CN103224246B - Chemical gypsum-to-ammonium sulfate reaction slurry concentration, waste heat recovery and waste ammonia recovery method - Google Patents
Chemical gypsum-to-ammonium sulfate reaction slurry concentration, waste heat recovery and waste ammonia recovery method Download PDFInfo
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- CN103224246B CN103224246B CN201310167981.4A CN201310167981A CN103224246B CN 103224246 B CN103224246 B CN 103224246B CN 201310167981 A CN201310167981 A CN 201310167981A CN 103224246 B CN103224246 B CN 103224246B
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Abstract
The invention discloses a chemical gypsum-to-ammonium sulfate reaction slurry concentration, waste heat recovery and waste ammonia recovery method. The method comprises a step of pretreatment, a step of ammonia water dissolution, a step of carbonation fixation reacting, a step of concentration and recovery, and a step of filtration, drying and evaporating crystallization. The above concentration and recovery step concretely comprises the following processes: letting a carbonation fixation reaction product into a concentration and recovery device, carrying out vacuum flash evaporating separation, pumping a generated gas out, carrying out an countercurrent washing operation, sending the prepared ammonia-containing washing liquid to a carbonation fixation reaction to supplement the ammonia in the carbonation reaction system, and discharging an uncondensed gas from the system. The chemical gypsum-to-ammonium sulfate reaction slurry concentration, waste heat recovery and waste ammonia recovery method has the characteristics of simple technology, low energy consumption, low cost, full utilization of the ammonia gas, energy saving, and substantial reduction of the industrial pollution.
Description
Technical field
The invention belongs to chemical fertilizer manufacturing technology field, specifically, relate to a kind of chemical gypsum sulphur ammonium reaction slurry and concentrate and ammonia recovery method more than waste heat.
Background technology
China's chemical gypsum is the solid waste produced from industries such as chemical industry, electric power, metallurgy and fluorine chemicals, mainly comprise phosphogypsum, desulfurized gesso of flue gas, fluorgypsum etc., annual quantity discharged nearly hundred million tons, suitable with plaster of paris year produced quantity, storing up in a large number of chemical gypsum brings serious environmental problem, and it is reasonable, effective utilization becomes problem demanding prompt solution.In the comprehensive Utilization Ways of chemical gypsum, utilize the CO of chemical gypsum and industrial discharge
2the technology of carrying out carbonation reaction generation fertilizer product ammonium sulfate has good development prospect, not only effectively can utilize Sulphur ressource valuable in chemical gypsum, and reduce greenhouse gases CO
2discharge, realize the treatment of wastes with processes of wastes against one another, turn waste into wealth.
Patent CN102627309A has disclosed one and has utilized calcium base large Industrial Solid Waste phosphogypsum strengthening carbonating to fix CO in industrial gaseous waste
2method, the method need use remaining ammonia excessive in sulfuric acid neutralization reaction slip, the ammonium sulfate liquor concentration not only obtained is lower, and the Lowlevel thermal energy of reaction slurry cannot reclaim, cause the raw material of the method and energy expenditure too high, seriously hinder applying of this technology, in addition, the accumulating of sulfuric acid and the concentrated further of ammonium sulfate liquor all need large chemical equipment, invest larger.
Patent CN102701256A discloses a kind of method utilizing chemical gypsum low temperature conversion preparing granular ammonium sulfate and calcium carbonate.The method is obtain higher gypsum transformation efficiency, need keep ammonia solution and CO in reaction system
2excessive, cause the ammonium sulfate liquor concentration of generation lower thus, and excessive remaining ammonia is stored in mother liquor with the form of volatile salt and bicarbonate of ammonia.The method that prior art all adopts sulfuric acid to neutralize, the ammonium sulfate liquor that purification generates, but the method is equal to additional sulfuric acid and volatile salt to produce ammonium sulfate, significantly increase the consumption of sulfuric acid and ammonia in production process, and need to consume more low-pressure steam and carry out the concentrated of ammonium sulfate liquor, the ammonium sulfate product cost causing this technology to obtain is higher, thus the applying of influence technique.
The shortcoming of prior art: CO in existing fixing industrial gaseous waste
2method in the utilization ratio of ammonia low, sulfuric acid consumption is large, and cost is high, and energy expenditure is large.
