CN104176957B - A kind of method of redispersable latex powder modification fluorgypsum - Google Patents
A kind of method of redispersable latex powder modification fluorgypsum Download PDFInfo
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- CN104176957B CN104176957B CN201410390599.4A CN201410390599A CN104176957B CN 104176957 B CN104176957 B CN 104176957B CN 201410390599 A CN201410390599 A CN 201410390599A CN 104176957 B CN104176957 B CN 104176957B
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Abstract
The invention discloses a kind of method of redispersable latex powder modification fluorgypsum, comprising: at 135-160 DEG C of thermal treatment 4-6h after fluorgypsum grinds and sieves; Add calcium hydroxide in fluorgypsum after heat treatment, alum, phosphogypsum, bauxite carries out a chemical modification; Add redispersable latex powder in fluorgypsum after a chemical modification, flyash, cement, corn stalk fiber, wheat stalk fiber, polyvinyl alcohol, rosin milk, Trisodium Citrate carry out secondary chemical modification; Described redispersable latex powder is polyacrylate(s) redispersable latex powder, by ammonium chloride, ammonium persulphate and Sodium dodecylbenzene sulfonate, methyl methacrylate, butyl acrylate, prepare colostric fluid, then add calcium hydroxide and polyvinyl alcohol spraying dry obtains.The fluorgypsum that the method for the invention is modified, time of coagulation is short, and hydration and hardening intensity is high; The method makes fluorgypsum turn waste into wealth simultaneously.
Description
Technical field
The present invention relates to gypsum technical field, particularly relate to a kind of method of redispersable latex powder modification 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 select suitable properties-correcting agent to carry out modification to fluorgypsum, solve the problem that fluorgypsum history is stored 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 redispersable latex powder modification fluorgypsum, by the fluorgypsum that the method is modified, time of coagulation is short, and hydration and hardening intensity is high, and fluorgypsum is turned waste into wealth.
The present invention proposes a kind of method of redispersable latex powder modification fluorgypsum, comprise the following steps:
S1, ground by fluorgypsum, heat-treat after sieving, thermal treatment temp is 135-160 DEG C, and heat treatment time is 4-6h;
Add 3-5 part calcium hydroxide, 0.5-1.5 part alum, 0.5-2 part phosphogypsum, 1-3 part bauxite in S2, fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, standing 15-30h carries out a chemical modification;
Add 5-8 part redispersable latex powder in S3, fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification;
Redispersable latex powder is that the preparation process of polyacrylate(s) redispersable latex powder is as follows:
A, in 100 parts of water, add 0.2-0.4 part ammonium chloride, 0.5-1.2 part ammonium persulphate and 0.5-1.0 part Sodium dodecylbenzene sulfonate successively by weight and be heated to 40-55 DEG C, 25-35 part methyl methacrylate and 30-40 part butyl acrylate is added after stirring 20-40min, be warming up to 85-95 DEG C, stir insulation 120-220min, after utilizing 50-80min to drip solution A, at 80-100 DEG C, stir insulation 120-250min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 30-45 part methyl methacrylate and 10-20 part butyl acrylate;
The calcium hydroxide aqueous solution that massfraction is 6-10wt% is dripped in B, the colostric fluid that obtains in A, adding distilled water regulates pH to be 8-10, then add the aqueous solution containing 1-3 part polyvinyl alcohol, send into spray-dryer after stirring and carry out spraying dry and obtain described redispersable latex powder; In spray-drying process, feeding rate is 10-18ml/min, and the inlet temperature of spray-dryer is 140-160 DEG C, and temperature out is 62-80 DEG C, and rotating speed is 20000-23000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification 100-150 DEG C insulation 5-6h, cooling after grinding.
Preferably, in S1, thermal treatment temp is 145-155 DEG C, and heat treatment time is 4.5-5.2h.
Preferably, in S1, thermal treatment temp is 148 DEG C, and heat treatment time is 5.0h.
Preferably, in S2, add 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 in the fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, leave standstill 18-22h.
