CN1096418C - Process for preparing high-quality low-salt low-potassium heavy sodium carbonate and ammonium chloride by direct calcine of vapor, washing and hydration - Google Patents
Process for preparing high-quality low-salt low-potassium heavy sodium carbonate and ammonium chloride by direct calcine of vapor, washing and hydration Download PDFInfo
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- CN1096418C CN1096418C CN01107296A CN01107296A CN1096418C CN 1096418 C CN1096418 C CN 1096418C CN 01107296 A CN01107296 A CN 01107296A CN 01107296 A CN01107296 A CN 01107296A CN 1096418 C CN1096418 C CN 1096418C
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Abstract
The present invention discloses a technology which is characterized in that steam is directly used for calcination, sodium chloride impurities and potassium sulfate impurities are washed by condensed water under the condition of high temperature, the water which is generated by reaction is directly hydrated with sodium carbonate to generate sodium carbonate monohydrate, and the sodium carbonate monohydrate is dried by hot air to prepare sodium carbonate and ammonium chloride with the advantages of good quality, low salt content, low potassium content and heavy weight. The present invention comprises the following technological processes: raw material preparation, carbonization, solid-liquid separation, calcination, packing of finished products of sodium carbonate with low salt content and low potassium content, cold-hot exchange of liquid, crystallization, precipitation, filtration of material liquid, and packing of finished products of ammonium chloride. The present invention has the characteristics of short technological processes, simple equipment, less investment, low energy consumption, low cost and easy acquisition of raw materials.
Description
Technical Field
The invention relates to a production process of sodium carbonate and ammonium chloride, in particular to a process for preparing low-salt low-potassium heavy sodium carbonate and ammonium chloride by directly calcining with low-pressure steam, washing impurities of sodium chloride and potassium sulfate with condensed water under a high-temperature condition, directly hydrating the generated water with sodium carbonate to generate sodium carbonate monohydrate and drying with hot air.
Background
The present industrial production method of heavy soda at home and abroad includes three kinds of processes of solid-phase extrusion process, solid-phase hydration process and liquid-phase hydration process, and they are characterized by that the sodium bicarbonate produced by ammonia-soda process and combined-soda process is firstly made into light soda, then the light soda is fed into hydration machine to make into sodium carbonate monohydrate. Calcining and drying at 120-140 ℃ by a rotary calciner to prepare heavy soda ash, or extruding into blocks by a solid-phase extrusion method to obtain the heavy soda ash after crushing and screening.
The method for directly preparing the heavy soda ash by taking the sodium bicarbonate as the raw material is abroad disclosed in U.S. patent No. 345176, and the method is characterized in that the sodium bicarbonate or the sodium carbonate is added into a reactor of sodium carbonate slurry, and is decomposed at 135-200 ℃ by a circulating heat exchanger: discharging the sodium carbonate in a suspended state, separating out monohydrate soda from the mother liquor, and calcining to obtain the heavy soda ash. Chinese patent ZL-94111741.3 is prepared by adding sodium bicarbonate containing catalyst into fixed steam decomposition reaction furnace, directly feeding process steam or saturated steam into fixed steam decomposition reaction furnace as temperature-raising and pressure-raising reaction medium, decomposing sodium bicarbonate into heavy soda at 0.3-0.8 Mpa (gauge pressure) and 140-180 deg.C in one step, preheating by heating with hot air to 120-150 deg.C, feeding superheated steam or saturated steam into decomposition reaction furnace, reacting at temperature higher than 200 deg.C and pressure of 0.3-0.8 Mpa and 140-180 deg.C, opening steam exhaust valve, exhausting mixed gas, discharging in two parts, one part is discharged from middle or lower part of decomposition furnace through gas-liquid flow receiver, the other part is discharged through another gas-water separator, the exhausted gas is cooled to room temperature by water after passing through evaporator, separator, and pressurizingForce 0.3EUnder 0.8MPa, CO can be directly fed by self pressure without compressor2And (5) preparing sodium bicarbonate in a carbonization tower. It has five drawbacks: firstly, the process selection is unreasonable in pressure holding, and the defect of the process selection is that CO is2The gas is injected into the carbonization tower, and the solid in the decomposing furnace is decomposed to produce a large amount of CO2The gas heating process, the decomposed gas is discharged out of the pressure building in time, the reaction is not favored to be carried out to the positive direction from the chemical reaction balance principle, the chemical reaction speed is slow, and the production period is long. Secondly, no sodium carbonate monohydrate forming process: during operation, hot