CN107416868B - A kind of preparation process of sodium bicarbonate and ammonium sulfate compound fertilizer - Google Patents
A kind of preparation process of sodium bicarbonate and ammonium sulfate compound fertilizer Download PDFInfo
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- CN107416868B CN107416868B CN201710452810.4A CN201710452810A CN107416868B CN 107416868 B CN107416868 B CN 107416868B CN 201710452810 A CN201710452810 A CN 201710452810A CN 107416868 B CN107416868 B CN 107416868B
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- sodium bicarbonate
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- ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Fertilizers (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses the preparation processes of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer, are significantly improved with the waste water high-purity sodium bicarbonate and ammonium sulfate fertilizer, economic benefit of production zinc borate.It is pollution-free and without emission.
Description
Technical field
The present invention relates to compound fertilizer's preparation technical fields, more particularly to the preparation of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer
Technique.
Background technique
The main component in the waste water of production zinc borate are as follows: the boric acid and 0.3- of sodium sulphate, 2-3% containing 15-17%
0.5% zinc sulfate.This general waste water gives free rein to evaporate, or produces awns by being concentrated by evaporation filtering in storing in reservoir
Nitre (sodium sulfate crystal), filtered fluid recycles, and does not generate economic benefit, or even loss substantially.How environmental-friendly processing
Waste water with using production zinc borate, while generating good economic benefit, can industrialized production, be needs of the present invention
The technical issues of solution.
Summary of the invention
The present invention provides the preparation process of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer aiming at above-mentioned defect,
The waste water for producing zinc borate is used to high-purity sodium bicarbonate and ammonium sulfate fertilizer, economic benefit significantly improves.And without discharge
Object, it is pollution-free.
The fabricating technology scheme of of the invention a kind of sodium bicarbonate and ammonium sulfate compound fertilizer is, using production zinc borate
Waste water high-purity sodium bicarbonate and ammonium sulfate fertilizer.
It is described production zinc borate waste water in containing by mass percentage the sodium sulphate of 15-17%, the boric acid of 2-3% and
The zinc sulfate of 0.3-0.5%.
The preparation process of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer, comprising the following steps: (1) zinc borate will be produced
Sewage treatment into evaporator, with sodium hydroxide solution be neutralized to PH be 7；
(2) the waste water negative pressure evaporation after neutralization is concentrated；
(3) it by ammonium bicarbonate soln, is swapped with Na base cation exchange resin, makes resin-bonded NH4 +, and by Na+
It is swapped out and HCO3- it is combined into sodium bicarbonate (NaHCO3) solution flows out to obtain sodium bicarbonate solution；With Nessler's reagent (how
This strangles reagent can be with NH4 +Red-brown precipitation is generated, the NH of 0.3 μ g (microgram) can be detected4 +, belong to trace detection) and examine outflow
Solution, until having red-brown precipitation generation；It is concentrated by evaporation at room temperature by negative pressure low-temperature evaporation tank and carbonic acid is made
Hydrogen sodium crystal, should not be using the method for directly heating concentration；Filtrate participates in the circulation concentration of next batch；
(4) metabisulfite solution made from step 2 is carried out backwash with the used ion exchange resin of step 3 to exchange, is made
The resin of ammonium is in conjunction at Na base cation exchange resin, and by NH4 +It is swapped out and SO4 2- it is combined into ammonium sulfate ((NH4)2SO4) solution outflow.The solution that outflow is examined with Nessler's reagent, until there is not red-brown precipitation；Obtained ammonium sulfate
Solution is evaporated concentration in evaporator, further crystallisation by cooling, is sulfuric acid ammonium product through centrifuge dripping；Under filtrate participates in
A batch of evaporation and concentration.
