CN104671682A - Method for preparing hemihydrate gypsum gel material and gypsum products on line by using phosphogypsum at hot stage - Google Patents
Method for preparing hemihydrate gypsum gel material and gypsum products on line by using phosphogypsum at hot stage Download PDFInfo
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Abstract
The invention relates to a method for preparing a hemihydrate gypsum gel material and gypsum products on line by using phosphogypsum at a hot stage. The method comprises the following steps: 1) phosphogypsum hot-state on-line processing process: scrubbing phosphogypsum discharged on line by using a water scrubbing process in the presence of a modifier and dehydrating to obtain phosphogypsum slurry; 2) phosphogypsum hot-state on-line hydrothermal preparation process: sufficiently mixing the phosphogypsum slurry with an activity agent and a crystal modifier to form material slurry and carrying out normal-pressure dynamic heat preservation reaction on the slurry material; carrying out solid-liquid separation to obtain hemihydrate gypsum slurry, wherein the scrubbing solution can be recycled after being treated; and 3) on-line preparation process of the hemihydrate gypsum gel material: washing the hemihydrate gypsum slurry with hot water, filtering and drying to obtain hemihydrate gypsum powder; or on-line preparation process of the phosphogypsum products: washing the hemihydrate gypsum slurry, filtering and directly preparing into building blocks, gypsum boards and other products online. The method has the advantages that the flotation process of phosphogypsum ore is omitted and phosphogypsum generated by a phosphorus chemical industry production line can be directly subjected to a normal-pressure hydrothermal reaction.
Description
Technical field
The invention belongs to phosphogypsum is the field that gypsum plaster prepared by raw material, is specifically related to the method utilizing phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering.
Background technology
Gypsum is the main raw material of production gelling material and gypsum building products, and the preparation process of gypsum plaster mainly dihydrate gypsum thermal dehydration changes the process of different dehydrated gypsum phase into.After dihydrate gypsum is heated to certain temperature, gypsum loses partial crystallization water, obtains semi-hydrated gypsum, semi-hydrated gypsum is a kind of air hardening cementitious materials, have α and β two kinds of forms, the two is without essential distinction on microscopic appearance, but its macroscopic property has very big-difference.Alpha semi-hydrated gypsum is fine and close, complete, thick primary particle, and its hydration rate is fast, hydration heat is high, hardenite intensity is high, is referred to as high strength gypsum.Be applicable to modeling, sculpture and decoration and other high value added products.Beta-type semi-hydrated gypsum is then sheet, secondary paticle that is irregular, that be made up of tiny single crystal grain, and its water requirement is large, hydration rate slow, hardenite intensity is low, is referred to as plaster of Paris.Be widely used in the plastering of building field, plasterboard and other decorated articles.
Phosphogypsum is the throw out based on terra alba of discharging in Wet-process Phosphoric Acid Production process, is the major industry byproduct that phosphorous chemical industry enterprise produces.Under normal circumstances, 1 ton of P is produced
2o
54.5-5.5 ton phosphogypsum will be discharged.Because phosphogypsum is usually in acid, and containing impurity such as phosphorus, fluorine, organism, complex chemical composition, does not also utilize measure so far preferably.At present, the quantity discharged of China's phosphogypsum, more than 200,000,000 tons, adopts common measure of storing up to take a large amount of land resources.At present, the phosphogypsum stored up mainly is prepared the products such as cement setting retarder, building gypsum plaster, gypsum block by the domestic mode of phosphogypsum that utilizes.The method of phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and goods thereof, can make full use of heat energy when phosphogypsum discharges online, has saved cost of land and transportation cost that phosphogypsum stores up, has had wide Social benefit and economic benefit.
At present, the preparation method of αsemiwatergypsum adopts steam pressure or pressurization usually.Autoclave method: the product of 1.5 crystal water sloughed by dihydrate gypsum in saturation steam medium; Hydrothermal method is the product that 1.5 crystal water sloughed under hydrothermal conditions by dihydrate gypsum.The αsemiwatergypsum of current China is mainly produced under steam pressure or high pressure water heat condition with natural dihydrate gypsum, becomes that production capacity consumption is high, production cost is high.Constant pressure hydro-thermal legal system is adopted to have the feature of mild condition, energy-conserving and environment-protective for αsemiwatergypsum gelling material.