air is firstly used for preheating to 140 ℃, the steam has small heat supply coefficient to air, the heat supply coefficient to materials and equipment by the hot air is small, and a large amount of steam and blower electric energy are needed for heating to 140 ℃, so that the energy consumption is high. The process is selected from the pressure-building CO delivery2Gaseous, to maintain 0.3 ~ 0.8Mpa and increased the steam energy consumption again, the third is the operation original, and physical strength is big: the upper sealing disc and the lower sealing disc of the method need manpower to be disassembled and assembled once in production, products in the furnace are fully excavated by manual feeding, and materials are excavated by manual feeding in the furnace when one tank is produced. The digging working environment is severe. Fourthly, the equipment is various, and the pipeline plugging equipment is operated. The method uses the preheated air to preheat the materials, and discharges the preheated air from the upper part or the lower part, so that the sodium bicarbonate in the furnace is easy to be blown off by the air; the separation liquid discharged from the reaction decomposition has a large amount of materials which are discharged through the water separator along with the separation liquid to block the water separator and the pipeline. Fifthly, a large amount of CO is wasted2Gas: the operation of the method is that hot air is firstly used for preheating to 140 ℃, and a large amount of sodium bicarbonate is heated to 120 ℃ to decompose a large amount of CO2A gas. Run away with the air, waste CO2And a large amount of CO needs to be supplemented2The energy consumption of raw materials of the heavy soda ash product is increased. Therefore, the method has the advantages of difficult realization of industrial large-scale production of process equipment, high raw material consumption and high energy consumption.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a process for preparing low-salt low-potassium heavy soda ash and ammonium chloride by directly calcining, washing and hydrating steam, which has the characteristics of short process flow, simple equipment, investment saving, low energy consumption, low cost and easily available raw materials, is directly calcined by low-pressure steam, does not hold back air, does not need to add air for preheating, does not run carbon dioxide, does not block the pipeline of the equipment, does not manually enter a tank for digging materials, and is convenient to operate.
The purpose of the invention is realized as follows:
the process flow of the invention is as follows: preparing raw materials, carbonizing, separating solid from liquid, calcining, packaging a low-salt heavy soda finished product, exchanging cold and heat of mother liquor II of mother liquor I, crystallizing and separating out ammonium chloride, filtering the ammonium chloride, and packaging an ammonium chloride finished product.
The invention relates to a method for directly calcining and decomposing wet sodium bicarbonate into sodium carbonate by steam in a calcining reactor, wherein the steam provides heat energy to be changed into condensed water to quickly dissolve and wash sodium chloride and potassium sulfate which are impurities under the high temperature condition, and water generated by reaction is directly hydrated with the sodium carbonate to generate sodium carbonate monohydrate and is dried by hot air.
The specific process flow of the invention is as follows:
A. raw material preparation
The raw materials comprise solid ammonium bicarbonate with the nitrogen content of more than 17.1 percent and carbon dioxide, semi-ammonium mother liquor II with the ammonium chloride concentration of 110-140 g/L and the sodium chloride concentration of 190-210 g/L and sodium chloride solid with the content of 96 percent;
B. carbonizing
Adding a semi-ammonium mother solution II into a carbonization tower, introducing carbon dioxide compressed by a compressor from a calcination reactor at the temperature of 24-48 ℃, and then adding solid ammonium bicarbonate for carbonization;
C. solid-liquid separation
Separating the solid-liquid mixture obtained after carbonization by a centrifuge to obtain granular wet sodium bicarbonate and mother liquor I, wherein the obtained wet sodium bicarbonate contains less than 4% of sodium chloride, less than 5% of ammonium bicarbonate, less than 0.8% of potassium sulfate and other impurities;
D. calcination of
Feeding the granular wet sodium bicarbonate into a calcination reactor, and simultaneously finishing calcination decomposition, washing, hydration, drying, stirring and discharging to obtain high-quality low-salt low-potassium heavy sodium carbonate and mixed gas containing carbon dioxide, ammonia and water vapor; after the mixed gas is subjected to waste heat recovery by a brine evaporator to prepare solid sodium chloride, introducing carbon dioxide obtained by cooling and separating the mixed gas into a carbonization tower by a compressor; the steam pressure of the water for washing hydration in the calcination reaction is 0.05-03 Mpa (gauge pressure), and the temperature is 90-140 ℃; the steam direct calcination, washing and hydration step is direct calcination without washing.