Using ammonium hydrogen carbonate and main component as the production zinc borate waste water solution of sodium sulphate repeatedly to resin swap with
Anticommuting and achieve the purpose that output sodium bicarbonate and ammonium sulfate, the chemical equation of exchange process (represents resin solid with R
Skeleton part) are as follows:
Positive exchange: R-SO3Na+NH4HCO3→R-SO3NH4+NaHCO3
Anticommuting: R-SO3NH4+1/2Na2SO4→R-SO3Na+1/2(NH4)2SO4
It can be seen that ammonium hydrogen carbonate (NH from the above chemical equation4HCO3) and sodium sulphate (Na2SO4) be all respectively with friendship
The exchangeable ion changed on resin is reacted, and output sodium bicarbonate (NaHCO respectively3) and ammonium sulfate ((NH4)2SO4).Therefore
High-purity sodium bicarbonate can be obtained and with ammonium sulfate compound fertilizer as main component.There is no other by-products, without pollutant emission.
In step (1), the evaporator is the sealable evaporator with stirring.
In step (2), sodium sulphate is concentrated into sulfur acid sodium 182-188 grams per liter solution (wherein containing Na+For 59-61 grams/
Rise), being cooled to temperature is 35-37 DEG C.
In step (3), the ammonium bicarbonate soln is NH4 +Content is the solution of 39-41 grams per liter.
In step (3), obtained sodium bicarbonate solution concentration is 8-10% or so.
In step (3), after sodium bicarbonate crystal is centrifugated, sodium bicarbonate is sent into hot air pipe, with hot wind and on a small quantity
CO2Sodium bicarbonate product is dried to obtain.
The invention has the benefit that
(1) since raw material of the present invention reaction is to swap respectively with cation exchange resin and anticommuting, tree is eliminated
The regeneration process of rouge, has saved cost, improves work efficiency.
(2) reactant is carried out under controlled condition, avoids other raw materials and by-product mixes product, therefore
Products obtained therefrom is with high purity, high-quality.
(3) due to gained sodium bicarbonate purity is high, without being cleaned, being separated repeatedly to product, cleaned, to eliminate
By soda carbonization be sodium bicarbonate process, by a relatively large margin reduce production cost.
(4) it is easy to go into operation due to subtracting links, the small investment of production equipment such as cleaning repeatedly, separation, removal of impurities.
(5) boracic and zinc (being the indispensable nutritional ingredient of crops as nitrogen) element in ammonium sulfate product, are one
The extraordinary high-quality compound fertilizer of kind, improves the quality of chemical fertilizer, and then improve economic benefit.
(6) without other byproduct emissions, basic non-environmental-pollution in production.
Specific embodiment:
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but this
Invention is not limited thereto.
A kind of preparation process of sodium bicarbonate and ammonium sulfate compound fertilizer, using the waste water high-purity little Su of production zinc borate
Beat and ammonium sulfate fertilizer.
It is described production zinc borate waste water in containing by mass percentage the sodium sulphate of 15-17%, the boric acid of 2-3% and
The zinc sulfate of 0.3-0.5%.
The preparation process of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer, comprising the following steps: (1) zinc borate will be produced
Sewage treatment to it is sealable with stirring evaporator evaporator in, with sodium hydroxide solution be neutralized to PH be 7；
(2) the waste water negative pressure evaporation after neutralization is concentrated, is concentrated into sodium sulphate to sulfur acid sodium 182-188 grams per liter solution
(wherein contain Na+For 59-61 grams per liter), being cooled to temperature is 35-37 DEG C.
