloses a kind of method of modifying of fluorgypsum, have employed grind, thermal treatment, twice chemical modification and calcining; Thermal treatment temp is 105-115 DEG C, and the time is 5-8h; In a chemical modification, in the fluorgypsum by weight after every 100 parts of thermal treatments, add the rhombspar after calcining in the alum in 1-1.8 part calcium hydroxide, 1-2 part blast-furnace slag, 1-1.5 part S1 after calcining, 0.5-0.8 part S2; In secondary chemical modification, in the fluorgypsum by weight after every 100 parts of calcinings, add 0.5-0.8 part flyash, 0.5-0.8 part corn straw modification fiber, 1-1.2 part wilkinite; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber.The method of modifying of fluorgypsum of the present invention, shortens the time of coagulation of modified fluorgypsum, improves the mechanical strength of modified fluorgypsum.
Description
Technical field
The present invention relates to fluorgypsum technical field, particularly relate to a kind of method of modifying of fluorgypsum.
Background technology
Fluorgypsum is the principal by product in hydrofluoric acid and sodium fluoroaluminate production process, mainly originates from inorganic fluoride and organic fluoride factory and other Acid of Hydrofluoric Acid Production factory.Often produce 1t hydrofluoric acid and generate the anhydrous fluorgypsum of about 3.6t.The main component of fluorgypsum is calcium sulfate, and containing partially fluorinated calcium and other fluorochemicals, and H sometimes
2sO
4content is very high, makes the fluorgypsum of discharging in acid, belongs to severe corrosive poisonous and harmful refuse, and the fluorgypsum not adding process directly can not be put and abandon, and is also difficult to be utilized.Again because the lower and dissolution rate of fluorgypsum solubleness is slow, time of coagulation is very long, and hydration and hardening body intensity is very little, its application of these drawbacks limit.At present, except part fluorgypsum is utilized, major part is stored up as general solid waste, not only land occupation, and simultaneously objectionable impurities wherein also can produce water body and pollute, and produces threaten physical environment.Therefore, how to solve the fluorgypsum especially history wet fluorgypsum problem of storing up, make it turn waste into wealth, the comprehensive utilization realizing gypsum resource is a very urgent problems.
Summary of the invention
The present invention proposes a kind of method of modifying of fluorgypsum, by the fluorgypsum that the method is modified, time of coagulation is short, and hydration and hardening intensity is high.
The present invention proposes a kind of method of modifying of fluorgypsum, comprise the following steps:
S1, fluorgypsum put into grinding in ball grinder and pulverize, put into baking oven after sieving and heat-treat, thermal treatment temp is 105-115 DEG C, and the time is 5-8h;
S2, alum is put into retort furnace calcine, calcining temperature is 600-650 DEG C, and calcination time is 0.8-1.3h, is cooled to grinding after room temperature, sieving for standby; Rhombspar is put into retort furnace calcine, calcining temperature is 700-800 DEG C, and calcination time is 1-1.5h, is cooled to grinding, sieving for standby after room temperature;
The rhombspar after calcining in the alum in calcium hydroxide, blast-furnace slag, S2 after calcining, S2 is added in S3, fluorgypsum in S1 after thermal treatment, stir, standing 10-20h carries out a chemical modification, and then 250-300 DEG C of calcining, calcination time is 0.5-1.5h; Wherein, the rhombspar after calcining in the alum in 1-1.8 part calcium hydroxide, 1-2 part blast-furnace slag, 1-1.5 part S1 after calcining, 0.5-0.8 part S2 is added in the fluorgypsum by weight after every 100 parts of thermal treatments;
Add flyash in S4, fluorgypsum in S3 after calcining, corn straw modification fiber, wilkinite carry out secondary chemical modification; Wherein, 0.5-0.8 part flyash, 0.5-0.8 part corn straw modification fiber, 1-1.2 part wilkinite is added in the fluorgypsum by weight after every 100 parts of calcinings; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber;
S5, the fluorgypsum obtained is put into curing field maintenance appear on the scene after 10 days in S4.
Preferably, in S1, thermal treatment temp is 110-113 DEG C, and the time is 6-7h.
Preferably, in S1, thermal treatment temp is 112 DEG C, and the time is 6.3h.
Preferably, in S3, after the fluorgypsum in S1 after thermal treatment carries out a chemical modification, 285-295 DEG C of calcining, calcination time is 0.8-1.2h.
Preferably, in S3, after the fluorgypsum in S1 after thermal treatment carries out a chemical modification, 290 DEG C of calcinings, calcination time is 1.0h.