The large multiplex rotary kiln of β semi-hydrated gypsum and mechanical frying pan carry out high-temperature calcination to produce.Wherein, heating and calcining process is the key of producing β semi-hydrated gypsum.Utilize rotary kiln to prepare the technological process of β semi-hydrated gypsum as follows: dihydrate gypsum enters feed bin through fragmentation, measured in feeding kiln by electric vibrating feeder, along cylindrical shell vergence direction, moved to kiln tail by kiln hood.In moving process, the thermal radiation air flow contacts that material and combustion chamber high temperature air-flow heating steel sheet produce, attached water is dried, and crystal water starts to decompose, and causes a large amount of dehydration, forms semi-hydrated gypsum.The shortcoming adopting this technique to prepare β semi-hydrated gypsum is that material calcining is uneven, it is unstable to calcine later half water gypsum quality, and kind is single, consumes amount of heat in calcination process simultaneously.It is as follows that another kind utilizes mechanical frying pan to prepare the technique of β semi-hydrated gypsum: first heated by mechanical frying pan in production process, add plaster stone gradually, under the stirring of stirrer, be warming up to 170-200 DEG C, dihydrate gypsum dewaters in a large number, forms semi-hydrated gypsum.This technique equipment used cost is low, and procedure of processing is simple, compared with upper a kind of technique, thermosteresis obviously reduces compared with the former, quality product is relatively stable, but equipment energy consumption is high, and production efficiency is low, in processes process, terra alba easily hardens into block, can not meet scale operation needs.Chinese patent CN103159418A discloses " a kind of beta-type semi-hydrated gypsum powder calcining preparation technology and calciner ", its technique is be the powder of 100-140 order size by grain diameter after grinding, calcine through rotary kiln, temperature of kiln head 450-550 DEG C, kiln end temperature 155-190 DEG C, powder temperature is 150-170 DEG C.
At phosphogypsum Dehydration in semi-hydrated gypsum, current employing constant pressure hydro-thermal legal system is common for the Measures compare of αsemiwatergypsum, but the method adopting phosphogypsum that give off online, that have 65 DEG C of-75 DEG C of heats to prepare semi-hydrated gypsum gelling material and plastering not yet occurs.
Summary of the invention
The object of this invention is to provide the method for phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering, the environmental pollution that the air storage solving phosphogypsum causes, decrease the expense that phosphogypsum is stored up and transported.
The present invention solves the problems of the technologies described above adopted technical scheme: the method for phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering, comprises the following steps:
1) the hot online pretreatment technology of phosphogypsum: utilize properties-correcting agent, the phosphogypsum discharged online washing to Leaching Properties of Soluble Phosphorus content is not more than 0.2wt.% by employing washing process, soluble fluorine content is not more than 0.1wt.% and organic content is not more than 0.1wt.%, pH value is between 5-7, and Dehydration obtains phosphogypsum slurry;
2) the hot online hydro-thermal preparation technology of phosphogypsum: by step 1) the phosphogypsum slurry that obtains of pre-treatment and activity agent, medium crystallization agent be thoroughly mixed to form slip, by slip dynamic insulation reaction 3-8 hour at normal pressure, 70-100 DEG C; After carrying out solid-liquid separation, obtain semi-hydrated gypsum slurry, washings is reusable edible after treatment;
3) semi-hydrated gypsum gelling material living broadcast technique: by step 2) the semi-hydrated gypsum slurry that obtains obtains semi-hydrated gypsum powder through hot wash, filtration, drying; Or comprise: phosphogypsum product living broadcast technique: by step 2) the semi-hydrated gypsum slurry of gained is through washing and filtering technique, and direct-on-line prepares the product such as building block, plasterboard.
