CN104628012A - Production method for preparing ammonium sulfate by alkylating waste acid - Google Patents
Production method for preparing ammonium sulfate by alkylating waste acid Download PDFInfo
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- CN104628012A CN104628012A CN201510014902.5A CN201510014902A CN104628012A CN 104628012 A CN104628012 A CN 104628012A CN 201510014902 A CN201510014902 A CN 201510014902A CN 104628012 A CN104628012 A CN 104628012A
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Abstract
The invention relates to a production method for preparing ammonium sulfate by alkylating waste acid. The production method consists of four parts namely neutralization reaction, flotation oil removal, activated carbon filtration and crystallization, and specifically comprises the following steps: enabling waste acid and ammonia water to perform neutralization reaction in a reactor; conveying hot steam which is produced by reaction to a raw material liquid ammonia vaporizer and a crystallizer by virtue of a steam pipeline to be applied to liquid ammonia vaporization and ammonium sulfate solution crystallization processes; performing flotation oil removal on the ammonium sulfate solution obtained by reaction and air by virtue of steam stripping flotation, and then performing activated carbon decoloration and deodorization on the ammonium sulfate solution after being subjected to flotation oil removal; and crystallizing the ammonium sulfate solution after being subjected to activated carbon adsorption to prepare an ammonium sulfate crystal. By adopting the production method disclosed by the invention, the problems that waste sulfuric acid is difficult to treat and polymerized oil is difficult to recycle can be solved, an alkylation process can be improved, and 13-15% of the total cost of the alkylation process can be reduced; and compared with a conventional ammonium sulfate preparation process, the time and cost can be saved, and the production efficiency can be increased by more than 20%.
Description
Technical field
The present invention relates to the production method that a kind of alkylation spent acid prepares ammonium sulfate.Comprise the operations such as neutralization reaction, flotation oil removing, decoloration and deodorization, evaporative crystallization.
Background technology
The national economic development is in recent years swift and violent, and the demand of market to stop bracket gasoline also strengthens thereupon, and alkylate oil has wide market potential.But often produce 1t alkylate oil in alkylation industry and will produce the Waste Sulfuric Acid that 80 ~ 100kg concentration is about 90%, this Waste Sulfuric Acid is dark red, and viscosity is larger, very muddy, character is unstable, distributes singularity stink, be difficult to process, bring severe contamination to ecotope.Outside its composition sulfuric acid, also contain organism (stand oil) and the moisture of 10%, stand oil complicated component, recycles very difficult.
Existing spent acid process is mainly divided into 6 classes: Waste Sulfuric Acid is concentrated, Waste Sulfuric Acid purification, Waste Sulfuric Acid regenerate, sell, neutralizing treatment, production chemical fertilizer.Waste Sulfuric Acid is concentrated mainly comprises that submerged combustion is concentrated, drum-type is concentrated, vacuum concentration, cooking-pot type are concentrated; Waste Sulfuric Acid purification mainly comprises the methods such as condensing crystal, dialysis and reverse osmosis, air lift, thermolysis and perfect combustion; Waste Sulfuric Acid regeneration is generally that Waste Sulfuric Acid is resolved into sulfurous gas and water vapor, after suitably purifying, oxidizing sulfur dioxide is become sulphur trioxide, thus obtained business level sulfuric acid; Produce chemical fertilizer and generate ammonium sulfate nitrogenous fertilizer by spent acid and ammonia react.
The technique of wherein producing ammonium sulfate fertilizer is comparatively ripe, but in existing technique, sulfuric acid and ammoniacal liquor react the amount of heat discharged and is all wasted, and the ammoniumsulphate soln many dependence natural subsidence containing stand oil that reaction generates is separated, and greatly, production efficiency is low for time loss.In addition, the general purity of spent acid production ammonia sulfate crystal is lower, and color and luster turns to be yellow, and is difficult to come into the market.
Therefore, alkylation spent acid treatment technology Waste Sulfuric Acid urgently to be resolved hurrily is difficult, the problem that stand oil difficulty reclaims, and it is serious that ammonium sulfate preparation technology is badly in need of solving thermal waste, and time loss is large, and production efficiency is low, and product purity is low, the problem of ammonia sulfate crystal jaundice.Whole chemical industry has great demand for a set of energy integrated, environmentally friendly chemical industry spent acid efficient solutions.
