CN104176957A - Method for modifying fluorine gypsum by using redispersible latex powder - Google Patents
Method for modifying fluorine gypsum by using redispersible latex powder Download PDFInfo
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- CN104176957A CN104176957A CN201410390599.4A CN201410390599A CN104176957A CN 104176957 A CN104176957 A CN 104176957A CN 201410390599 A CN201410390599 A CN 201410390599A CN 104176957 A CN104176957 A CN 104176957A
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Abstract
The invention discloses a method for modifying fluorine gypsum by using redispersible latex powder. The method comprises the following steps: grinding, crushing and sieving fluorine gypsum, and then performing heat treatment at 135-160 DEG C for 4-6 hours; adding calcium hydroxide, alum, phosphorus gypsum and bauxite into fluorine gypsum which is subjected to heat treatment so as to perform primary chemical modification; adding the redispersible latex powder, pulverized fuel ash, cement, corn straw fiber, wheat straw fiber, polyvinyl alcohol, a rosin emulsion and sodium citrate into fluorine gypsum which is subjected to primary chemical modification so as to perform secondary chemical modification, wherein the redispersible latex powder is polyacrylate redispersible latex powder, and is prepared through the following steps: preparing an initial emulsion from ammonium chloride, ammonium persulfate, sodium dodecyl benzene sulfonate, methyl methacrylate and butyl acrylate, then adding calcium hydroxide and polyvinyl alcohol, and performing spray drying. The fluorine gypsum modified by the method disclosed by the invention is short in coagulation time and high in hydration and hardening strength; meanwhile, by adopting the method disclosed by the invention, the fluorine gypsum can be changed into treasure from waste.
Description
Technical field
The present invention relates to gypsum technical field, relate in particular to a kind of method of redispersable latex powder modification fluorgypsum.
Background technology
Fluorgypsum is the main byproduct 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.Every production 1t hydrofluoric acid generates the anhydrous fluorgypsum of about 3.6t.The main component of fluorgypsum is calcium sulfate, and contains partially fluorinated calcium and other fluorochemicals, and H sometimes
2sO
4content is very high, makes the fluorgypsum of discharging be acid, belongs to severe corrosive poisonous and harmful refuse, and the fluorgypsum that does not add processing can not directly be put and abandon, and is also difficult to be utilized.Because fluorgypsum solubleness is lower and dissolution rate is slow, time of coagulation is very long again, and hydration and hardening body intensity is very little, these drawbacks limit its application.At present, except part fluorgypsum is utilized, most of as general solid waste, stored up, land occupation not only, objectionable impurities wherein also can produce and pollute water body simultaneously, and physical environment is produced and threatened.Therefore, the properties-correcting agent that How to choose is suitable carries out modification to fluorgypsum, solves the problem that fluorgypsum history is stored up, and it is turned waste into wealth, and the comprehensive utilization that realizes gypsum resource is a very urgent problem.
Summary of the invention
A kind of method that the present invention proposes redispersable latex powder modification fluorgypsum, by the fluorgypsum after the method modification, time of coagulation is short, and hydration and hardening intensity is high, and fluorgypsum is turned waste into wealth.
A kind of method that the present invention proposes redispersable latex powder modification fluorgypsum, comprises the following steps:
S1, fluorgypsum is ground, after sieving, heat-treat, thermal treatment temp is 135-160 ℃, and heat treatment time is 4-6h;
S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add 3-5 part calcium hydroxide, 0.5-1.5 part alum, 0.5-2 part phosphogypsum, 1-3 part bauxite by weight, stir, standing 15-30h carries out chemical modification one time;
S3, in the fluorgypsum after 100 parts of chemical modifications, add 5-8 part redispersable latex powder, 0.5-1.3 part flyash, 0.2-1.5 part cement, 0.5-2.5 part corn stalk fiber, 0.5-1.5 part wheat stalk fiber, 0.2-1 part polyvinyl alcohol, 0.1-0.5 part rosin milk, 0.2-0.7 part Trisodium Citrate to carry out secondary chemical modification by weight;
Redispersable latex powder is that the preparation process of polyacrylate(s) redispersable latex powder is as follows:
A, in 100 parts of water, add successively 0.2-0.4 part ammonium chloride, 0.5-1.2 part ammonium persulphate and 0.5-1.0 part Sodium dodecylbenzene sulfonate to be heated to 40-55 ℃ by weight, after stirring 20-40min, add 25-35 part methyl methacrylate and 30-40 part butyl acrylate, be warming up to 85-95 ℃, stir insulation 120-220min, utilize 50-80min to drip after solution A, at 80-100 ℃, stir insulation 120-250min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 30-45 part methyl methacrylate and 10-20 part butyl acrylate;
In B, the colostric fluid that obtains, drip the calcium hydroxide aqueous solution that massfraction is 6-10wt% in A, adding distilled water to regulate pH is 8-10, then add the aqueous solution that contains 1-3 part polyvinyl alcohol, after stirring, send into the spray-dryer dry described redispersable latex powder that obtains of spraying; In spray-drying process, feeding rate is 10-18ml/min, and the inlet temperature of spray-dryer is 140-160 ℃, and temperature out is 62-80 ℃, and rotating speed is 20000-23000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification at 100-150 ℃ of insulation 5-6h, after cooling, grind.
