CN1048841A - A kind of method of producing ammonium sulfate and utilizing ammonium sulfate production compound fertilizer - Google Patents

A kind of method of producing ammonium sulfate and utilizing ammonium sulfate production compound fertilizer Download PDF

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CN1048841A
CN1048841A CN 90105643 CN90105643A CN1048841A CN 1048841 A CN1048841 A CN 1048841A CN 90105643 CN90105643 CN 90105643 CN 90105643 A CN90105643 A CN 90105643A CN 1048841 A CN1048841 A CN 1048841A
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ammonium sulfate
liquor
calcium
production
waste liquid
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CN1020155C (en
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孙进林
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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
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05B—PHOSPHATIC FERTILISERS
    • C05B1/00—Superphosphates, i.e. fertilisers produced by reacting rock or bone phosphates with sulfuric or phosphoric acid in such amounts and concentrations as to yield solid products directly
    • C05B1/02—Superphosphates

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Abstract

The invention discloses a kind of method of producing ammonium sulfate and utilizing ammonium sulfate production compound fertilizer, (class is: vinylformic acid, acrylate, methacrylic acid, methacrylic ester to utilize two class industry, another kind of is the Wyler's process trimeric cyanamide) the production waste liquid, directly hybrid reaction is produced ammonium sulfate under normal temperature, normal pressure, utilize ammonium sulfate liquor coproduction of ammonia sulfate-Pu calcium simultaneously, as the raw material of producing compound fertilizer.Both solved the waste water pollution problem of two class industry, produced a large amount of ammonium sulfate again, and also saved a large amount of vitriol oils in the production process, synthetic ammonia and the energy (ammonium sulfate per ton is saved 0.258 ton of synthetic ammonia, 0.744 ton of vitriol oil, 1.3-1.5 ton steam).Has the huge social economic benefit.