Summary of the invention
For solving above technical problem, the chemical gypsum sulphur ammonium reaction slurry that a kind of cost is low, efficiency is high, energy expenditure is low is the object of the present invention is to provide to concentrate and ammonia recovery method more than waste heat.
The present invention seeks to realize like this: a kind of chemical gypsum sulphur ammonium reaction slurry concentrated with waste heat more than ammonia recovery method, by (1) pre-treatment; (2) ammoniacal liquor alkali is molten; (3) carbonating fixation reaction; (4) concentrated and recovery; (5) filtration, evaporative crystallization obtain calcium carbonate three steps compositions, it is characterized in that described step (4) is concentrated to be specially with recovery: the product of described carbonating fixation reaction is passed into concentrated and retrieving arrangement, first be 0.01-0.1MPa at working pressure be carry out vacuum flashing under the condition of 60-120 DEG C to be separated with service temperature, make the volatile salt of carbonation reaction by-product and ammonium bicarbonate breaks down be ammonia and CO
2, then extracted out by the gas produced, carry out countercurrent washing operation, the ammonia contained in gas is only absorbed by the water, and send in described carbonating fixation reaction by obtained containing ammonia stripping liquid, supplement the ammonia content in carbonation reaction system, non-condensable gas then discharges system.Pass through aforesaid operations, in flash distillation mode, carbonation reaction heat is used for reaction product to concentrate, ammonium sulfate concentrations in the slip of discharging bottom vacuum flasher is improved, simultaneously, do not need to add in system again in sulfuric acid and remaining ammonia, in extraction ammonia sulfate crystal process, reduce the required energy consumption of evaporation, directly can pass through concentrated and retrieving arrangement, by remaining ammonia and waste heat recovery, make full use of ammonia and heat energy, avoid the waste of resource, decrease the consumption of energy, reduce the production cost of product.
Above-mentioned concentrating is made up of reducing valve, vacuum flasher, washing tower, recycle pump and vacuum pump with retrieving arrangement, described reducing valve is connected with the opening for feed of vacuum flasher, the top gas discharge port of described vacuum flasher is communicated with washing tower opening for feed by pipeline, the top gas discharge port of described washing tower is communicated with vacuum pump by pipeline, and the bottom wash liquid discharge port of this washing tower is communicated with recycle pump.Adopt said structure, the concentrated of slurry can be realized by vacuum flasher, the separation of gas, realized the recovery of ammonia and waste heat by washing tower and recycle pump and vacuum pump.
Above-mentioned steps (1) pre-treatment is specially: by chemical gypsum hot wash, removes the water-soluble salt of water-soluble phosphorus, sulphur trioxide, fluorochemical and potassium, sodium, magnesium and aluminium.
Above-mentioned steps (2) ammoniacal liquor alkali is molten to be specially: step (1) pretreated chemical gypsum is added ammoniacal liquor and carries out the molten reaction of alkali at normal temperatures, leaching section calcium ion.
Above-mentioned steps (3) carbonating fixation reaction is specially: add in closed reactor by the solidliquid mixture that step (2) produces, pass into CO
2waste gas carries out the heterogeneous CO of gas-liquid-solid
2carbonating fixation reaction, CO
2partial pressure is 0.1-2.0Mpa, and temperature of reaction is 50-150 DEG C, constantly supplements ammoniacal liquor simultaneously, and the pH value maintaining reaction system is 8.0-10.0, reaction times 5-60min, generates ammonium sulfate and calcium carbonate crystal.
Above-mentioned chemical gypsum is made up of one or more in industrial phosphogypsum, desulfurized gesso of flue gas, fluorgypsum, citric acid gypsum, boron gypsum, titanium gypsum and mirabilite gypsum.
Above-mentioned steps (5) filtration, drying and evaporative crystallization are specially: discharge in step (4) bottom vacuum flasher through concentrated solid-liquid mixture, filter, obtain filtrate and filter cake, by filtrate after evaporative crystallization operation, obtain ammonia sulfate crystal; By filter cake after washing drying, obtain calcium carbonate crystal.