Preferably, in S1, thermal treatment temp is 145-155 ℃, and heat treatment time is 4.5-5.2h.
Preferably, in S1, thermal treatment temp is 148 ℃, and heat treatment time is 5.0h.
Preferably, in S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add by weight 3.8-4.2 part calcium hydroxide, 0.8-1.2 part alum, 1.2-1.5 part phosphogypsum, 1.8-2.3 part bauxite, stir, standing 18-22h.
Preferably, in S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add by weight 4.1 parts of calcium hydroxides, 1.1 parts of alum, 1.4 parts of phosphogypsums, 2.1 parts of bauxite, stir, standing 20h.
Preferably, in S3, in the fluorgypsum after 100 parts of chemical modifications, add by weight 6-7.2 part redispersable latex powder, 0.8-1.2 part flyash, 0.7-1.2 part cement, 1.5-1.8 part corn stalk fiber, 0.8-1.3 part wheat stalk fiber, 0.4-0.8 part polyvinyl alcohol, 0.2-0.35 part rosin milk, 0.4-0.6 part Trisodium Citrate to carry out secondary chemical modification.
Preferably, in S3, in the fluorgypsum after 100 parts of chemical modifications, add by weight 7 parts of redispersable latex powders, 1.0 parts of flyash, 0.9 part of cement, 1.6 parts of corn stalk fibers, 1.2 parts of wheat stalk fibers, 0.6 part of polyvinyl alcohol, 0.27 part of rosin milk, 0.5 part of Trisodium Citrate to carry out secondary chemical modification.
Preferably, in S3, in steps A, in 100 parts of water, add successively by weight 0.3-0.35 part ammonium chloride, 0.7-1.0 part ammonium persulphate and 0.6-0.8 part Sodium dodecylbenzene sulfonate to be heated to 45-50 ℃, after stirring 30-35min, add 30-32 part methyl methacrylate and 33-36 part butyl acrylate, be warming up to 90-93 ℃, stir insulation 150-175min, utilize 60-75min to drip after solution A, at 90-95 ℃, stir insulation 170-190min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 35-42 part methyl methacrylate and 12-16 part butyl acrylate.
Preferably, in S3, in steps A, in 100 parts of water, add successively by weight 0.33 part of ammonium chloride, 0.8 part of ammonium persulphate and 0.75 part of Sodium dodecylbenzene sulfonate to be heated to 48 ℃, after stirring 33min, add 31 parts of methyl methacrylates and 35 parts of butyl acrylates, be warming up to 92 ℃, stir insulation 169min, utilize 70min to drip after solution A, at 92 ℃, stir insulation 180min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 38 parts of methyl methacrylates and 15 parts of butyl acrylates.
Preferably, in S3, in spray-drying process described in step B, feeding rate is 15-16ml/min, and the inlet temperature of spray-dryer is 132-134 ℃, and temperature out is 65-68 ℃, and rotating speed is 21000-22000r/min.
In the method for redispersable latex powder modification fluorgypsum of the present invention, adopted and ground and thermal treatment, change, destroyed the crystal lattice of fluorgypsum after modification, its lattice distortion and defect have been increased, increased the irregularity of its specific surface area and surface tissue, improve the hydration activity of fluorgypsum after modification, promoted the hardening of fluorgypsum after modification, adopt chemical modification twice, in a chemical modification, added calcium hydroxide, bauxite, alum, neutralized fluorgypsum, improved the intensity of fluorgypsum after modification, in secondary chemical modification, added redispersable latex powder, particle in redispersable latex powder can deposit or condense upon the fluorgypsum surface after aquation and form polymeric film, along with completing of hydration, film can form inierpeneirating network structure and be filled in the pore of fluorgypsum, stop the generation of hallrcuts, improved the bending strength of fluorgypsum after modification, ultimate compression strength and and different substrate materials between adhesive tensile resistance intensity, improved the water tolerance of fluorgypsum after modification simultaneously, added wheat stalk fiber and corn stalk fiber, fibrous bundle is wherein evenly distributed in fluorgypsum, and each fibrous bundle is respectively to distribution, has improved folding strength and the ultimate compression strength of fluorgypsum after modification, added polyvinyl alcohol, it can shrink and form gel, fluorgypsum after modification is after Jia Shui mixes, polyvinyl alcohol can be dispersed in after modification in fluorgypsum slurry, its can fade away along with the consumption of moisture in fluorgypsum hardenite and evaporation, formation has the regid gel of certain toughness, polyvinyl alcohol gel forms gradually the irregular nethike embrane with resistance effect in fluorgypsum hardenite, fill the hole of fluorgypsum hardenite, improve the degree of compactness of fluorgypsum hardenite, even can seal capillary porosity duct completely, block penetrating passage, improve the hardness of fluorgypsum hardenite, improve the water tolerance of stone fluorine cream hardenite.