Description

A kind of method of producing ammonium sulfate and utilizing ammonium sulfate production compound fertilizer
The present invention relates to a kind of chemical fertilizers production novel method, particularly utilize industry to dump thing and produce ammonium sulfate and produce compound fertilizer with ammonium sulfate.
For the sulphur ammonium, industrial production method (China Translation and Publishing Corporation, chemical fertilizer handbook, 1984) mainly contains following four kinds of methods:
(1) under vacuum or condition of normal pressure, synthetic ammonia and sulfuric acid react in saturex-vaporizer.
The problem that exists is to consume sulfuric acid and synthetic ammonia, and investment is big, the cost height.
(2) gashouse to pay method for product be with sulfuric acid scrubbing town gas or coke(oven)gas.This method has been saved synthetic ammonia than method (1), but consumes the vitriol oil, and complex process, investment are huge.
(3) volatile salt and phosphogypsum natural or that pay product or gypsum reaction.
The problem that method (3) exists is, consume synthetic ammonia and carbonic acid gas and be difficult to directly obtain solid ammonium sulfate, simultaneously, reclaims solid ammonium sulfate and need a large amount of steam from rarer solution, and complex process is invested hugely, and cost is also high.
(4) reclaim a pair product liquid sulfur ammonium, generally do not have crystallization sulphur ammonium solid, ammonium sulfate liquor content lower (about 40%), and evaporative process needs a large amount of steam.
And nitrogenous fertilizer and general calcium that existing method of producing compound fertilizer needs account for 80-90%, in addition the potash fertilizer of composite 10-20%.The thermal compensation because the reaction process of ammonium sulfate production compound fertilizer responds, help the drying of compound fertilizer product and can save dry required expense in some cases, simultaneously, the fertile physicochemical property of the compound that the sulphur ammonium is produced is good, therefore, ammonium sulfate remains produces compound fertilizer main raw material preferably, along with a large amount of uses of compound fertilizer, has aggravated the market shortages situation of ammonium sulfate.
The situation that problem that exists in view of above-mentioned existing production ammonium sulfate technology and production of compound fertilizer need ammonium sulfate in a large number the present invention seeks to:
-seek a kind of ammonium sulfate production method little, that cost is low of investing.
-with the direct coproduction of ammonia sulfate of ammonium sulfate liquor-Pu calcium, replace producing basic raw material ammonium sulfate, the general calcium of compound fertilizer, thus the production cost of compound fertilizer reduced.
-solve the spent acid severe contamination problem in present methacrylic acid, methacrylate, vinylformic acid, the acrylate production process.
Waste liquid in-solution trimeric cyanamide (melamine) production process: (urea-ammoniacal liquor) severe contamination problem.
Technical solution of the present invention is to utilize two class industry (class is: vinylformic acid, acrylate, methacrylic acid, methacrylate, another kind of is the Wyler's process trimeric cyanamide) the production waste liquid, directly hybrid reaction is produced sulfuric acid and is pressed under normal temperature, normal pressure.
Major ingredient (weight ratio) in the waste liquid of the methacrylic acid that the acetone cyanohydrin method is produced, methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate:
NH 4HSO 4: 40-55%; H 2SO 4: 20-42%; Superpolymer≤1%; Other is a water.
In the waste liquid of vinylformic acid, methyl acrylate, butyl acrylate (by weight):
NH 4HSO 4: 60-88%; H 2SO 4: 11-38%; Other is water and superpolymer.
Wyler's process is produced in the urea ammonia liquor of trimeric cyanamide, and major ingredient is:
Wherein contain N:20-33%
The chemical equation of above-mentioned urea ammonia liquor and above-mentioned monoammonium sulfate-sulfuric acid waste is as follows:
Above-mentioned reaction process is emitted heat, reacts when normal temperature, and temperature of charge can reach 40-80 ℃.
Its process flow sheet is as follows:
See Fig. 1.
Under normal temperature, the condition of normal pressure,, be the 3.0-6.0 scope, when preferably pH value is 3.5-5.0, the suspended substance on the ammonium sulfate liquor removed at pH value by the ratio of two kinds of waste liquids of pH value control.
Pilot scale, lab scale show that above-mentioned reaction yield is high, the crystalline sulfuric acid ammonium that directly obtains account for input two kinds of raw material summations 30-70%(by weight), simultaneously, the saturated ammonium sulphate mother liquor of by-product 10-60% also, utilize trade waste direct production ammonium sulfate, it is beat all that high like this productive rate is arranged.
For example:
Drop into: urea-ammoniacal liquor (1T)+butyl acrylate waste liquid (1.5T) →
(containing N:28%) (contains NH 4HSO 4: 85%; H 2SO 4: 14%)
Output: ammonium sulfate (solid)+saturated ammonium sulphate mother liquor
1.8T??0.4T
By weight, the solid ammonium sulfate of output account for drop into two kinds of raw materials and 72%, pay and produce a saturated ammonium sulphate mother liquor and account for 16%.
Again for example:
Drop into: urea-ammoniacal liquor (1T)+methyl methacrylate waste liquid (1.3T) →
(containing N:28%) (contains NH 4HSO 4: 55%; H 2SO 4: 40%)
Output: ammonium sulfate (solid)+saturated ammonium sulphate mother liquor
0.9T??1.1T
By weight, directly the solid ammonium sulfate of output account for input two kinds of raw materials and 39%, pay and produce a saturated ammonium sulphate mother liquor and account for 48%.
The present invention combines two kinds of waste liquids rightly, is the important means of producing the productive rate raising of ammonium sulfate.