Beneficial effect:
A kind of chemical gypsum sulphur of the present invention ammonium reaction slurry concentrated with waste heat more than ammonia recovery method, the feature such as have that technique is simple, energy consumption is low and cost is low, fully can reuse ammonia and energy, has saved the energy, greatly reduce industrial pollution.
Accompanying drawing explanation
Fig. 1 is structural representation that is concentrated and retrieving arrangement.
Embodiment
Embodiment 1:
A kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat, by (1) pre-treatment; (2) ammoniacal liquor alkali is molten; (3) carbonating fixation reaction; (4) concentrated and recovery; (5) filtration, evaporative crystallization obtain calcium carbonate three steps compositions:
(1) pre-treatment: by chemical gypsum hot wash, removes the water-soluble salt of water-soluble phosphorus, sulphur trioxide, fluorochemical and potassium, sodium, magnesium and aluminium.
(2) ammoniacal liquor alkali is molten: step (1) pretreated chemical gypsum is added ammoniacal liquor and carries out the molten reaction of alkali at normal temperatures, leaching section calcium ion.
(3) carbonating fixation reaction: join in airtight carbonation reactor by the solidliquid mixture that step (2) produces, wherein in solidliquid mixture, calcium sulphate content is 70%, then passes into CO
2waste gas carries out the heterogeneous CO of gas-liquid-solid
2carbonating fixation reaction, CO
2partial pressure is 2.0Mpa, and temperature of reaction is 150 DEG C, constantly supplements ammoniacal liquor simultaneously, and the pH value maintaining reaction system is 8.0, reaction times 5min.
(4) concentrated and recovery: the product of described carbonating fixation reaction is passed into concentrated and retrieving arrangement, first be 0.01MPa at working pressure be carry out vacuum flashing under the condition of 120 DEG C to be separated with service temperature, the volatile salt of carbonation reaction by-product and ammonium bicarbonate breaks down is made to be ammonia and CO2, then the gas produced is extracted out, carry out countercurrent washing operation, the ammonia contained in gas is only absorbed by the water, obtained is sent in described carbonating fixation reaction containing ammonia stripping liquid, supplement the ammonia content in carbonation reaction system, non-condensable gas then discharges system by vacuum pump.
Described concentrating is made up of reducing valve 10, vacuum flasher 6, washing tower 7, recycle pump 8 and vacuum pump 9 with retrieving arrangement, described reducing valve 10 is connected with the opening for feed of vacuum flasher 6, the top gas discharge port of described vacuum flasher 6 is communicated with washing tower 7 opening for feed by pipeline, the top gas discharge port of described washing tower 7 is communicated with vacuum pump 9 by pipeline, and the bottom wash liquid discharge port of this washing tower 7 is communicated with recycle pump 8.
(5) filtration, dry and evaporative crystallization: discharge in step (4) bottom vacuum flasher through concentrated solid-liquid mixture, filter, obtain filtrate and filter cake, in filtrate, the content of ammonium sulfate is 46%, directly through evaporative crystallization operation, ammonia sulfate crystal can be obtained; By filter cake after washing drying, obtain calcium carbonate, its purity is 92%.
Embodiment 2:
A kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat, by (1) pre-treatment; (2) ammoniacal liquor alkali is molten; (3) carbonating fixation reaction; (4) concentrated and recovery; (5) filtration, evaporative crystallization obtain calcium carbonate three steps compositions:
(1) pre-treatment: by chemical gypsum hot wash, removes the water-soluble salt of water-soluble phosphorus, sulphur trioxide, fluorochemical and potassium, sodium, magnesium and aluminium.
(2) ammoniacal liquor alkali is molten: step (1) pretreated chemical gypsum is added ammoniacal liquor and carries out the molten reaction of alkali at normal temperatures, leaching section calcium ion.
(3) carbonating fixation reaction: join in airtight carbonation reactor by the solidliquid mixture that step (2) produces, wherein in solidliquid mixture, calcium sulphate content is 65%, then passes into CO
2waste gas carries out the heterogeneous CO of gas-liquid-solid
2carbonating fixation reaction, CO
2partial pressure is 0.1Mpa, and temperature of reaction is 50 DEG C, constantly supplements ammoniacal liquor simultaneously, and the pH value maintaining reaction system is 10.0, reaction times 60min.