In the method for redispersable latex powder modification fluorgypsum of the present invention, selected suitable properties-correcting agent, controlled the content of each composition in properties-correcting agent, optimized the modified technique of fluorgypsum, adopt the fluorgypsum of the method modification short time of coagulation, after hydration and hardening, there is excellent tensile strength, bending strength, 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 the present invention is described, rather than for the present invention is limited, and any modification of making on basis of the present invention, is equal to replacement etc. all in protection scope of the present invention.
Embodiment 1
The method of redispersable latex powder modification fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum is ground, after sieving, heat-treat, thermal treatment temp is 148 ℃, and heat treatment time is 5.0h;
S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add 4.1 parts of calcium hydroxides, 1.1 parts of alum, 1.4 parts of phosphogypsums, 2.1 parts of bauxite by weight, stir, standing 20h carries out chemical modification one time;
S3, in the fluorgypsum after 100 parts of chemical modifications, add 7 parts of redispersable latex powders, 1.0 parts of flyash, 0.9 part of cement, 1.6 parts of corn stalk fibers, 1.2 parts of wheat stalk fibers, 0.6 part of polyvinyl alcohol, 0.27 part of rosin milk, 0.5 part of Trisodium Citrate to carry out secondary chemical modification by weight;
Wherein, described redispersable latex powder is that the preparation process of polyacrylate(s) redispersable latex powder is specific as follows:
A, in 100 parts of water, add successively 0.33 part of ammonium chloride, 0.5 part of ammonium persulphate and 0.75 part of Sodium dodecylbenzene sulfonate to be heated to 48 ℃ by weight, after stirring 33min, add 31 parts of methyl methacrylates and 35 parts of butyl acrylates, be warming up to 92 ℃, stir insulation 169min, utilize 70min to drip after solution A, at 92 ℃, stir insulation 180min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 38 parts of methyl methacrylates and 15 parts of butyl acrylates;
In B, the colostric fluid that obtains, drip the calcium hydroxide aqueous solution that massfraction is 7wt% in A, adding distilled water to regulate pH is 9, then add the aqueous solution that contains 2 parts of polyvinyl alcohol, after stirring, send into the spray-dryer dry described redispersable latex powder that obtains of spraying; In spray-drying process, feeding rate is 15ml/min, and the inlet temperature of spray-dryer is 153 ℃, and temperature out is 66 ℃, and rotating speed is 21500r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification at 142 ℃ of insulation 5.2h, after cooling, grind.
Embodiment 2
The method of redispersable latex powder modification fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum is ground, after sieving, heat-treat, thermal treatment temp is 135 ℃, and heat treatment time is 6h;
S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add 5 parts of calcium hydroxides, 1.5 parts of alum, 0.5 part of phosphogypsum, 3 parts of bauxite by weight, stir, standing 15h carries out chemical modification one time;
S3, in the fluorgypsum after 100 parts of chemical modifications, add 5 parts of redispersable latex powders, 0.5 part of flyash, 1.5 parts of cement, 2.5 parts of corn stalk fibers, 0.5 part of wheat stalk fiber, 0.2 part of polyvinyl alcohol, 0.1 part of rosin milk, 0.7 part of Trisodium Citrate to carry out secondary chemical modification by weight;
Wherein, described redispersable latex powder is that the preparation process of polyacrylate(s) redispersable latex powder is specific as follows:
A, in 100 parts of water, add successively 0.4 part of ammonium chloride, 1.2 parts of ammonium persulphates and 1.0 parts of Sodium dodecylbenzene sulfonatees to be heated to 40 ℃ by weight, after stirring 40min, add 25 parts of methyl methacrylates and 30 parts of butyl acrylates, be warming up to 85 ℃, stir insulation 220min, utilize 50min to drip after solution A, at 100 ℃, stir insulation 120min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 30 parts of methyl methacrylates and 20 parts of butyl acrylates;
In B, the colostric fluid that obtains, drip the calcium hydroxide aqueous solution that massfraction is 10wt% in A, adding distilled water to regulate pH is 8, then add the aqueous solution that contains 3 parts of polyvinyl alcohol, after stirring, send into the spray-dryer dry described redispersable latex powder that obtains of spraying; In spray-drying process, feeding rate is 18ml/min, and the inlet temperature of spray-dryer is 160 ℃, and temperature out is 62 ℃, and rotating speed is 20000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification at 150 ℃ of insulation 5h, after cooling, grind.