To first kind industrial effluent, major ingredient is NH 4HSO 4, H 2SO 4, if use ammonia synthesis reaction, the cost height, with the ammoniacal liquor of general fertilizer plant discharging, then because concentration is low, thereby productive rate is low.
To the second class industrial effluent, promptly produce the waste liquid (urea ammonia liquor) that discharges in the trimeric cyanamide process, if absorb with the vitriol oil, cost height not only then, and also because the vitriol oil does not contain NH 4HSO 4, productive rate is also low.If with not containing NH 4HSO 4Sulfur waste acid, same productive rate is lower.
The further technology of another kind of the present invention is that above-mentioned saturated ammonium sulfate liquor (certainly, also can be the product-ammonium sulfate liquor of paying of other producer) is replaced the general calcium of aquatic product (normal superphosphate), is coproduction of ammonia sulfate-Pu calcium in fact.The consumption of ammonium sulfate liquor is about 2 times (strictly say, calculate by the water consumption that the water content in the ammonium sulfate liquor equals in the general calcium production) of the water consumption in the general calcium production.Ammonium sulfate liquor with ground phosphate rock and above-mentioned quantity mixes earlier, and again with strong sulfuric acid response, its reaction process and general calcium are produced similar.
Its technical process is as follows:
See Fig. 2
Lab scale, pilot scale show, the ammonium sulfate of being produced-Pu calcium, and physical and chemical performance well (contains N:6%, P 2O 5: 10%).
By above-mentioned flow process, producing under the identical consumption situation with general calcium, fully with general calcium processing method, voluminous 20-35% ammonium sulfate.Promptly produce the raw material consumption of 1 ton of general calcium, can produce ammonium sulfate-Pu calcium (wherein containing general calcium 1T) of 1.20-1.35T.
Contain N 〉=21% with the ammonium sulfate of aforesaid method production and meet national standard.The ammonium sulfate of coproduction-Pu calcium, general calcium wherein contains P 2O 5〉=14%, meet national standard, ammonium sulfate contains N 〉=21%, equally also meets national standard.By weight, general calcium accounts for 70-85%, and ammonium sulfate accounts for 15-30%.In addition, on probation through the farmland big area, fertilizer efficiency is good, and is harmless to farm crop.The first kind waste liquid that is utilized contains a small amount of superpolymer, and in the hybrid reaction process, forming scum silica frost can remove earlier, shows do not have other in the waste liquid to the farm crop nuisance by analysis.
The present invention has following effect: owing to directly utilize two kinds of waste liquid hybrid reactions, such reaction process is carried out under normal temperature, normal pressure, simple more than traditional method (1), (2), (3), (4) technology, control easily, thereby invest little (factory of steam is being arranged, only need 20,000 yuan in).Productive rate is unexpectedly high simultaneously, directly can obtain the solid ammonium sulfate of 30-75%, and need not consume steam.Again because waste liquid itself is cheap, so high efficiency (rate of profit is up to 40-80%).
Compare with above-mentioned 4 kinds of methods, the cost that the present invention produces ammonium sulfate is minimum.Because, contain higher monoammonium sulfate (40-88%) in the waste liquid of the vinylformic acid that is utilized, acrylate, methacrylic acid, methacrylic ester, replace sulfuric acid with monoammonium sulfate, see that from chemical reaction itself productive rate is just high, simultaneously, utilize the urea ammonia liquor (containing N:20-33%) of Wyler's process trimeric cyanamide discharging, it is also higher to contain the N amount, produce ammonium sulfate like this, can be under the situation that does not consume steam, direct crystallization goes out the sulphur ammonium solid of 30-75%, also pays the saturated ammonium sulphate mother liquor that produces 10-60% simultaneously.Can evaporate by traditional method (4) saturated ammonium sulfate liquor.But it is capable of reducing energy consumption by coproduction of ammonia sulfate of the present invention-Pu calcium.Because evaporation saturated ammonium sulphate mother liquor, ammonium sulfate product per ton needs 1.3-1.5 ton steam.Directly produce ammonium sulfate-Pu calcium, consuming under the identical prerequisite, can fecund go out the ammonium sulfate of 20-35%, because therefore the price of ammonium sulfate, can reduce general calcium production cost more than 30% than high nearly one times of general calcium with general calcium raw materials for production with the saturated ammonium sulphate mother liquor.Conclusion is got up, effect have following some:
1. less investment, output height:
The factory of steam is being arranged, only need acquire reactor, whizzer, pump, a small amount of utility appliance, less investment (in 20,000 yuan).Rate of profit is up to 40-80%.
2. produce 1500 tons of methyl methacrylates per year, near the factory that the trimeric cyanamide annual output is about 1200 tons, can produce 4000-5000 ton ammonium sulfate.Annual value of production can reach about 2,000,000 yuan, and annual return can reach 1,000,000 yuan.Can save synthetic ammonia 1000T-1250T, sulfuric acid: 3000-3750T.
3. solve the severe contamination problem of a large amount of spent acid of vinylformic acid, acrylate, methacrylic acid, the annual discharging of this class industry of methacrylic ester, simultaneously, also can solve the severe contamination problem of the waste liquid (urea-ammoniacal liquor) of trimeric cyanamide factory discharging.
4. there are the large and small vinylformic acid of nearly various schools of thinkers, acrylate, methacrylic acid, methacrylic ester factory in the whole nation, and annual the pollution by 2000 tons of spent acid of average every factory calculated, and the annual whole nation has about about 200,000 tons spent acid to pollute.The whole nation has tens tame melamine plant at present, and on average the annual waste liquid of pressing 5000T of each factory is discharged, and the annual waste liquor contamination that few hundred thousand tonnes of is arranged is approximately only administered above industry and polluted, and its benefit is that social benefit or economic benefit are all extremely considerable.