Preferably, in S3, in a chemical modification, in the fluorgypsum by weight after every 100 parts of thermal treatments, add the rhombspar after calcining in the alum in 1.2-1.6 part calcium hydroxide, 1.5-1.7 part blast-furnace slag, 1.2-1.3 part S2 after calcining, 0.6-0.65 part S2.
Preferably, in S3, in a chemical modification, in the fluorgypsum by weight after every 100 parts of thermal treatments, add the rhombspar after calcining in the alum in 1.4 parts of calcium hydroxides, 1.6 parts of blast-furnace slags, 1.25 parts of S2 after calcining, 0.63 part of S2.
Preferably, in S4, in secondary chemical modification, in the fluorgypsum by weight after every 100 parts of calcinings, add 0.6-0.68 part flyash, 0.6-0.7 part corn straw modification fiber, 1.1-1.15 part wilkinite.
Preferably, in S4, in secondary chemical modification, in the fluorgypsum by weight after every 100 parts of calcinings, add 0.65 part of flyash, 0.68 part of corn straw modification fiber, 1.13 parts of wilkinites.
In the method for modifying of fluorgypsum of the present invention, have employed and grind and thermal treatment, change, destroy the crystal lattice of modified fluorgypsum, increase its lattice distortion and defect, increase the irregularity of its specific surface area and surface tissue, improve the hydration activity of modified fluorgypsum, facilitate the hardening of modified fluorgypsum; Have employed twice chemical modifying process, in a chemical modification, with the addition of the rhombspar after the alum after calcining and calcining, make modified fluorgypsum, dihydrate gypsum crystal increasing number, and crystal development is complete, length-to-diameter ratio increases, and how in needle-like, decreases obvious bulk or bulk crystalline, between crystal, overlap joint is fine and close, improves the hydration and hardening intensity of modified fluorgypsum; In secondary chemical modification, with the addition of Modification of Styrene-Acrylate Emulsion corn stalk fiber, the existence of benzene emulsion, on the one hand, the surface of the original rough porous of corn stalk fiber is filled, improve effective contact area of corn stalk fiber and fluorgypsum matrix, improve the interface bond strength of corn stalk fiber and fluorgypsum matrix; On the other hand, the interface cohesion place of corn stalk fiber and fluorgypsum matrix is made to form a flexible interface, when the micro-crack extension that fluorgypsum matrix carry load produces is to this interfacial layer, its propagation rate can slow down because of the existence of flexible interface layer, alleviate material to suddenly change the stress concentration caused, improve the bending and compressive strength of modification fluorgypsum.
In the method for modifying of fluorgypsum of the present invention, optimize the modified technique of fluorgypsum, have selected suitable properties-correcting agent, control the content of each composition in properties-correcting agent, adopt the fluorgypsum of the method modification, time of coagulation is short, after hydration and hardening, mechanical strength is high, and fluorgypsum is turned waste into wealth.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail; should understand; embodiment is only for illustration of the present invention, instead of for limiting the present invention, any amendment, equivalent replacement etc. made on basis of the present invention is all in protection scope of the present invention.
Embodiment 1
The method of modifying of fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum put into grinding in ball grinder and pulverize, put into baking oven after crossing 80 mesh sieves and heat-treat, thermal treatment temp is 105 DEG C, and the time is 8h;
S2, alum is put into retort furnace calcine, calcining temperature is 650 DEG C, and calcination time is 0.8h, and grinding after being cooled to room temperature, to cross 100 mesh sieves for subsequent use; Rhombspar is put into retort furnace calcine, calcining temperature is 800 DEG C, and calcination time is 1h, grinds, 100 mesh sieves are for subsequent use excessively after being cooled to room temperature;
Add the rhombspar after calcining in the alum in calcium hydroxide, blast-furnace slag, S2 after calcining, S2 in S3, fluorgypsum in S1 after thermal treatment, stir, standing 20h carries out a chemical modification, and then 268 DEG C of calcinings, calcination time is 1.3h; Wherein, the calcium hydroxide added in the fluorgypsum by weight after every 100 parts of thermal treatments is 1.4 parts, blast-furnace slag is 1 part, alum in S2 after calcining is 1 part, rhombspar in S2 after calcining is 0.8 part;
Add flyash in S4, fluorgypsum in S3 after calcining, corn straw modification fiber, wilkinite carry out secondary chemical modification; Wherein, the flyash added in the fluorgypsum by weight after every 100 parts of calcinings is 0.6 part, corn straw modification fiber is 0.5 part, wilkinite is 1 part; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber;
S5, the fluorgypsum obtained is put into curing field maintenance appear on the scene after 10 days in S4.