Embodiment 3
The method of redispersable latex powder modification fluorgypsum of the present invention, comprises the following steps:
S1, fluorgypsum is ground, after sieving, heat-treat, thermal treatment temp is 160 ℃, and heat treatment time is 4h;
S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add 3 parts of calcium hydroxides, 1.5 parts of alum, 2 parts of phosphogypsums, 1 part of bauxite by weight, stir, standing 30h carries out chemical modification one time;
S3, in the fluorgypsum after 100 parts of chemical modifications, add 8 parts of redispersable latex powders, 1.3 parts of flyash, 0.2 part of cement, 0.5 part of corn stalk fiber, 1.5 parts of wheat stalk fibers, 1 part of polyvinyl alcohol, 0.5 part of rosin milk, 0.2 part of Trisodium Citrate to carry out secondary chemical modification by weight;
Wherein, described redispersable latex powder is that the preparation process of polyacrylate(s) redispersable latex powder is specific as follows:
A, in 100 parts of water, add successively 0.2 part of ammonium chloride, 0.5 part of ammonium persulphate and 0.5 part of Sodium dodecylbenzene sulfonate to be heated to 55 ℃ by weight, after stirring 20min, add 35 parts of methyl methacrylates and 40 parts of butyl acrylates, be warming up to 95 ℃, stir insulation 120min, utilize 80min to drip after solution A, at 80 ℃, stir insulation 250min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 45 parts of methyl methacrylates and 10 parts of butyl acrylates;
In B, the colostric fluid that obtains, drip the calcium hydroxide aqueous solution that massfraction is 6wt% in A, adding distilled water to regulate pH is 10, then add the aqueous solution that contains 1 part of polyvinyl alcohol, after stirring, send into the spray-dryer dry described redispersable latex powder that obtains of spraying; In spray-drying process, feeding rate is 10ml/min, and the inlet temperature of spray-dryer is 140 ℃, and temperature out is 80 ℃, and rotating speed is 23000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification at 100 ℃ of insulation 6h, after cooling, grind.
Claims (10)
1. a method for redispersable latex powder modification fluorgypsum, is characterized in that, comprises the following steps:
S1, fluorgypsum is ground, after sieving, heat-treat, thermal treatment temp is 135-160 ℃, and heat treatment time is 4-6h;
S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add 3-5 part calcium hydroxide, 0.5-1.5 part alum, 0.5-2 part phosphogypsum, 1-3 part bauxite by weight, stir, standing 15-30h carries out chemical modification one time;
S3, in the fluorgypsum after 100 parts of chemical modifications, add 5-8 part redispersable latex powder, 0.5-1.3 part flyash, 0.2-1.5 part cement, 0.5-2.5 part corn stalk fiber, 0.5-1.5 part wheat stalk fiber, 0.2-1 part polyvinyl alcohol, 0.1-0.5 part rosin milk, 0.2-0.7 part Trisodium Citrate to carry out secondary chemical modification by weight;
Redispersable latex powder is that the preparation process of polyacrylate(s) redispersable latex powder is as follows:
A, in 100 parts of water, add successively 0.2-0.4 part ammonium chloride, 0.5-1.2 part ammonium persulphate and 0.5-1.0 part Sodium dodecylbenzene sulfonate to be heated to 40-55 ℃ by weight, after stirring 20-40min, add 25-35 part methyl methacrylate and 30-40 part butyl acrylate, be warming up to 85-95 ℃, stir insulation 120-220min, utilize 50-80min to drip after solution A, at 80-100 ℃, stir insulation 120-250min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 30-45 part methyl methacrylate and 10-20 part butyl acrylate;
In B, the colostric fluid that obtains, drip the calcium hydroxide aqueous solution that massfraction is 6-10wt% in A, adding distilled water to regulate pH is 8-10, then add the aqueous solution that contains 1-3 part polyvinyl alcohol, after stirring, send into the spray-dryer dry described redispersable latex powder that obtains of spraying; In spray-drying process, feeding rate is 10-18ml/min, and the inlet temperature of spray-dryer is 140-160 ℃, and temperature out is 62-80 ℃, and rotating speed is 20000-23000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification at 100-150 ℃ of insulation 5-6h, after cooling, grind.