5, by participate in general calcium production directly with ammonium sulfate liquor, obtain sulphur ammonium-Pu calcium,, can save a large amount of energy consumption (sulphur ammonium per ton is saved 1.3-1.5T steam) for producing compound fertilizer.
The invention will be further described by the following examples
Example 1: with 1T Production of Cyanuramide waste liquid: urea-ammoniacal liquor (establish it and contain N:28%) adds butyl acrylate or vinylformic acid formicester waste liquid about 1.5T: (establish and contain NH 4HSO 4: 85%; H 2SO 4: 14%), at normal temperatures and pressures, make two kinds of waste liquid hybrid reactions, when reaction eases up, ammonium sulfate liquor takes a morsel, with the PH test paper it is tested, when pH value greater than 7 the time, it is an amount of to add monoammonium sulfate-sulfuric acid waste, when pH value less than 2 the time, it is an amount of to add urea-ammoniacal liquor, and when pH value was 3.0-6.5, reaction got final product.When being preferably in pH value and being 3.5-5.0, remove the scum silica frost that floats over the ammonium sulfate liquor top layer.At this moment, can get the about 1.8T of ammonium sulfate solids, simultaneously, can get saturated ammonium sulfate liquor and be about 0.4T, the saturated ammonium sulphate mother liquor is put into the saturated ammonium sulphate mother liquor tank, the saturated ammonium sulphate mother liquor is for producing ammonium sulfate-Pu calcium.
Example 2: produce ammonium sulfate-Pu calcium with ammonium sulfate liquor.The required raw material consumption of general calcium per ton is:
Ground phosphate rock (P 2O 5: 0.626T 33%)
Sulfuric acid (92.5%) 0.390T
Water 0.25T
Change into now:
Ground phosphate rock (P 2O 5: 0.626T 33%)
Sulfuric acid (92.5%) 0.390T
Saturated ammonium sulphate mother liquor 0.50T
(containing 50% sulphur ammonium)
Earlier ground phosphate rock (0.626T) and saturated ammonium sulphate mother liquor (0.5T) are mixed, react with the vitriol oil (0.39T), output 1.25T ammonium sulfate-Pu calcium promptly removes and produces 1 ton of P like this 2O 5Be outside 20% the general calcium, also have the ammonium sulfate crystallization of 0.25T to separate out simultaneously, be mixed in 1 ton the general calcium.Production technique is the same with general calcium.This method is utilized chemical process, whenever separates out 1 ton of ammonium sulfate, saves 1.3-1.5T steam.
Example 3: with 1T Production of Cyanuramide waste liquid: urea-ammoniacal liquor (establish and contain N:28%), the waste liquid that adds 1.3 tons methyl methacrylate (is established and is wherein contained NH 4HSO 4: 55%, H 2SO 4: 40%), under normal temperature, normal pressure, make two kinds of waste liquid hybrid reactions, survey pH value, add wherein a kind of waste liquid and make pH value, remove the scum silica frost that floats over the mother liquor top layer this moment at 3.5-5.0.Can obtain the about 0.9T of ammonium sulfate solids, also obtain about 1.1 tons saturated ammonium sulphate mother liquor, to ammonium sulfate liquor certainly by traditional method (4) evaporate, centrifugal, dry, solid ammonium sulfate that can about 0.5T.The N amount (containing N:21%) that contains of test ammonium sulfate.
Example 4: with the waste liquid of 1 ton of trimeric cyanamide: urea-ammoniacal liquor (establish it and contain N:20%), the waste liquid that adds about 0.9 ton methyl acrylate (contains NH 4HSO 4: 70%, H 2SO 4: 25%), at normal temperatures and pressures, make two kinds of waste liquid hybrid reactions, the control pH value is removed the scum silica frost that floats over the mother liquor top layer when 3.5-5.0, and can get 0.9 ton of ammonium sulfate solids this moment, also obtains 0.8 ton saturated ammonium sulphate mother liquor.This moment the solid ammonium sulfate productive rate account for drop into two kinds of raw material weights and 47%, pay and produce a saturated ammonium sulphate mother liquor and account for 42%.
Example 5: with the waste liquid of 1T trimeric cyanamide: urea-ammoniacal liquor (establish it and contain N:20%), the waste liquid that adds the 0.85T methacrylic acid (is established and is contained NH 4HSO 4: 60%, H 2SO 4: 35%), hybrid reaction is controlled pH value when 3.5-5.0 at normal temperatures and pressures, removes the scum silica frost on mother liquor top layer.Can get 0.9 ton of solid ammonium sulfate this moment, also can get 0.7 ton of saturated ammonium sulphate mother liquor, and solid ammonium sulfate is carried out centrifugal drying, just gets ammonium sulfate product.Pay product saturated ammonium sulphate mother liquor and can be sold to peasant's use.
Example 6: with 1 ton of urea-ammoniacal liquor (establish and contain N:20%), add the waste liquid of the Jia Jibingxisuanyizhi about about 1T, under normal temperature, normal pressure, hybrid reaction control pH value just can obtain ammonium sulfate at 3.0-6.5.
Example 7: with 1 ton of urea-ammoniacal liquor (establish and contain N:20%), the waste liquid that adds an amount of butyl methacrylate (contains NH 4HSO 4And H 2SO 4), hybrid reaction under normal temperature, normal pressure, control pH value just can get ammonium sulfate solids and saturated ammonium sulphate mother liquor at 3.0-6.5, to the saturated ammonium sulphate mother liquor can evaporate, centrifugal, dry, a part of again solid ammonium sulfate.
Look the different waste liquid of different sorts and effective component content, design the proportioning of two kinds of different waste liquids, only need the mother liquor pH value after the hybrid reaction is controlled at the scope of 3.0-6.5, and in this scope, suitably regulate pH value, but with regard to the suitable ammonium sulfate of production grain size.
Because this reaction process is thermopositive reaction, heat of reaction can also be recycled.