E. Product package
Packaging the obtained product to obtain high-quality low-salt low-potassium heavy soda ash;
F. liquid heat and cold exchange
Sending the mother liquor I after the sodium bicarbonate is separated by the centrifuge into a heat exchanger for cooling, and cooling theliquid from 32 ℃ to 24 ℃;
G. crystallization of ammonium chloride
Feeding the cooled mother liquor I into a crystallizer, adding ammonia gas and solid sodium chloride with the content of 96%, introducing ammonia, performing cold separation, salting out, and thickening in the crystallizer to obtain a feed liquid containing more than 60% of ammonium chloride particles;
H. ammonium chloride filtration
Separating the feed liquid containing more than 60% of ammonium chloride particles by a centrifugal machine to obtain solid ammonium chloride and semi-ammonium mother liquor II, heating the semi-ammonium mother liquor II from 12 ℃ to 24 ℃ by a heat exchanger, and sending the semi-ammonium mother liquor II back to the carbonization tower.
I. Ammonium chloride finished product package
And (5) metering and packaging by using a packaging machine.
The crystallizer of the invention is a normal pressure tank type ammonium chloride crystallizer, which is a tank type one-step process flow ammonium chloride crystallizer in another patent application technology of the applicant, and the patent application number is 01214583.1.
The carbonization tower adopts a normal pressure carbonization tower, and the diameter-height ratio of the carbonization tower is 1: 2-8.
The calcination reactor of the present invention employs a "one steam direct calcination reactor" of patent application No. 01213889.4 owned by Leshan cattle Huawang Xiaojie chemical plant. And the reaction steps of calcining, washing, hydrating, drying, cooling, discharging and the like are completed in the calcining reactor in one step.
The heavy soda ash has the advantages of large bulk density, no caking, less package, no dust in storage, transportation and use, etc., and the low-salt heavy soda ash also has the advantage of much lower corrosion to the used equipment than the common heavy soda ash.
The main working principle of the invention is as follows:
1. calcination of
The wet sodium bicarbonate is decomposed into soda ash at the high temperature of 90-140 ℃, steam is directly calcined and provides heat energy to be changed into condensed water, and impurities are quickly dissolved and washed at the high temperature.
2. Hydration of
Generation of sodium carbonate monohydrate: selecting the condition with highest hydration rate in the calcining reactor, and hydrating sodium carbonate and water generated by calcining into sodium carbonate monohydrate
3. Dewatering
Drying and dehydrating the sodium carbonate monohydrate in a calcining reactor to prepare the high-quality low-salt low-potassium heavy soda ash.
The technical indexes of the low-salt low-potassium heavy soda ash finished product are as follows:
the appearance is white fine particles, the total alkali content (calculated by sodium carbonate) is 99.70%, the chloride content (calculated by sodium chloride) is 0.061%, the content of water-insoluble substances is 0.03%, and the sulfate is SO4 2-) 0.01 percent, 0.017 percent of iron, 0.70 percent of ignition loss, 0.98 g/ml of bulk density and 2.2 mg/kg of potassium (calculated by K).
The technical indexes of the ammonium chloride product are as follows:
the ammonium chloride content is greater than 91.20%, the sodium chloride content is less than 3.3%, and the water content is less than 5%.
The complete process for preparing high-quality low-salt low-potassium heavy soda ash and ammonium chloride has the characteristics of short process flow, simple equipment, investment saving, low energy consumption, low cost and easily available raw materials.
Drawings
The following figures of the present invention are given.
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a flow chart of the process equipment for preparing high-quality low-salt low-potassium heavy soda ash and ammonium chloride.
FIG. 3 is a schematic diagram of the structure of an ammonium chloride crystallizer according to the present invention.
FIG. 4 is a schematic view of the structure of the calcination reactor of the present invention.
FIG. 5 is a block flow diagram of the apparatus of the present invention.
In fig. 2, symbol 1 represents a carbonization tower, symbol 2 represents a calcination reactor, and symbol 3 represents an ammonium chloride crystallizer.
The process flow of the invention is as follows: preparing raw materials, carbonizing, separating solid from liquid, calcining, packaging a heavy soda finished product, carrying out liquid heat and cold exchange on mother liquor I and mother liquor II, crystallizing and separating out ammonium chloride, filtering the ammonium chloride, and packaging an ammonium chloride finished product.
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, wherein all amounts, parts and percentages are by weight unless otherwise specified.