2. the method for redispersable latex powder modification fluorgypsum according to claim 1, is characterized in that, in S1, thermal treatment temp is 145-155 ℃, and heat treatment time is 4.5-5.2h.
3. the method for redispersable latex powder modification fluorgypsum according to claim 2, is characterized in that, in S1, thermal treatment temp is 148 ℃, and heat treatment time is 5.0h.
4. according to the method for the redispersable latex powder modification fluorgypsum described in any one in claim 1-3, it is characterized in that, in S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add by weight 3.8-4.2 part calcium hydroxide, 0.8-1.2 part alum, 1.2-1.5 part phosphogypsum, 1.8-2.3 part bauxite, stir, standing 18-22h.
5. the method for redispersable latex powder modification fluorgypsum according to claim 4, it is characterized in that, in S2, in 100 parts of S1, in the fluorgypsum after thermal treatment, add by weight 4.1 parts of calcium hydroxides, 1.1 parts of alum, 1.4 parts of phosphogypsums, 2.1 parts of bauxite, stir, standing 20h.
6. according to the method for the redispersable latex powder modification fluorgypsum described in any one in claim 1-5, it is characterized in that, in S3, in the fluorgypsum after 100 parts of chemical modifications, add by weight 6-7.2 part redispersable latex powder, 0.8-1.2 part flyash, 0.7-1.2 part cement, 1.5-1.8 part corn stalk fiber, 0.8-1.3 part wheat stalk fiber, 0.4-0.8 part polyvinyl alcohol, 0.2-0.35 part rosin milk, 0.4-0.6 part Trisodium Citrate to carry out secondary chemical modification.
7. the method for redispersable latex powder modification fluorgypsum according to claim 6, it is characterized in that, in S3, in the fluorgypsum after 100 parts of chemical modifications, add by weight 7 parts of redispersable latex powders, 1.0 parts of flyash, 0.9 part of cement, 1.6 parts of corn stalk fibers, 1.2 parts of wheat stalk fibers, 0.6 part of polyvinyl alcohol, 0.27 part of rosin milk, 0.5 part of Trisodium Citrate to carry out secondary chemical modification.
8. according to the method for the redispersable latex powder modification fluorgypsum described in any one in claim 1-7, it is characterized in that, in S3, in steps A, in 100 parts of water, add successively by weight 0.3-0.35 part ammonium chloride, 0.7-1.0 part ammonium persulphate and 0.6-0.8 part Sodium dodecylbenzene sulfonate are heated to 45-50 ℃, after stirring 30-35min, add 30-32 part methyl methacrylate and 33-36 part butyl acrylate, be warming up to 90-93 ℃, stir insulation 150-175min, utilize 60-75min to drip after solution A, at 90-95 ℃, stir insulation 170-190min, filtration obtains colostric fluid, wherein, described solution A is the aqueous solution that contains 35-42 part methyl methacrylate and 12-16 part butyl acrylate.
9. the method for redispersable latex powder modification fluorgypsum according to claim 8, it is characterized in that, in S3, in steps A, in 100 parts of water, add successively by weight 0.33 part of ammonium chloride, 0.8 part of ammonium persulphate and 0.75 part of Sodium dodecylbenzene sulfonate to be heated to 48 ℃, after stirring 33min, add 31 parts of methyl methacrylates and 35 parts of butyl acrylates, be warming up to 92 ℃, stir insulation 169min, utilize 70min to drip after solution A, at 92 ℃, stir insulation 180min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution that contains 38 parts of methyl methacrylates and 15 parts of butyl acrylates.
10. according to the method for the redispersable latex powder modification fluorgypsum described in any one in claim 1-9, it is characterized in that, in S3, in spray-drying process described in step B, feeding rate is 15-16ml/min, the inlet temperature of spray-dryer is 150-155 ℃, and temperature out is 65-68 ℃, and rotating speed is 21000-22000r/min.
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CN110760148A (en) * | 2019-10-10 | 2020-02-07 | 江苏兆佳建材科技有限公司 | Preparation method of modified redispersible latex powder |
CN113845320A (en) * | 2021-09-23 | 2021-12-28 | 中建材创新科技研究院有限公司 | Plaster of paris and preparation method thereof |
CN113845320B (en) * | 2021-09-23 | 2022-10-18 | 中建材创新科技研究院有限公司 | Plaster of paris and preparation method thereof |
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