Claims (7)

1, a kind of method of producing ammonium sulfate and utilizing ammonium sulfate production compound fertilizer, (class is: vinylformic acid, acrylate, methacrylic acid, methacrylate to it is characterized in that utilizing two class industry, another kind of is the Wyler's process trimeric cyanamide) the production waste liquid, directly hybrid reaction is produced ammonium sulfate under normal temperature, normal pressure.
2, the waste liquid of vinylformic acid according to claim 1, CALCIUM ACRYLATE, methacrylic acid, methacrylate is characterized in that containing NH 4HSO 4And H 2SO 4, the waste liquid feature of Wyler's process trimeric cyanamide is to contain urea, ammoniacal liquor, volatile salt.
3, CALCIUM ACRYLATE according to claim 1 is vinylformic acid formicester, Butyl acrylate, and methacrylic ester is methymethacrylate, methacrylic acid second fat, methacrylic acid fourth fat.
4, according to the described method of claim 1, it is characterized in that the ratio of two kinds of waste liquids, be controlled at the scope of 3.0-6.5 by pH value, preferably scope is 3.5-5.0.
5, method according to claim 1 is characterized in that removing the suspended substance on ammonium sulfate liquor top layer when the ammonium sulfate liquor pH value after the hybrid reaction is 3.5-5.0.
6,, it is characterized in that with ammonium sulfate liquor coproduction of ammonia sulfate-Pu calcium according to right 1 described method.
7, according to claim 6, a kind of method of making ammonium sulfate-Pu calcium, its feature:
(1) ammonium sulfate liquor consumption (making wherein, water content equals water consumption in the general calcium production).
(2) earlier ground phosphate rock and an amount of ammonium sulfate liquor are mixed after, again with strong sulfuric acid response.
CN 90105643 1990-04-20 1990-04-20 Method for producing ammonium sulphate Expired - Fee Related CN1020155C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101643369B (en) * 2009-08-28 2012-04-18 洛阳市天誉环保工程有限公司 Process and device for producing (NH4)2SO4 fertilizer by using ammonium sulfite solution
CN106146104A (en) * 2016-08-23 2016-11-23 邯郸市同达矿用电器有限公司 Hopcalite agent waste liquid prepares the method for chemical fertilizer
CN107846900A (en) * 2015-06-19 2018-03-27 地球科学实验室 The chelating alkali product handled for water based systems and the method for preparing alkali product
US10807889B2 (en) 2015-06-19 2020-10-20 Earth Science Laboratories Chelating base product for use in water-based system treatments

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101265129B (en) * 2008-04-16 2010-09-01 江苏华昌化工股份有限公司 Composite nitrogen fertilizer

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101643369B (en) * 2009-08-28 2012-04-18 洛阳市天誉环保工程有限公司 Process and device for producing (NH4)2SO4 fertilizer by using ammonium sulfite solution
CN107846900A (en) * 2015-06-19 2018-03-27 地球科学实验室 The chelating alkali product handled for water based systems and the method for preparing alkali product
US10807889B2 (en) 2015-06-19 2020-10-20 Earth Science Laboratories Chelating base product for use in water-based system treatments
CN106146104A (en) * 2016-08-23 2016-11-23 邯郸市同达矿用电器有限公司 Hopcalite agent waste liquid prepares the method for chemical fertilizer

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