(4) concentrated and recovery: the product of described carbonating fixation reaction is passed into concentrated and retrieving arrangement, first be 0.1MPa at working pressure be carry out vacuum flashing under the condition of 60 DEG C to be separated with service temperature, make the volatile salt of carbonation reaction by-product and ammonium bicarbonate breaks down be ammonia and CO
2, then extracted out by the gas produced, carry out countercurrent washing operation, the ammonia contained in gas is only absorbed by the water, and send in described carbonating fixation reaction by obtained containing ammonia stripping liquid, supplement the ammonia content in carbonation reaction system, non-condensable gas then discharges system.
Described concentrating is made up of reducing valve 10, vacuum flasher 6, washing tower 7, recycle pump 8 and vacuum pump 9 with retrieving arrangement, described reducing valve 10 is connected with the opening for feed of vacuum flasher 6, the top gas discharge port of described vacuum flasher 6 is communicated with washing tower 7 opening for feed by pipeline, the top gas discharge port of described washing tower 7 is communicated with vacuum pump 9 by pipeline, and the bottom wash liquid discharge port of this washing tower 7 is communicated with recycle pump 8.
(5) filtration, dry and evaporative crystallization: discharge in step (4) bottom vacuum flasher through concentrated solid-liquid mixture, filter, obtain filtrate and filter cake, in filtrate, the content of ammonium sulfate is 45%, directly through evaporative crystallization operation, ammonia sulfate crystal can be obtained; By filter cake after washing drying, obtain calcium carbonate, its purity is 93%.
Embodiment 3:
A kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat, by (1) pre-treatment; (2) ammoniacal liquor alkali is molten; (3) carbonating fixation reaction; (4) concentrated and recovery; (5) filtration, evaporative crystallization obtain calcium carbonate three steps compositions:
(1) pre-treatment: by chemical gypsum hot wash, removes the water-soluble salt of water-soluble phosphorus, sulphur trioxide, fluorochemical and potassium, sodium, magnesium and aluminium.
(2) ammoniacal liquor alkali is molten: step (1) pretreated chemical gypsum is added ammoniacal liquor and carries out the molten reaction of alkali at normal temperatures, leaching section calcium ion.
(3) carbonating fixation reaction: the solidliquid mixture that step (2) produces is joined in airtight carbonation reactor, passes into CO
2waste gas carries out the heterogeneous CO of gas-liquid-solid
2carbonating fixation reaction, CO
2partial pressure is 1.0Mpa, and temperature of reaction is 90 DEG C, constantly supplements ammoniacal liquor simultaneously, and the pH value maintaining reaction system is 9.0, reaction times 30min.
(4) concentrated and recovery: the product of described carbonating fixation reaction is passed into concentrated and retrieving arrangement, first be 0.07MPa at working pressure be carry out vacuum flashing under the condition of 90 DEG C to be separated with service temperature, make the volatile salt of carbonation reaction by-product and ammonium bicarbonate breaks down be ammonia and CO
2, then extracted out by the gas produced, carry out countercurrent washing operation, the ammonia contained in gas is only absorbed by the water, and send in described carbonating fixation reaction by obtained containing ammonia stripping liquid, supplement the ammonia content in carbonation reaction system, non-condensable gas then discharges system.
Described concentrating is made up of reducing valve 10, vacuum flasher 6, washing tower 7, recycle pump 8 and vacuum pump 9 with retrieving arrangement, described reducing valve 10 is connected with the opening for feed of vacuum flasher 6, the top gas discharge port of described vacuum flasher 6 is communicated with washing tower 7 opening for feed by pipeline, the top gas discharge port of described washing tower 7 is communicated with vacuum pump 9 by pipeline, and the bottom wash liquid discharge port of this washing tower 7 is communicated with recycle pump 8.
(5) filtration, dry and evaporative crystallization: discharge in step (4) bottom vacuum flasher through concentrated solid-liquid mixture, filter, obtain filtrate and filter cake, in filtrate, the content of ammonium sulfate is 45%, directly through evaporative crystallization operation, ammonia sulfate crystal can be obtained; By filter cake after washing drying, obtain calcium carbonate, its purity is 92%.