By such scheme, step 1) described in phosphogypsum be the byproduct of phosphoric acid by wet process discharge, in canescence, sulfate dihydrate calcium contents >=90wt.%.
By such scheme, step 1) described in properties-correcting agent be alkaline aqueous solution.
By such scheme, step 1) described in alkaline aqueous solution be aqua calcis or sodium hydroxide solution.
By such scheme, step 2) described in activity agent be divalence or monovalent metallic ion solution, be any one or a few compound in magnesium chloride, sodium-chlor, Repone K, sodium sulfate, potassium sulfate, calcium chloride, magnesium sulfate; The quality of wherein said activity agent accounts for the 40-90% of phosphogypsum quality, and concentration is 10-40wt.%.
By such scheme, step 2) described in medium crystallization agent be organic multicomponent acid, it is tartrate, succinic acid or citric acid, and its volume is the 0.01%-2% of phosphogypsum quality; Or organic multicomponent hydrochlorate, it is sodium tartrate, soluble tartrate, potassium succinate, Soduxin, Tripotassium Citrate or Trisodium Citrate, and its volume is the 0.01%-2% of phosphogypsum quality; Or tensio-active agent, it is Sodium dodecylbenzene sulfonate or single stearic acid glycerine lipoprotein, and its volume is the 0.01%-2% of phosphogypsum quality; Or the soluble sulphate of trivalent metal, it is Tai-Ace S 150 or ferric sulfate, and its volume is the 1%-8% of phosphogypsum quality.
By such scheme, step 2) described in dynamic insulation reaction process in the rotating speed of paddle remain on 50-300rpm.
By such scheme, step 2) described in solid-liquid separation be that vacuum hydro-extraction or centrifuge dehydration to slurry reach plaster of Paris GT9776-2008 required standard denseness.
By such scheme, step 3) described in hot water temperature be 70-100 DEG C.
By such scheme, step 3) described in the drying temperature of semi-hydrated gypsum slurry be 35-65 DEG C, time of drying is 1-5 hour.
Principle of the present invention: the impurity in properties-correcting agent and phosphogypsum carries out physical-chemical reaction, eliminates the impact of impurity double water gypsum plaster performance in phosphogypsum, is conducive to the recycle of salts solution; Dihydrate gypsum, in the solution of a complexing metal ion and medium crystallization agent, in atmospheric conditions, through dissolving-recrystallization process, can be converted into semi-hydrated gypsum by dihydrate gypsum; Metal ion does not consume in conversion process, plays a part to reduce crystalline form invert point, stablize semi-hydrated gypsum crystalline form; Medium crystallization agent is carried out selective adsorption by double water gypsum crystal, is changed crystal to the surface energy of medium, make the crystal habit of semi-hydrated gypsum turn to length-to-diameter ratio close to the αsemiwatergypsum of short cylinder of 1 by elongated needle, column, play effect semi-hydrated gypsum being carried out to crystalline form regulation and control.
Beneficial effect of the present invention is: the process decreasing the flotation of phosphogypsum ore deposit, the phosphogypsum that phosphorous chemical industry production line produces directly carries out constant pressure hydro-thermal reaction, by activity agent, medium crystallization agent inducing catalysis, obtained semi-hydrated gypsum crystal, obtains semi-hydrated gypsum gelling material after fast filtering drying and dehydrating.The hot constant pressure hydro-thermal legal system of phosphogypsum, for the method for semi-hydrated gypsum gelling material and goods thereof, can make full use of the heat of 65-75 DEG C that has when phosphogypsum gives off online, reduces phosphogypsum and stores up shared cost of land and transportation cost; The semi-hydrated gypsum gelling material simultaneously prepared is simultaneously containing α and β two kinds of crystal formations, by control temperature of reaction, activity agent and medium crystallization agent volume, reaction times etc. because of usually preparing satisfactory semi-hydrated gypsum powder and plastering, crystal formation control is workable, reliability is strong.