Summary of the invention
The present invention, according to the deficiencies in the prior art, proposes the production method that a kind of alkylation spent acid prepares ammonium sulfate, solves Waste Sulfuric Acid difficult, the problem that stand oil difficulty reclaims, and perfect alkylation process, reduce further the production cost of alkylate oil.Solve traditional ammonium sulfate preparation technology thermal waste serious simultaneously, time loss is large, production efficiency is low, product purity is low, the problem of ammonia sulfate crystal jaundice, has prepared purity higher, and product are good ammonia sulfate crystal mutually, in addition heat energy recycling, proposes integrated, the environmentally friendly chemical spent material efficient solutions of energy.
The technology of the present invention is as follows:
Alkylation spent acid prepares a production method for ammonium sulfate, is made up of neutralization reaction, flotation oil removing, activated carbon filtration and crystallization four part; Spent acid and ammoniacal liquor carry out neutralization reaction in reactor; Reaction Heat of Formation steam is delivered to raw materials ammonia vaporizer and crystallizer by steam-pipe, for liquid ammonia vaporization and ammoniumsulphate soln Crystallization Procedure; React ammoniumsulphate soln and air carry out stripping flotation oil removing, after flotation oil removing, ammoniumsulphate soln carries out activated carbon decolorizing deodorization; After charcoal absorption, ammoniumsulphate soln carries out crystallization; Obtain ammonia sulfate crystal.
Described ammoniacal liquor is vaporizated into ammonia by liquefied ammonia by vaporizer, passes into reactor dissolve generation ammoniacal liquor through gas distributor.
Described spent acid and ammoniacal liquor carry out neutralization reaction in reactor; Reactor operating pressure 1 ?10bar, service temperature 100 ?120 DEG C.
Described flotation oil removing completes at flotation tower; Solution is at flotation tower internal circulation flow, and gas drives mixed solution light constituent in tower to move upward, and realizes oily water separation; After flotation oil removing, oil phase is by the extraction of tower top stand oil extraction mouth.
Described flotation unit tower top tower reactor is respectively oil-collecting section and liquid collecting section; Be provided with inner sleeve in each tower joint of interlude, lower end is furnished with gas extractor; Solution is in the flowing of sleeve inner-outer circulation, and gas drives mixed solution light constituent in tower to move upward; Flotation unit working pressure 1 ?10bar, service temperature 60 ?100 DEG C.
Described activated carbon filtration completes in activated carbon adsorber: ammoniumsulphate soln passes into activated carbon adsorber, and the ammoniumsulphate soln of decoloration and deodorization is by the extraction of ammonium sulfate extraction mouth; Activated carbon adsorber working pressure 1 ?10bar, service temperature 40 ?100 DEG C.
Described crystallization operation pressure 1 ?10bar, service temperature 60 ?200 DEG C.
The mole of feed throughput ratio of raw material spent acid and ammonia is as the criterion close to saturated with reaction product ammoniumsulphate soln.
Advantage of the present invention:
1. by the neutralization reaction of Waste Sulfuric Acid and ammonia, generate ammonia sulfate crystal, reclaim alkylate oil, solve alkylation spent acid difficult, the problem that stand oil difficulty reclaims, perfect alkylation process, and considerably reduce the production cost of alkylate oil;
2. the hot steam that neutralization reaction generates is used for raw materials ammonia vaporization and ammoniumsulphate soln crystallization use, achieves energy integrated, avoid thermal waste, the low alkylation process total cost of co-falling 13% ?15%;
3. flotation oil removal plant can realize oily water separation fast, compares traditional ammonium sulfate preparation technology and to save time cost, enhance productivity more than 20%;
4. by flotation oil removing and activated carbon filtration, it is higher that the present invention can obtain purity, and product are good ammonia sulfate crystal mutually, can reach GB nitrogenous fertilizer premium grads standard (nitrogen content >=21%), solve traditional ammonium sulfate preparation technology product purity low, the problem of ammonia sulfate crystal jaundice.
Accompanying drawing explanation
Figure 1 ?process flow sheet;
Wherein: equipment 1 ?liquid ammonia vaporization device; 2 ?neutralization reactor; 3 ?flotation oil removing tower; 4 ?activated carbon adsorber; 5 ?crystallizer;
Stream stock A ?raw water; B ?raw material to give up the vitriol oil; C ?raw materials ammonia; D ?hot steam; E ?react to obtain ammoniumsulphate soln; F ?air; G ?stand oil; H ?ammoniumsulphate soln after flotation oil removing; I ?ammoniumsulphate soln after charcoal absorption; J ?ammonia sulfate crystal.