Preferably, in S2, add 4.1 parts of calcium hydroxides, 1.1 parts of alum, 1.4 parts of phosphogypsums, 2.1 parts of bauxite in the fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, leave standstill 20h.
Preferably, in S3, add 6-7.2 part redispersable latex powder in the fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification.
Preferably, in S3, add 7 parts of redispersable latex powders in the fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification.
Preferably, in S3, in step, in 100 parts of water, add 0.3-0.35 part ammonium chloride, 0.7-1.0 part ammonium persulphate and 0.6-0.8 part Sodium dodecylbenzene sulfonate be by weight successively heated to 45-50 DEG C, add 30-32 part methyl methacrylate and 33-36 part butyl acrylate after stirring 30-35min, be warming up to 90-93 DEG C, stir insulation 150-175min, after utilizing 60-75min to drip solution A, at 90-95 DEG C, stir insulation 170-190min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 35-42 part methyl methacrylate and 12-16 part butyl acrylate.
Preferably, in S3, in step, in 100 parts of water, add 0.33 part of ammonium chloride, 0.8 part of ammonium persulphate and 0.75 part of Sodium dodecylbenzene sulfonate be by weight successively heated to 48 DEG C, add 31 parts of methyl methacrylates and 35 parts of butyl acrylates after stirring 33min, be warming up to 92 DEG C, stir insulation 169min, after utilizing 70min to drip solution A, at 92 DEG C, stir insulation 180min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 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 DEG C, and temperature out is 65-68 DEG C, and rotating speed is 21000-22000r/min.
In the method for redispersable latex powder modification fluorgypsum of the present invention, have employed and grind and thermal treatment, change, destroy the crystal lattice of modified fluorgypsum, add 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 modification, in a chemical modification, with the addition of calcium hydroxide, bauxite, alum, neutralized fluorgypsum, improve the intensity of modified fluorgypsum, in secondary chemical modification, with the addition of redispersable latex powder, fluorgypsum surface after particle in redispersable latex powder can deposit or condense upon aquation also forms 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, improve the bending strength of modified fluorgypsum, ultimate compression strength and and different substrate materials between adhesive tensile resistance intensity, improve the water tolerance of modified fluorgypsum simultaneously, with the addition of wheat stalk fiber and corn stalk fiber, fibrous bundle is wherein evenly distributed in fluorgypsum, and each fibrous bundle is respectively to distribution, improves folding strength and the ultimate compression strength of modified fluorgypsum, with the addition of polyvinyl alcohol, it can shrink and form gel, modified fluorgypsum is after adding water and mixing, polyvinyl alcohol can in the dispersed slurry of fluorgypsum after modification, it can fade away along with the consumption of moisture in fluorgypsum hardenite and evaporation, form the regid gel with certain toughness, polyvinyl alcohol gel forms the irregular nethike embrane with resistance effect gradually in fluorgypsum hardenite, fill the hole of fluorgypsum hardenite, improve the degree of compactness of fluorgypsum hardenite, even can close 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, have selected suitable properties-correcting agent, control the content of each composition in properties-correcting agent, optimize the modified technique of fluorgypsum, adopt the fluorgypsum of the method modification short for time of coagulation, there is after hydration and hardening 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 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 redispersable latex powder modification fluorgypsum of the present invention, comprises the following steps:
S1, ground by fluorgypsum, heat-treat after sieving, thermal treatment temp is 148 DEG C, and heat treatment time is 5.0h;
Add 4.1 parts of calcium hydroxides, 1.1 parts of alum, 1.4 parts of phosphogypsums, 2.1 parts of bauxite in S2, fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, standing 20h carries out a chemical modification;
Add 7 parts of redispersable latex powders in S3, fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification;
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 0.33 part of ammonium chloride, 0.5 part of ammonium persulphate and 0.75 part of Sodium dodecylbenzene sulfonate successively by weight and be heated to 48 DEG C, 31 parts of methyl methacrylates and 35 parts of butyl acrylates are added after stirring 33min, be warming up to 92 DEG C, stir insulation 169min, after utilizing 70min to drip solution A, at 92 DEG C, stir insulation 180min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 38 parts of methyl methacrylates and 15 parts of butyl acrylates;
The calcium hydroxide aqueous solution that massfraction is 7wt% is dripped in B, the colostric fluid that obtains in A, adding distilled water regulates pH to be 9, then add the aqueous solution containing 2 parts of polyvinyl alcohol, send into spray-dryer after stirring and carry out spraying dry and obtain described redispersable latex powder; In spray-drying process, feeding rate is 15ml/min, and the inlet temperature of spray-dryer is 153 DEG C, and temperature out is 66 DEG C, and rotating speed is 21500r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification 142 DEG C insulation 5.2h, cooling after grinding.