Embodiment 2
The method of modifying of fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum put into grinding in ball grinder and pulverize, put into baking oven after crossing 100 mesh sieves and heat-treat, thermal treatment temp is 115 DEG C, and the time is 5h;
S2, alum is put into retort furnace calcine, calcining temperature is 600 DEG C, and calcination time is 1.3h, and grinding after being cooled to room temperature, to cross 100 mesh sieves for subsequent use; Rhombspar is put into retort furnace calcine, calcining temperature is 722 DEG C, and calcination time is 1.38h, grinds, 100 mesh sieves are for subsequent use excessively after being cooled to room temperature;
Add the rhombspar after calcining in the alum in calcium hydroxide, blast-furnace slag, S2 after calcining, S2 in S3, fluorgypsum in S1 after thermal treatment, stir, standing 10h carries out a chemical modification, and then 250 DEG C of calcinings, calcination time is 1.5h; Wherein, the calcium hydroxide added in the fluorgypsum by weight after every 100 parts of thermal treatments is 1 part, blast-furnace slag is 2 parts, alum in S2 after calcining is 1.3 parts, rhombspar in S2 after calcining is 0.5 part;
Add flyash in S4, fluorgypsum in S3 after calcining, corn straw modification fiber, wilkinite carry out secondary chemical modification; Wherein, the flyash added in the fluorgypsum by weight after every 100 parts of calcinings is 0.8 part, corn straw modification fiber is 0.8 part, wilkinite is 1.1 parts; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber;
S5, the fluorgypsum obtained is put into curing field maintenance appear on the scene after 10 days in S4.
Embodiment 3
The method of modifying of fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum put into grinding in ball grinder and pulverize, put into baking oven after sieving and heat-treat, thermal treatment temp is 108 DEG C, and the time is 6.3h;
S2, alum is put into retort furnace calcine, calcining temperature is 621 DEG C, and calcination time is 0.95h, is cooled to grinding after room temperature, sieving for standby; Rhombspar is put into retort furnace calcine, calcining temperature is 700 DEG C, and calcination time is 1.5h, is cooled to grinding, sieving for standby after room temperature;
Add the rhombspar after calcining in the alum in calcium hydroxide, blast-furnace slag, S2 after calcining, S2 in S3, fluorgypsum in S1 after thermal treatment, stir, standing 14h carries out a chemical modification, and then 300 DEG C of calcinings, calcination time is 0.5h; Wherein, the calcium hydroxide added in the fluorgypsum by weight after every 100 parts of thermal treatments is 1.8 parts, blast-furnace slag is 1.3 parts, alum in S2 after calcining is 1.5 parts, rhombspar in S2 after calcining is 0.6 part;
Add flyash in S4, fluorgypsum in S3 after calcining, corn straw modification fiber, wilkinite carry out secondary chemical modification; Wherein, the flyash added in the fluorgypsum by weight after every 100 parts of calcinings is 0.5 part, corn straw modification fiber is 0.7 part, wilkinite is 1.2 parts; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber;
S5, the fluorgypsum obtained is put into curing field maintenance appear on the scene after 10 days in S4.
Embodiment 4
The method of modifying of fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum put into grinding in ball grinder and pulverize, put into baking oven after sieving and heat-treat, thermal treatment temp is 112 DEG C, and the time is 6.3h;
S2, alum is put into retort furnace calcine, calcining temperature is 640 DEG C, and calcination time is 1.05h, is cooled to grinding after room temperature, sieving for standby; Rhombspar is put into retort furnace calcine, calcining temperature is 750 DEG C, and calcination time is 1.3h, is cooled to grinding, sieving for standby after room temperature;
Add the rhombspar after calcining in the alum in calcium hydroxide, blast-furnace slag, S2 after calcining, S2 in S3, fluorgypsum in S1 after thermal treatment, stir, standing 16h carries out a chemical modification, and then 290 DEG C of calcinings, calcination time is 1.0h; Wherein, the calcium hydroxide added in the fluorgypsum by weight after every 100 parts of thermal treatments is 1.4 parts, blast-furnace slag is 1.6 parts, alum in S2 after calcining is 1.25 parts, rhombspar in S2 after calcining is 0.63 part;
Add flyash in S4, fluorgypsum in S3 after calcining, corn straw modification fiber, wilkinite carry out secondary chemical modification; Wherein, the flyash added in the fluorgypsum by weight after every 100 parts of calcinings is 0.65 part, corn straw modification fiber is 0.68 part, wilkinite is 1.13 parts; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber;
S5, the fluorgypsum obtained is put into curing field maintenance appear on the scene after 10 days in S4.