In a word, the environmental pollution that the air storage that this technique reduces phosphogypsum causes, decreases the expense that phosphogypsum is stored up and transported, has stronger economic benefit and social benefit.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
The method of phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering, is specially:
1) the hot online pre-treatment of phosphogypsum: the aqueous solution utilizing calcium hydroxide, adopt that the phosphogypsum discharged online washing to Leaching Properties of Soluble Phosphorus content is 0.1wt.% by washing process, soluble fluorine content be 0.08wt.% and organic content is 0.07wt.%, pH value is between 5-7, and Dehydration obtains phosphogypsum slurry;
2) the hot online hydro-thermal preparation technology of phosphogypsum: by step 1) the phosphogypsum slurry that obtains of pre-treatment and calcium chloride solution, succinic acid be thoroughly mixed to form slip, wherein the quality of calcium chloride solution accounts for the 40%-90% of phosphogypsum quality, the concentration of calcium chloride solution is 24wt.%, succinic acid volume is the 0.01-2% of phosphogypsum quality, by slip in normal pressure, dynamic insulation reaction 5 hours at 90 DEG C, stirring blade rotating speed is 200rpm; Adopt vacuum hydro-extraction to carry out solid-liquid separation to slurry and reach plaster of Paris GT9776-2008 required standard denseness, obtain semi-hydrated gypsum slurry, washings is reusable edible after treatment;
3) semi-hydrated gypsum gelling material living broadcast technique: by step 2) semi-hydrated gypsum that obtains filters through 90 DEG C of hot washes, and 50 DEG C of drying installations can obtain semi-hydrated gypsum powder after dry 3 hours; Phosphogypsum is converted into the productive rate of semi-hydrated gypsum powder more than 70%, and wherein the content of αsemiwatergypsum is more than 80%; Or comprise:
4) phosphogypsum product living broadcast technique: by step 2) the semi-hydrated gypsum slurry of gained through washing and filtering technique, directly prepare the product such as building block, plasterboard.
Embodiment 2:
The method of phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering, is specially:
1) the hot online pre-treatment of phosphogypsum: the aqueous solution utilizing calcium hydroxide, adopt that the phosphogypsum discharged online washing to Leaching Properties of Soluble Phosphorus content is 0.1wt.% by washing process, soluble fluorine content be 0.08wt.% and organic content is 0.07wt.%, pH value is between 5-7, and Dehydration obtains phosphogypsum slurry.
2) the hot online hydro-thermal preparation technology of phosphogypsum: by step 1) the phosphogypsum slurry that obtains of pre-treatment and activity agent, medium crystallization agent be thoroughly mixed to form slip, wherein the quality of activity agent solution accounts for 50% of phosphogypsum quality, the concentration of activity agent solution is 24wt.%, activity agent is wherein calcium chloride, sodium-chlor, potassium sulfate; Medium crystallization agent volume is 4% of phosphogypsum quality, and wherein medium crystallization agent is Tai-Ace S 150, ferric sulfate; By slip in normal pressure, dynamic insulation reaction 6 hours at 90 DEG C, stirring blade rotating speed is 200rpm; Adopt vacuum hydro-extraction to carry out solid-liquid separation to slurry and reach plaster of Paris GT9776-2008 required standard denseness, obtain semi-hydrated gypsum slurry, washings is reusable edible after treatment;
3) semi-hydrated gypsum gelling material living broadcast technique: by step 2) semi-hydrated gypsum that obtains filters through 90 DEG C of hot washes, can obtain semi-hydrated gypsum powder at 50 DEG C of drying installations after dry 3 hours; Phosphogypsum is converted into the productive rate of semi-hydrated gypsum powder more than 70%, and wherein the content of αsemiwatergypsum is more than 80%; Or comprise:
4) phosphogypsum product living broadcast technique: by step 2) the semi-hydrated gypsum slurry of gained through washing and filtering technique, directly prepare the product such as building block, plasterboard.