Embodiment 2
The method of redispersable latex powder modification fluorgypsum of the present invention, comprises the following steps:
S1, ground by fluorgypsum, heat-treat after sieving, thermal treatment temp is 135 DEG C, and heat treatment time is 6h;
Add 5 parts of calcium hydroxides, 1.5 parts of alum, 0.5 part of phosphogypsum, 3 parts of bauxite in S2, fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, standing 15h carries out a chemical modification;
Add 5 parts of redispersable latex powders in S3, fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification;
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 0.4 part of ammonium chloride, 1.2 parts of ammonium persulphates and 1.0 parts of Sodium dodecylbenzene sulfonatees successively by weight and be heated to 40 DEG C, 25 parts of methyl methacrylates and 30 parts of butyl acrylates are added after stirring 40min, be warming up to 85 DEG C, stir insulation 220min, after utilizing 50min to drip solution A, at 100 DEG C, stir insulation 120min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 30 parts of methyl methacrylates and 20 parts of butyl acrylates;
The calcium hydroxide aqueous solution that massfraction is 10wt% is dripped in B, the colostric fluid that obtains in A, adding distilled water regulates pH to be 8, then add the aqueous solution containing 3 parts of polyvinyl alcohol, send into spray-dryer after stirring and carry out spraying dry and obtain described redispersable latex powder; In spray-drying process, feeding rate is 18ml/min, and the inlet temperature of spray-dryer is 160 DEG C, and temperature out is 62 DEG C, and rotating speed is 20000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification 150 DEG C insulation 5h, cooling after grinding.
Embodiment 3
The method of redispersable latex powder modification fluorgypsum of the present invention, comprises the following steps:
S1, ground by fluorgypsum, heat-treat after sieving, thermal treatment temp is 160 DEG C, and heat treatment time is 4h;
Add 3 parts of calcium hydroxides, 1.5 parts of alum, 2 parts of phosphogypsums, 1 part of bauxite in S2, fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, standing 30h carries out a chemical modification;
Add 8 parts of redispersable latex powders in S3, fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification;
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 0.2 part of ammonium chloride, 0.5 part of ammonium persulphate and 0.5 part of Sodium dodecylbenzene sulfonate successively by weight and be heated to 55 DEG C, 35 parts of methyl methacrylates and 40 parts of butyl acrylates are added after stirring 20min, be warming up to 95 DEG C, stir insulation 120min, after utilizing 80min to drip solution A, at 80 DEG C, stir insulation 250min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 45 parts of methyl methacrylates and 10 parts of butyl acrylates;
The calcium hydroxide aqueous solution that massfraction is 6wt% is dripped in B, the colostric fluid that obtains in A, adding distilled water regulates pH to be 10, then add the aqueous solution containing 1 part of polyvinyl alcohol, send into spray-dryer after stirring and carry out spraying dry and obtain described redispersable latex powder; In spray-drying process, feeding rate is 10ml/min, and the inlet temperature of spray-dryer is 140 DEG C, and temperature out is 80 DEG C, and rotating speed is 23000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification 100 DEG C insulation 6h, cooling after grinding.