Embodiment
Be described in detail below in conjunction with accompanying drawing:
As shown in Figure 1, alkylation spent acid of the present invention prepares the production technique of ammonium sulfate, is using the useless vitriol oil, liquefied ammonia as preparing ammonium sulfate.Raw water (A) is by water-transmission line input reactor (2), liquefied ammonia (C) is vaporizated into ammonia by vaporizer (1), pass into reactor through gas distributor and dissolve generation ammoniacal liquor, spent acid (B) is delivered in reactor through sparger, carries out neutralization reaction with ammoniacal liquor.Reaction Heat of Formation steam (D) is delivered to raw materials ammonia vaporizer (1) and crystallizer (5), for liquid ammonia vaporization and ammoniumsulphate soln Crystallization Procedure by steam-pipe.React ammoniumsulphate soln (E) is delivered to flotation oil removing tower (3) by impeller pump, enter air (F) at the bottom of tower and carry out stripping flotation, stand oil (G) is by the extraction of tower top oil-collecting section, after flotation oil removing, ammoniumsulphate soln (H) is delivered to activated carbon adsorber (4), by activated carbon decolorizing deodorization by extraction at the bottom of tower.After charcoal absorption, ammoniumsulphate soln (I) is by the extraction of ammonium sulfate extraction mouth, is delivered to ammonium sulphate crystallizer and carrying (5), and crystallizer thermal source is hot steam (D).Crystallization gained ammonia sulfate crystal (J) is by crystalliser feet extraction.
Processing condition are preferably:
Neutralization reaction, water is by water-transmission line input reactor, and liquefied ammonia is vaporizated into ammonia by vaporizer, and pass into reactor through gas distributor and dissolve generation ammoniacal liquor, spent acid is delivered in reactor through sparger, reacts with ammoniacal liquor.Reactor operating pressure 1 ?10bar, service temperature 100 ?120 DEG C.
Neutralization reaction is that spent acid and ammoniacal liquor carry out neutralization reaction; Reacting ammonia is excessive, and reaction environment is alkalescence; Generate a large amount of hot steam and be delivered to raw materials ammonia vaporising device and crystallizer by steam-pipe, for liquid ammonia vaporization and ammoniumsulphate soln Crystallization Procedure.
Described raw materials ammonia is greater than 2:1 with the ratio of the mole of feed flow of spent acid, and reaction product ammoniumsulphate soln is close to saturated.
Described flotation oil removing is: passed in flotation unit by neutralization reaction gained solution and carry out stripping flotation, and solution is at flotation unit tower internal circulation flow, and gas drives mixed solution light constituent in tower to move upward, and realizes oily water separation; After flotation oil removing, oil phase is by the extraction of tower top stand oil extraction mouth.
Described flotation unit tower top tower reactor is respectively oil-collecting section and liquid collecting section; Be provided with inner sleeve in each tower joint of interlude, lower end is furnished with gas extractor; Solution is in the flowing of sleeve inner-outer circulation, and gas drives mixed solution light constituent in tower to move upward, and realizes oily water separation fast.Flotation unit working pressure 1 ?10bar, service temperature 60 ?100 DEG C.Described activated carbon filtration is: flotation unit tower reactor ammoniumsulphate soln passes into activated carbon adsorber by extraction at the bottom of tower, and the ammoniumsulphate soln of decoloration and deodorization is by the extraction of ammonium sulfate extraction mouth.Activated carbon adsorber working pressure 1 ?10bar, service temperature 40 ?100 DEG C.
Described crystallization is: utilize crystallizer to carry out crystallization to ammoniumsulphate soln, obtain product ammonia sulfate crystal.Crystallizer operation pressure 1 ?10bar, service temperature 60 ?200 DEG C.