Embodiment 3:
The method of phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering, is specially:
1) the hot online pre-treatment of phosphogypsum: the aqueous solution utilizing calcium hydroxide, adopt that the phosphogypsum discharged online washing to Leaching Properties of Soluble Phosphorus content is 0.1wt.% by washing process, soluble fluorine content be 0.08wt.% and organic content is 0.07wt.%, pH value is between 5-7, and Dehydration obtains phosphogypsum slurry.
2) the hot online hydro-thermal preparation technology of phosphogypsum: by step 1) the phosphogypsum slurry that obtains of pre-treatment and calcium chloride solution, citric acid be thoroughly mixed to form slip, wherein the quality of calcium chloride solution accounts for 50% of phosphogypsum quality, and the concentration of activity agent solution is 24wt.%; Citric acid volume is the 0.01-2% of phosphogypsum quality, and by slip in normal pressure, dynamic insulation reaction 5 hours at 90 DEG C, stirring blade rotating speed is 200rpm; Adopt vacuum hydro-extraction to carry out solid-liquid separation to slurry and reach plaster of Paris GT9776-2008 required standard denseness, obtain semi-hydrated gypsum slurry, washings is reusable edible after treatment;
3) semi-hydrated gypsum gelling material living broadcast technique: by step 2) semi-hydrated gypsum that obtains filters through 90 DEG C of hot washes, and 35-65 DEG C of drying installation can obtain semi-hydrated gypsum powder after dry 3 hours; Phosphogypsum is converted into the productive rate of semi-hydrated gypsum powder more than 70%, and wherein the content of αsemiwatergypsum is more than 80%; Or comprise:
4) phosphogypsum product living broadcast technique: by step 2) the semi-hydrated gypsum slurry of gained through washing and filtering technique, directly prepare the product such as building block, plasterboard.
Claims (10)
1. the method for phosphogypsum hot living broadcast semi-hydrated gypsum gelling material and plastering, comprises the following steps:
1) the hot online pretreatment technology of phosphogypsum: utilize properties-correcting agent, the phosphogypsum discharged online washing to Leaching Properties of Soluble Phosphorus content is not more than 0.2wt.% by employing washing process, soluble fluorine content is not more than 0.1wt.% and organic content is not more than 0.1wt.%, pH value is between 5-7, and Dehydration obtains phosphogypsum slurry;
2) the hot online hydro-thermal preparation technology of phosphogypsum: by step 1) the phosphogypsum slurry that obtains of pre-treatment and activity agent, medium crystallization agent be thoroughly mixed to form slip, by slip dynamic insulation reaction 3-8 hour at normal pressure, 70-100 DEG C; After carrying out solid-liquid separation, obtain semi-hydrated gypsum slurry, washings is reusable edible after treatment;
3) semi-hydrated gypsum gelling material living broadcast technique: by step 2) the semi-hydrated gypsum slurry that obtains obtains semi-hydrated gypsum powder through hot wash, filtration, drying; Or comprise: phosphogypsum product living broadcast technique: by step 2) the semi-hydrated gypsum slurry of gained is through washing and filtering technique, and direct-on-line prepares the product such as building block, plasterboard.
2. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, it is characterized in that: step 1) described in phosphogypsum be phosphoric acid by wet process discharge byproduct, in canescence, sulfate dihydrate calcium contents >=90wt.%.
3. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, is characterized in that: step 1) described in properties-correcting agent be alkaline aqueous solution.
4. the method for phosphogypsum according to claim 3 hot living broadcast semi-hydrated gypsum gelling material and plastering, is characterized in that: step 1) described in alkaline aqueous solution be aqua calcis or sodium hydroxide solution.
5. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, it is characterized in that: step 2) described in activity agent be divalence or monovalent metallic ion solution, be any one or a few compound in magnesium chloride, sodium-chlor, Repone K, sodium sulfate, potassium sulfate, calcium chloride, magnesium sulfate; The quality of wherein said activity agent accounts for the 40-90% of phosphogypsum quality, and concentration is 10-40wt.%.
6. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, it is characterized in that: step 2) described in medium crystallization agent be organic multicomponent acid, it is tartrate, succinic acid or citric acid, and its volume is the 0.01%-2% of phosphogypsum quality; Or organic multicomponent hydrochlorate, it is sodium tartrate, soluble tartrate, potassium succinate, Soduxin, Tripotassium Citrate or Trisodium Citrate, and its volume is the 0.01%-2% of phosphogypsum quality; Or tensio-active agent, it is Sodium dodecylbenzene sulfonate or single stearic acid glycerine lipoprotein, and its volume is the 0.01%-2% of phosphogypsum quality; Or the soluble sulphate of trivalent metal, it is Tai-Ace S 150 or ferric sulfate, and its volume is the 1%-8% of phosphogypsum quality.
7. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, is characterized in that: step 2) described in dynamic insulation reaction process in the rotating speed of paddle remain on 50-300rpm.
8. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, is characterized in that: step 2) described in solid-liquid separation be that vacuum hydro-extraction or centrifuge dehydration to slurry reach plaster of Paris GT9776-2008 required standard denseness.
9. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, is characterized in that, step 3) described in hot water temperature be 70-100 DEG C.
10. the method for phosphogypsum according to claim 1 hot living broadcast semi-hydrated gypsum gelling material and plastering, is characterized in that: step 3) described in semi-hydrated gypsum slurry drying temperature be 35-65 DEG C, time of drying is 1-5 hour.
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| CN107324677A (en) * | 2017-08-25 | 2017-11-07 | 四川屹科环保科技有限公司 | High-strength semi-hydrated gypsum powder normal pressure semidry method preparation method, preparation facilities |
| CN109369046A (en) * | 2018-11-19 | 2019-02-22 | 湖北双环科技股份有限公司 | A kind of technique that salt chemical engineering waste prepares high strength gypsum |
| CN113402185A (en) * | 2021-07-28 | 2021-09-17 | 泰山石膏有限公司 | Separation treatment method of eutectic phosphorus in phosphogypsum |
| CN115010161A (en) * | 2022-01-19 | 2022-09-06 | 昆明理工大学 | Method for converting waste gypsum into alpha semi-hydrated gypsum |
| CN115745443A (en) * | 2022-11-29 | 2023-03-07 | 武汉理工大学 | Method for preparing alpha-type semi-hydrated gypsum from undisturbed phosphogypsum under low reaction medium dosage |
| CN116553849A (en) * | 2023-04-06 | 2023-08-08 | 湖北工业大学 | Method for preparing regenerated alpha high-strength gypsum by using waste gypsum |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324677A (en) * | 2017-08-25 | 2017-11-07 | 四川屹科环保科技有限公司 | High-strength semi-hydrated gypsum powder normal pressure semidry method preparation method, preparation facilities |
| CN109369046A (en) * | 2018-11-19 | 2019-02-22 | 湖北双环科技股份有限公司 | A kind of technique that salt chemical engineering waste prepares high strength gypsum |
| CN113402185A (en) * | 2021-07-28 | 2021-09-17 | 泰山石膏有限公司 | Separation treatment method of eutectic phosphorus in phosphogypsum |
| CN115010161A (en) * | 2022-01-19 | 2022-09-06 | 昆明理工大学 | Method for converting waste gypsum into alpha semi-hydrated gypsum |
| CN115010161B (en) * | 2022-01-19 | 2024-01-05 | 昆明理工大学 | Method for converting waste gypsum into alpha semi-hydrated gypsum |
| CN115745443A (en) * | 2022-11-29 | 2023-03-07 | 武汉理工大学 | Method for preparing alpha-type semi-hydrated gypsum from undisturbed phosphogypsum under low reaction medium dosage |
| CN115745443B (en) * | 2022-11-29 | 2023-11-03 | 武汉理工大学 | Method for preparing alpha-hemihydrate gypsum from undisturbed phosphogypsum with low reaction medium dosage |
| CN116553849A (en) * | 2023-04-06 | 2023-08-08 | 湖北工业大学 | Method for preparing regenerated alpha high-strength gypsum by using waste gypsum |
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