(3) by NH4 +Content is the ammonium bicarbonate soln of 39-41 grams per liter, is swapped with Na base cation exchange resin,
Make resin-bonded NH4 +, and by Na+It is swapped out and HCO3- it is combined into sodium bicarbonate (NaHCO3) solution flows out to obtain sodium bicarbonate
Solution, obtained sodium bicarbonate solution concentration are 8-10% or so；With Nessler's reagent, (Nessler's reagent can be with NH4 +It generates red
Brown precipitate can detect the NH of 0.3 μ g (microgram)4 +, belong to trace detection) and the solution of outflow is examined, until there is red-brown precipitation
Until generation；It is concentrated by evaporation at room temperature by negative pressure low-temperature evaporation tank and sodium bicarbonate crystal is made, it should not be using direct
The method for heating concentration, after sodium bicarbonate crystal is centrifugated, send sodium bicarbonate into hot air pipe, with hot wind and a small amount of CO2
Sodium bicarbonate product is dried to obtain；Filtrate participates in the circulation concentration of next batch；
(4) metabisulfite solution made from step 2 is carried out backwash with the used ion exchange resin of step 3 to exchange, is made
The resin of ammonium is in conjunction at Na base cation exchange resin, and by NH4 +It is swapped out and SO4 2- it is combined into ammonium sulfate ((NH4)2SO4) solution outflow.The solution that outflow is examined with Nessler's reagent, until there is not red-brown precipitation；Obtained ammonium sulfate
Solution is evaporated concentration in evaporator, further crystallisation by cooling, is sulfuric acid ammonium product through centrifuge dripping；Under filtrate participates in
A batch of evaporation and concentration.
Using ammonium hydrogen carbonate and main component as the production zinc borate waste water solution of sodium sulphate repeatedly to resin swap with
Anticommuting and achieve the purpose that output sodium bicarbonate and ammonium sulfate, the chemical equation of exchange process (represents resin solid with R
Skeleton part) are as follows:
Positive exchange: R-SO3Na+NH4HCO3→R-SO3NH4+NaHCO3
Anticommuting: R-SO3NH4+1/2Na2SO4→R-SO3Na+1/2(NH4)2SO4
It can be seen that ammonium hydrogen carbonate (NH from the above chemical equation4HCO3) and sodium sulphate (Na2SO4) be all respectively with friendship
The exchangeable ion changed on resin is reacted, and output sodium bicarbonate (NaHCO respectively3) and ammonium sulfate ((NH4)2SO4).Therefore
High-purity sodium bicarbonate can be obtained and with ammonium sulfate compound fertilizer as main component.There is no other by-products, without pollutant emission.
Embodiment 1
1, the built-in 732 cation exchange resin column (flow produced with Taicang Hong Ze chemical anticorrosion apparatus Co., Ltd
For 6m3/h).Ammonium hydrogen carbonate is made into the solution of 173.8 grams per liters, allows solution by ion exchange resin, is examined with Nessler's reagent
The solution for testing outflow, until having red-brown precipitation generation.9% sodium bicarbonate solution is obtained, it is dense through negative pressure low-temperature evaporation
Contract, be centrifugated high-purity sodium bicarbonate (sodium bicarbonate), sodium bicarbonate content reach 99.9%.
2, it is examined by the ion exchange resin of ammonium with Nessler's reagent with the metabisulfite solution of 184.6 grams per liters
The solution of outflow, until there is not red-brown precipitation.8% ammonium sulfate is obtained, is concentrated by evaporation, is centrifugated
Ammonium sulfate product, wherein ammonium sulphate content is 97.6%, boric acid 1.9%, zinc sulfate 0.5%.
Embodiment 2
1, the built-in 732 cation exchange resin column (flow produced with Taicang Hong Ze chemical anticorrosion apparatus Co., Ltd
For 6m3/h).Ammonium hydrogen carbonate is made into the solution of 175 grams per liters, allows solution by ion exchange resin, is examined with Nessler's reagent
The solution of outflow, until having red-brown precipitation generation.9.1% sodium bicarbonate solution is obtained, it is dense through negative pressure low-temperature evaporation
It contracts, be centrifugated to obtain sodium bicarbonate, sodium bicarbonate content reaches 99.87%.
2, it is examined by the ion exchange resin of ammonium with Nessler's reagent with the metabisulfite solution of 186.8 grams per liters
The solution of outflow, until there is not red-brown precipitation.7.9% ammonium sulfate is obtained, is concentrated by evaporation, is centrifugated
Ammonium sulfate product is obtained, wherein ammonium sulphate content is 97.4%, boric acid 2%, zinc sulfate 0.6%.