Claims (9)
1. a method of modifying for fluorgypsum, is characterized in that, comprises the following steps:
S1, fluorgypsum put into grinding in ball grinder and pulverize, put into baking oven after sieving and heat-treat, thermal treatment temp is 105-115 DEG C, and the time is 5-8h;
S2, alum is put into retort furnace calcine, calcining temperature is 600-650 DEG C, and calcination time is 0.8-1.3h, is cooled to grinding after room temperature, sieving for standby; Rhombspar is put into retort furnace calcine, calcining temperature is 700-800 DEG C, and calcination time is 1-1.5h, is cooled to grinding, sieving for standby after room temperature;
The rhombspar after calcining in the alum in calcium hydroxide, blast-furnace slag, S2 after calcining, S2 is added in S3, fluorgypsum in S1 after thermal treatment, stir, standing 10-20h carries out a chemical modification, and then 250-300 DEG C of calcining, calcination time is 0.5-1.5h; Wherein, the rhombspar after calcining in the alum in 1-1.8 part calcium hydroxide, 1-2 part blast-furnace slag, 1-1.5 part S2 after calcining, 0.5-0.8 part S2 is added in the fluorgypsum by weight after every 100 parts of thermal treatments;
Add flyash in S4, fluorgypsum in S3 after calcining, corn straw modification fiber, wilkinite carry out secondary chemical modification; Wherein, 0.5-0.8 part flyash, 0.5-0.8 part corn straw modification fiber, 1-1.2 part wilkinite is added in the fluorgypsum by weight after every 100 parts of calcinings; Described corn straw modification fiber is Modification of Styrene-Acrylate Emulsion corn stalk fiber;
S5, the fluorgypsum obtained is put into curing field maintenance appear on the scene after 10 days in S4.
2. the method for modifying of fluorgypsum according to claim 1, is characterized in that, in S1, thermal treatment temp is 110-113 DEG C, and the time is 6-7h.
3. the method for modifying of fluorgypsum according to claim 2, is characterized in that, in S1, thermal treatment temp is 112 DEG C, and the time is 6.3h.
4. the method for modifying of the fluorgypsum according to any one of claim 1-3, is characterized in that, in S3, after the fluorgypsum in S1 after thermal treatment carries out a chemical modification, 285-295 DEG C of calcining, calcination time is 0.8-1.2h.
5. the method for modifying of fluorgypsum according to claim 4, is characterized in that, in S3, after the fluorgypsum in S1 after thermal treatment carries out a chemical modification, 290 DEG C of calcinings, calcination time is 1.0h.
6. the method for modifying of the fluorgypsum according to any one of claim 1-3, it is characterized in that, in S3, in a chemical modification, in the fluorgypsum by weight after every 100 parts of thermal treatments, add the rhombspar after calcining in the alum in 1.2-1.6 part calcium hydroxide, 1.5-1.7 part blast-furnace slag, 1.2-1.3 part S2 after calcining, 0.6-0.65 part S2.
7. the method for modifying of fluorgypsum according to claim 6, it is characterized in that, in S3, in a chemical modification, in the fluorgypsum by weight after every 100 parts of thermal treatments, add the rhombspar after calcining in the alum in 1.4 parts of calcium hydroxides, 1.6 parts of blast-furnace slags, 1.25 parts of S2 after calcining, 0.63 part of S2.
8. the method for modifying of the fluorgypsum according to any one of claim 1-3, it is characterized in that, in S4, in secondary chemical modification, in the fluorgypsum by weight after every 100 parts of calcinings, add 0.6-0.68 part flyash, 0.6-0.7 part corn straw modification fiber, 1.1-1.15 part wilkinite.
9. the method for modifying of fluorgypsum according to claim 8, it is characterized in that, in S4, in secondary chemical modification, in the fluorgypsum by weight after every 100 parts of calcinings, add 0.65 part of flyash, 0.68 part of corn straw modification fiber, 1.13 parts of wilkinites.
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| CN107915464A (en) * | 2017-11-30 | 2018-04-17 | 明光市裕阳新材料有限公司 | A kind of antibacterial light cellular partition board and preparation method thereof |
| CN115073112B (en) * | 2022-06-10 | 2023-06-30 | 四川方大新型建材科技开发有限责任公司 | Gypsum-based self-leveling mortar and preparation method thereof |
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Address after: 242310 Ningguo Xuancheng Anhui port town industrial concentration area Patentee after: Jinyang hi tech material Limited by Share Ltd Address before: 242310 provincial eco industrial park, port town, Xuancheng, Ningguo, Anhui Patentee before: Anhui Jinyang Fluorine Chemicals Co., Ltd. |