Claims (5)
1. chemical gypsum sulphur ammonium reaction slurry concentrates and an ammonia recovery method more than waste heat, by (1) pre-treatment, (2) ammoniacal liquor alkali is molten, (3) carbonating fixation reaction, (4) concentrated and recovery, (5) filter, dry and evaporative crystallization five steps forms, it is characterized in that described step (4) is concentrated to be specially with recovery: the product of described carbonating fixation reaction is passed into concentrated and retrieving arrangement, first be 0.01-0.1MPa at working pressure be carry out vacuum flashing under the condition of 60-120 DEG C to be separated with service temperature, then the gas produced is extracted out, carry out countercurrent washing operation, the ammonia contained in gas is only absorbed by the water, obtained is sent in described carbonating fixation reaction containing ammonia stripping liquid, supplement the ammonia content in carbonation reaction system, non-condensable gas then discharges system,
Described concentrating is made up of reducing valve (10), vacuum flasher (6), washing tower (7), recycle pump (8) and vacuum pump (9) with retrieving arrangement, described reducing valve (10) is connected with the opening for feed of vacuum flasher (6), the top gas discharge port of described vacuum flasher (6) is communicated with washing tower (7) opening for feed by pipeline, the top gas discharge port of described washing tower (7) is communicated with vacuum pump (9) by pipeline, and the bottom wash liquid discharge port of this washing tower (7) is communicated with recycle pump (8);
Described step (1) pre-treatment is specially: by chemical gypsum hot wash, removes the water-soluble salt of water-soluble phosphorus, sulphur trioxide, fluorochemical and potassium, sodium, magnesium and aluminium.
2. a kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat according to claim 1, it is characterized in that described step (2) ammoniacal liquor alkali is molten to be specially: step (1) pretreated chemical gypsum is added ammoniacal liquor and carries out the molten reaction of alkali at normal temperatures, leaching section calcium ion, obtains chemical gypsum slurry.
3. a kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat according to claim 2, it is characterized in that described step (3) carbonating fixation reaction is specially: joined in airtight carbonation reactor by the solidliquid mixture that step (2) produces, pass into CO
2waste gas carries out the heterogeneous CO of gas-liquid-solid
2carbonating fixation reaction, CO
2partial pressure is 0.1-2.0MPa, and temperature of reaction is 50-150 DEG C, constantly supplements ammoniacal liquor simultaneously, and the pH value maintaining reaction system is 8.0-10.0, reaction times 5-60min.
4. a kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat according to claim 3, it is characterized in that: described chemical gypsum is made up of one or more in industrial phosphogypsum, desulfurized gesso of flue gas, fluorgypsum, citric acid gypsum, boron gypsum, titanium gypsum and mirabilite gypsum.
5. a kind of chemical gypsum sulphur ammonium reaction slurry concentrates and ammonia recovery method more than waste heat according to claim 4, it is characterized in that described step (5) filtration, drying and evaporative crystallization are specially: discharge in step (4) bottom vacuum flasher through concentrated solid-liquid mixture, filter, obtain filtrate and filter cake, by filtrate after evaporative crystallization operation, obtain ammonium sulfate; By filter cake after washing drying, obtain calcium carbonate.
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| CN103923242B (en) * | 2014-04-19 | 2015-04-08 | 商南天和泥浆有限公司 | Hydrolyzed polyacrylonitrile ammonium salt production system |
| CN104071805B (en) * | 2014-06-30 | 2015-12-09 | 北京阳光欣禾科技有限公司 | A kind of industry subtracts the processing method of carbon emission and solid waste comprehensive utilization |
| CN107051176A (en) * | 2017-06-02 | 2017-08-18 | 中化重庆涪陵化工有限公司 | The ardealite solid waste processing reutilization system and processing method of environmental protection |
| CN110467203B (en) * | 2019-09-12 | 2023-03-14 | 内蒙古星汉新材料有限公司 | System for carry out reutilization to heat that preparation potassium fluoride produced |
| CN114074953A (en) * | 2020-08-10 | 2022-02-22 | 四川大学 | Titanium-containing blast furnace slag or chlorinated tailings and red gypsum mineralized CO2Method (2) |
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