Typical example:
To give up the vitriol oil to produce 1000t per year, the alkylation plant of production time in year 8000h is example.Raw water (A) (250kg/h, 25 DEG C, 1.5bar) by water-transmission line input reactor (2), liquefied ammonia (C) (50kg/h, 25 DEG C, 10bar) be vaporizated into ammonia by vaporizer (1), pass into reactor through gas distributor and dissolve generation ammoniacal liquor, by spent acid (B) (125kg/h, 25 DEG C, 1.5bar) be delivered in reactor through sparger, carry out neutralization reaction with ammoniacal liquor.Reaction Heat of Formation steam (D) (80kg/h, 117 DEG C, 1.5bar) is delivered to raw materials ammonia vaporizer (1) and crystallizer (5), for liquid ammonia vaporization and ammoniumsulphate soln Crystallization Procedure by steam-pipe.React to obtain ammoniumsulphate soln (E) (ammonium sulfate massfraction 41.9%, stand oil massfraction 3%) be delivered to flotation oil removing tower (3) by impeller pump, enter air (F) at the bottom of tower and carry out stripping flotation, stand oil (G) is by the extraction of tower top oil-collecting section, after flotation oil removing, ammoniumsulphate soln (H) (ammonium sulfate massfraction 43.1%) is delivered to activated carbon adsorber (4), by activated carbon decolorizing deodorization by extraction at the bottom of tower.After charcoal absorption, ammoniumsulphate soln (I) (ammonium sulfate massfraction 43.2%) is by the extraction of ammonium sulfate extraction mouth, is delivered to ammonium sulphate crystallizer and carrying (5), and crystallizer thermal source is hot steam (D).Crystallization gained ammonia sulfate crystal (J) is by crystalliser feet extraction.Produce ammonia sulfate crystal 1275t per year, its nitrogen content is 21%, reaches GB nitrogenous fertilizer premium grads standard.
The useless vitriol oil and ammonia are reacted, save the investment of useless vitriol oil post-processed, the large energy simultaneously utilizing the vitriol oil and ammonia neutralization reaction process to discharge, reduces the energy consumption investment of whole technical process, finally alkylating production cost can be reduced by 15%.
The above example is only the preferred embodiment absolutely proving the present invention and lift, and protection scope of the present invention is not limited thereto.The equivalent alternative or conversion that those skilled in the art do on basis of the present invention, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (7)
1. alkylation spent acid prepares a production method for ammonium sulfate, it is characterized in that being made up of neutralization reaction, flotation oil removing, activated carbon filtration and crystallization four part; Spent acid and ammoniacal liquor carry out neutralization reaction in reactor; Reaction Heat of Formation steam is delivered to raw materials ammonia vaporizer and crystallizer by steam-pipe, for liquid ammonia vaporization and ammoniumsulphate soln Crystallization Procedure; React ammoniumsulphate soln and air carry out stripping flotation oil removing, after flotation oil removing, ammoniumsulphate soln carries out activated carbon decolorizing deodorization; After charcoal absorption, ammoniumsulphate soln carries out crystallization; Obtain ammonia sulfate crystal.
2. the method for claim 1, is characterized in that liquefied ammonia is vaporizated into ammonia by vaporizer, passes into reactor dissolve generation ammoniacal liquor through gas distributor.
3. the method for claim 1, is characterized in that spent acid and ammoniacal liquor carry out neutralization reaction in reactor; Reactor operating pressure 1-10bar, service temperature 100-120 DEG C.
4. the method for claim 1, is characterized in that described flotation oil removing completes at flotation tower; Solution is at flotation tower internal circulation flow, and gas drives mixed solution light constituent in tower to move upward, and realizes oily water separation; After flotation oil removing, oil phase is by the extraction of tower top stand oil extraction mouth.
5. method as claimed in claim 4, is characterized in that described flotation unit tower top tower reactor is respectively oil-collecting section and liquid collecting section; Be provided with inner sleeve in each tower joint of interlude, lower end is furnished with gas extractor; Solution is in the flowing of sleeve inner-outer circulation, and gas drives mixed solution light constituent in tower to move upward; Flotation unit working pressure 1-10bar, service temperature 60-100 DEG C.
6. the method for claim 1, is characterized in that described activated carbon filtration completes in activated carbon adsorber: ammoniumsulphate soln passes into activated carbon adsorber, and the ammoniumsulphate soln of decoloration and deodorization is by the extraction of ammonium sulfate extraction mouth; Activated carbon adsorber working pressure 1-10bar, service temperature 40-100 DEG C.
7. the method for claim 1, is characterized in that described crystallization operation pressure 1-10bar, service temperature 60-200 DEG C.
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| CN105600826A (en) * | 2015-12-17 | 2016-05-25 | 广西大学 | Method for preparation of manganese sulfate by use of wood cellulose ester for catalytic processing of alkylation waste sulfuric acid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104961141A (en) * | 2015-06-12 | 2015-10-07 | 安徽东至广信农化有限公司 | Production process of ammonium sulfate |
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| CN105600826A (en) * | 2015-12-17 | 2016-05-25 | 广西大学 | Method for preparation of manganese sulfate by use of wood cellulose ester for catalytic processing of alkylation waste sulfuric acid |
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Application publication date: 20150520 |