Detailed Description
Example one
A. Raw material preparation
The raw materials comprise 6.0 tons of solid ammonium bicarbonate with the nitrogen content of more than 17.1 percent, carbon dioxide, and 60 cubic meters of semi-ammonia mother liquor II with the ammonium chloride concentration of 120 grams/liter and the sodium chloride concentration of 210 grams/liter;
B. carbonizing
Adding 60 cubic meters of semi-ammonium mother liquor II into a carbonization tower, introducing carbon dioxide gas compressed by a compressor from a calcining reactor at the temperature of 24-48 ℃, and then adding 6.0 tons of solid ammonium bicarbonate for carbonization to obtain qualified sodium bicarbonate liquid;
C. separation of feed liquid
Separating the sodium bicarbonate solution obtained after carbonization by a centrifuge to obtain 13 tons of granular wet sodium bicarbonate and liquid mother liquor I68 cubic meters, wherein the obtained wet sodium bicarbonate contains less than 4 percent of sodium chloride, less than 5 percent of ammonium bicarbonate, less than 0.8 percent of potassium sulfate and other impurities;
D. calcination of
13 tons of granular wet sodium bicarbonate is sent into a calcination reactor to complete calcination decomposition, washing, hydration, drying, stirring and discharging simultaneously, 6.3 tons of low-salt low-potassium heavy sodium carbonate (the content of the sodium bicarbonate is 99.6 percent, the content of sodium chloride is 0.07 percent, the content of sulfate is 0.01 percent, the content of Fe is 0.002 percent, the content of potassium chloride is 0.003 percent, the content of water-insoluble substances is 0.03 percent, and the bulk density is 0.98) is obtained, and meanwhile, mixed gas containing carbon dioxide, ammonia and water vapor is obtained; recovering waste heat of the mixed gas by a brine evaporator to prepare 5.6 tons of solid sodium chloride, and compressing and introducing carbon dioxide obtained after cooling and separating the mixed gas into a carbonization tower by a compressor; the pressure of washing water vapor of the calcination reaction is 0.05-03 Mpa (gauge pressure), the calcination temperature is 90-140 ℃, the time is 8-12 hours, the hydration pressure is 0.05-0.15 Mpa (gauge pressure), the temperature is 90-120 ℃, the time is 4 hours, and the drying and discharging time is 10 hours;
E. packing the heavy soda ash finished product
Packaging the obtained soda ash by a frequency modulation stirrer (10-500 rpm) to prepare high-quality low-salt low-potassium heavy soda ash;
F. liquid heat and cold exchange
Separating by a centrifuge to obtain mother liquor I68 cubic meters, sending the mother liquor I into a heat exchanger for cooling, and reducing the temperature of the mother liquor I from 32 ℃ to 24 ℃;
G. crystallization of ammonium chloride
Feeding the cooledmother liquor I into an ammonium chloride crystallizer with a normal pressure tank lacking, adding 8 tons of ammonia and 80 tons of solid sodium chloride with the content of 96%, introducing ammonia into the ammonium chloride crystallizer with the normal pressure tank lacking for 0.5 hour, cooling the ammonia and the water for 8 hours, completing salting out and cold separation at the same time, and thickening to obtain 15 cubic meters of ammonium chloride feed liquid containing more than 60% of particles;
H. ammonium chloride filtration
The feed liquid containing more than 60 percent of granular ammonium chloride is separated by a centrifuge to obtain 6.95 tons of solid ammonium chloride and 60 cubic meters of semi-ammonia mother liquor II, and the semi-ammonia mother liquor II is heated by a heat exchanger and sent back to the carbonization tower from 12 ℃ to 24 ℃.
I. Ammonium chloride finished product package
And (5) metering and packaging by using a packaging machine.
The invention has the characteristics of short process flow, simple equipment, investment saving, low energy consumption, low cost, easily obtained raw materials and the like.
Claims (10)
1. The process for preparing the low-salt low-potassium heavy soda ash and ammonium chloride is characterized by comprising the step of directly calcining, washing and hydrating wet sodium bicarbonate by using steam in a calcining reactor, wherein the step of calcining wet sodium bicarbonate is directly calcined and decomposed into sodium carbonate by using the steam, the steam provides heat energy to become condensed water, sodium chloride and potassium sulfate impurities are quickly dissolved and washed under the high-temperature condition, water generated by reaction is directly hydrated with the sodium carbonate to generate sodium carbonate monohydrate, the sodium carbonate monohydrate is dried by using hot air, the calcining and washing pressure is 0.05-0.3 Mpa, the temperature is 90-140 ℃, the hydrating and drying pressure is 0.05-0.15 Mpa, and the temperature is 90-120 ℃.
2. The process for preparing low-salt low-potassium dense soda ash and ammonium chloride as claimed in claim 1, wherein the steam direct calcination washing water is not washed, and the steam direct calcination wet sodium bicarbonate.