Claims (9)
1. a method for redispersable latex powder modification fluorgypsum, is characterized in that, comprises the following steps:
S1, ground by fluorgypsum, heat-treat after sieving, thermal treatment temp is 135-160 DEG C, and heat treatment time is 4-6h;
Add 3-5 part calcium hydroxide, 0.5-1.5 part alum, 0.5-2 part phosphogypsum, 1-3 part bauxite in S2, fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, standing 15-30h carries out a chemical modification;
Add 5-8 part redispersable latex powder in S3, fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification;
Redispersable latex powder is polyacrylate(s) redispersable latex powder, and its preparation process is as follows:
A, in 100 parts of water, add 0.2-0.4 part ammonium chloride, 0.5-1.2 part ammonium persulphate and 0.5-1.0 part Sodium dodecylbenzene sulfonate successively by weight and be heated to 40-55 DEG C, 25-35 part methyl methacrylate and 30-40 part butyl acrylate is added after stirring 20-40min, be warming up to 85-95 DEG C, stir insulation 120-220min, drip solution A, wherein, time for adding is 50-80min, at 80-100 DEG C, stir insulation 120-250min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 30-45 part methyl methacrylate and 10-20 part butyl acrylate;
The calcium hydroxide aqueous solution that massfraction is 6-10wt% is dripped in B, the colostric fluid that obtains in A, adding distilled water regulates pH to be 8-10, then add the aqueous solution containing 1-3 part polyvinyl alcohol, send into spray-dryer after stirring and carry out spraying dry and obtain described redispersable latex powder; In spray-drying process, feeding rate is 10-18ml/min, and the inlet temperature of spray-dryer is 140-160 DEG C, and temperature out is 62-80 DEG C, and rotating speed is 20000-23000r/min;
S4, by S3 through the fluorgypsum of secondary chemical modification 100-150 DEG C insulation 5-6h, cooling after grinding.
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 DEG C, 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 DEG C, and heat treatment time is 5.0h.
4. the method for the redispersable latex powder modification fluorgypsum according to any one of claim 1-3, it is characterized in that, in S2,3.8-4.2 part calcium hydroxide, 0.8-1.2 part alum, 1.2-1.5 part phosphogypsum, 1.8-2.3 part bauxite is added in fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, leave standstill 18-22h.
5. the method for redispersable latex powder modification fluorgypsum according to claim 4, it is characterized in that, in S2,4.1 parts of calcium hydroxides, 1.1 parts of alum, 1.4 parts of phosphogypsums, 2.1 parts of bauxite are added in fluorgypsum by weight in 100 parts of S1 after thermal treatment, stir, leave standstill 20h.
6. the method for the redispersable latex powder modification fluorgypsum according to any one of claim 1-3, it is characterized in that, in S3, add 6-7.2 part redispersable latex powder in the fluorgypsum by weight after 100 parts of chemical modifications, 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 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, add 7 parts of redispersable latex powders in the fluorgypsum by weight after 100 parts of chemical modifications, 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 carry out secondary chemical modification.
8. the method for the redispersable latex powder modification fluorgypsum according to any one of claim 1-3, it is characterized in that, in S3, in step, 0.3-0.35 part ammonium chloride is added successively by weight in 100 parts of water, 0.7-1.0 part ammonium persulphate and 0.6-0.8 part Sodium dodecylbenzene sulfonate are heated to 45-50 DEG C, 30-32 part methyl methacrylate and 33-36 part butyl acrylate is added after stirring 30-35min, be warming up to 90-93 DEG C, stir insulation 150-175min, drip solution A, wherein, time for adding is 60-75min, insulation 170-190min is stirred at 90-95 DEG C, filtration obtains colostric fluid, wherein, described solution A is the aqueous solution containing 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 step, in 100 parts of water, add 0.33 part of ammonium chloride, 0.8 part of ammonium persulphate and 0.75 part of Sodium dodecylbenzene sulfonate be by weight successively heated to 48 DEG C, 31 parts of methyl methacrylates and 35 parts of butyl acrylates are added after stirring 33min, be warming up to 92 DEG C, stir insulation 169min, drip solution A, wherein, time for adding is 70min, at 92 DEG C, stir insulation 180min, filter and obtain colostric fluid; Wherein, described solution A is the aqueous solution containing 38 parts of methyl methacrylates and 15 parts of butyl acrylates.
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