Above embodiments device therefor price:
Ion exchange resin column (flow 6m3/ h) 2: 20,000
It is concentrated by evaporation 2 sets: 40,000 of tank
2: 40,000, centrifuge
Dryer 2: 200,000
Product price and yield:
Sodium bicarbonate: 1600 yuan/ton of price, daily 20 ton/days of production.
Ammonium sulfate: 600 yuan/ton, 15 ton/days of price.
The output value:
32000+9000 yuan/days of yuan/day=4.1 ten thousand yuan/day
Producing cost (artificial, water power): 1.6 ten thousand yuan/day.
Profit: ten thousand yuan/day of 4.1-1.6=2.5.
Claims (3)
1. the preparation process of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer, which is characterized in that produced using the waste water of production zinc borate
High-purity sodium bicarbonate and ammonium sulfate fertilizer, wherein contain 15-17% by mass percentage in the waste water of the production zinc borate
Sodium sulphate, the boric acid of 2-3% and the zinc sulfate of 0.3-0.5%, the preparation process the following steps are included:
(1) Sewage treatment of zinc borate will be produced into evaporator, being neutralized to pH with sodium hydroxide solution is 7；
(2) the waste water negative pressure evaporation after neutralization is concentrated, is concentrated into sulfur acid sodium 182-188 grams per liter solution, being cooled to temperature is
35-37℃；
(3) it by ammonium bicarbonate soln, is swapped with Na base cation exchange resin, makes resin-bonded NH4 +, and by Na+Exchange
Out and HCO3- be combined into sodium bicarbonate solution and flow out to obtain sodium bicarbonate solution；The solution of outflow is examined with Nessler's reagent,
Until having red-brown precipitation generation；It is concentrated by evaporation at room temperature by negative pressure low-temperature evaporation tank and sodium bicarbonate crystalline substance is made
Body；Filtrate participates in the circulation concentration of next batch, and the ammonium bicarbonate soln is NH4+Content is the solution of 39-41 grams per liter, is obtained
The sodium bicarbonate solution concentration arrived is 8-10%；
(4) metabisulfite solution made from step 2 is carried out backwash with the used ion exchange resin of step 3 to exchange, makes ammonium
Resin in conjunction at Na base cation exchange resin, and by NH4 +It is swapped out and SO4 2- it is combined into ammonium sulfate outflow；With
Nessler's reagent examines the solution of outflow, until there is not red-brown precipitation；Obtained ammonium sulfate is in evaporator
It is evaporated concentration, further crystallisation by cooling, is sulfuric acid ammonium product through centrifuge dripping；The evaporation that filtrate participates in next batch is dense
Contracting.
2. the preparation process of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer according to claim 1, which is characterized in that step
(1) in, the evaporator is the sealable evaporator with stirring.
3. the preparation process of a kind of sodium bicarbonate and ammonium sulfate compound fertilizer according to claim 1, which is characterized in that step
(3) in, after sodium bicarbonate crystal is centrifugated, sodium bicarbonate is sent into hot air pipe, with hot wind and a small amount of CO2It is dried
Sodium bicarbonate product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2416954A1 (en) * | 1978-02-08 | 1979-09-07 | Pechiney Ugine Kuhlmann | NON-POLLUTING TREATMENT OF URANIUM EFFLUENTS FROM AN ALKALINE ATTACK OF A URANIUM ORE CONTAINING SULFUR |
| CN1089235A (en) * | 1993-12-29 | 1994-07-13 | 张祥林 | The method of the single-phase decomposition system sodium bicarbonate of sodium sulfate and bicarbonate of ammonia |
| CN101704532A (en) * | 2009-11-10 | 2010-05-12 | 武汉大学 | Preparation method of zinc borate |
| CN105600805B (en) * | 2016-01-20 | 2017-06-16 | 西北大学 | A kind of method that ammonium sulfate is isolated and purified in the regenerative process by-product solution from fume desulfurizing agent |
| CN105645514B (en) * | 2016-01-20 | 2017-06-16 | 西北大学 | The isolation and purification method of ammonium sulfate and sodium sulphate mixed solution in a kind of fume desulfurizing agent regenerative process |
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