3. The process for preparing low-salt low-potassium heavy soda ash and ammonium chloride as claimed in claim 1 or 2, further comprising the steps of raw material preparation, carbonization, solid-liquid separation, packing of the finished heavy soda ash, heat and cold exchange of liquid, crystallization and precipitation of ammonium chloride, filtration of ammonium chloride, and packing of the finished ammonium chloride.
4. The process for preparing low-salt low-potassium dense soda ash and ammonium chloride as claimed in claim 3, wherein the raw material comprises solid ammonium bicarbonate with nitrogen content greater than 17.1% and carbon dioxide, semi-ammonium mother liquor II with ammonium chloride concentration of 110-140 g/l and sodium chloride concentration of 190-210 g/l and sodium chloride solid content of 96%.
5. The process for preparing low-salt low-potassium dense soda ash and ammonium chloride as claimed in claim 3, wherein the carbonization step comprises adding semi-ammonium mother liquor II into a carbonization tower, introducing carbon dioxide at 24-48 ℃, and adding solid ammonium bicarbonate for carbonization.
6. The process according to claim 3, wherein the solid-liquid separation step comprises subjecting the solid-liquid mixture obtained after carbonization to centrifuge separation to obtain wet granular sodium bicarbonate and liquid mother liquor I, wherein the obtained wet sodium bicarbonate contains less than 4% of sodium chloride, less than 5% of ammonium bicarbonate and less than 0.8% of potassium sulfate and other impurities.
7. The process for preparing low-salt low-potassium dense soda ash and ammonium chloride as claimed in claim 3, wherein the calcining step is to send the granular wet sodium bicarbonate into a calcining reactor to calcine, decompose, wash and hydrate to obtain low-salt low-potassium soda ash and obtain a mixed gas containing carbon dioxide, ammonia and water vapor; the mixed gas is used for recovering waste heat through a brine evaporator to prepare solid sodium chloride, and carbon dioxide obtained after cooling and separating the mixed gas is compressed and introduced into a carbonization tower.
8. The process for preparing low-salt low-potassium dense soda ash and ammonium chloride as claimed in claim 3, wherein the liquid heat and cold exchange step is to send the mother liquor I separated by centrifuge into heat exchanger to cool, and the temperature of mother liquor I is decreased from 32 ℃ to 24 ℃.
9. The process for preparing low-salt potassium heavy soda ash and ammonium chloride as claimed in claim 3, wherein the ammonium chloride crystallization step comprises feeding the cooled mother liquor I into an atmospheric pressure tank type ammonium chloride crystallizer, adding ammonia gas and solid sodium chloride with the content of more than 96%, and passing through ammonia, salting out, cold separation, ammonia cooling, water cooling and thickening in the atmospheric pressure tank type ammonium chloride crystallizer to obtain a feed liquid containing more than 60% of ammonium chloride particles.
10. The process for preparing low-salt low-potassium dense soda ash and ammonium chloride as claimed in claim 3, wherein said ammonium chloride filtering step is to separate the feed liquid containing more than 60% of ammonium chloride particles by a centrifuge to obtain solid ammonium chloride and semi-ammonium mother liquor II, and the semi-ammonium mother liquor II is heated from 12 ℃ to 24 ℃ by a heat exchanger and sent back to the carbonization tower.
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| CN01107296A CN1096418C (en) | 2001-03-29 | 2001-03-29 | Process for preparing high-quality low-salt low-potassium heavy sodium carbonate and ammonium chloride by direct calcine of vapor, washing and hydration |
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| CN01107296A CN1096418C (en) | 2001-03-29 | 2001-03-29 | Process for preparing high-quality low-salt low-potassium heavy sodium carbonate and ammonium chloride by direct calcine of vapor, washing and hydration |
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| CN1096418C true CN1096418C (en) | 2002-12-18 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108615A (en) * | 1994-03-14 | 1995-09-20 | 门伟 | Method for production of refined white alkali |
| CN1111214A (en) * | 1994-05-04 | 1995-11-08 | 喻中甫 | Catalytic one-stage produced heavy soda ash and fixed steam decomposition reaction furnace device |
| CN1156124A (en) * | 1996-01-26 | 1997-08-06 | 化学工业部大连化工研究设计院 | Process for producing low-salt heavy sodium carbonate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108615A (en) * | 1994-03-14 | 1995-09-20 | 门伟 | Method for production of refined white alkali |
| CN1111214A (en) * | 1994-05-04 | 1995-11-08 | 喻中甫 | Catalytic one-stage produced heavy soda ash and fixed steam decomposition reaction furnace device |
| CN1156124A (en) * | 1996-01-26 | 1997-08-06 | 化学工业部大连化工研究设计院 | Process for producing low-salt heavy sodium carbonate |
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