CN104649298A - Production method of ammonium sulfate - Google Patents

Production method of ammonium sulfate Download PDF

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Publication number
CN104649298A
CN104649298A CN201410159944.3A CN201410159944A CN104649298A CN 104649298 A CN104649298 A CN 104649298A CN 201410159944 A CN201410159944 A CN 201410159944A CN 104649298 A CN104649298 A CN 104649298A
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ammonium sulfate
saturex
product
ammoniacal liquor
crystallization
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CN201410159944.3A
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CN104649298B (en
Inventor
王伟男
邹骏
彭光文
罗小华
谭绍栋
邓军生
石继东
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Liuzhou Iron and Steel Co Ltd
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Liuzhou Iron and Steel Co Ltd
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Abstract

The invention discloses a production method of ammonium sulfate, which comprises the following steps: A, reacting coke oven gas and ammonia gas with a sulfuric acid solution in a spray area of a saturator so as to obtain a product a; B, guiding aqueous ammonia into an overflow tank to react with a sulfuric acid solution so as to obtain a product b, and conveying the product b to the inside of the saturator by a small mother liquor circulating pump to react with the sprayed sulfuric acid solution in the spray area of the saturator, so that a product c is obtained; C, feeding the product a and the product c into a crystallization area of the saturator, so that ammonium sulfate in the product a and the product c is gradually crystallized and separated out; D, conveying ammonium sulfate-containing crystallizing liquid to the inside of a crystallizing elevated tank from a crystallizing liquid outlet by a crystallizing pump; and E, conveying the crystallizing liquid in the crystallizing elevated tank to a centrifugal machine to separate, and conveying precipitates obtained by separating to a dryer to dry, so that ammonium sulfate is obtained. According to the invention, an ammonium sulfate product is produced by taking aqueous ammonia produced in the process of ammonia washing implemented by using phosphoric acid as a raw material, so that the problem that aqueous ammonia produced in the process of ammonia washing implemented by using phosphoric acid is surplus is solved.

Description

The production method of ammonium sulfate
Technical field
The present invention relates to ammonium sulfate production technical field, especially a kind of coke-oven gas that utilizes washes the method for the ammoniacal liquor production ammonium sulfate that ammonia is produced by phosphoric acid.
Background technology
Coke-oven gas is the flammable mixed gas of the one that produces in process of coking, usually adopts sulfuric acid to wash ammonia and phosphoric acid and washes ammonia in ammonia two kinds of processing method purifying coke oven gas; Wherein adopt saturex sulfuric acid to wash ammonia process method to produce ammonium sulfate, ammonium sulfate can directly export trade; The ammoniacal liquor that phosphorus ammonium method utilizes the ammonia in coke-oven gas to produce, ammoniacal liquor provides nitrogenous source for the desulfurization of sintering ammonia, realizes the treatment of wastes with processes of wastes against one another.At present, in Liu Gang coke-oven plant purifying coke oven gas, the production line of ammonia comprises three cover phosphoric acid and washes ammonia equipment and a set of saturex sulfuric acid washes ammonia equipment, and the configuration of this production line causes the output of ammoniacal liquor to be much higher than the demand of sintering flue gas desulfurization operation, causes ammoniacal liquor to waste.
Summary of the invention
The object of this invention is to provide a kind of method that strong aqua can be used to be preparing ammonium sulfate, the production method of this ammonium sulfate can solve the problem that amount that phosphoric acid washes the ammoniacal liquor that ammonia operation is produced is greater than the demand of sintering ammonia desulfurization process.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: the production method of this ammonium sulfate, use a kind of ammonium sulfate production equipment, this ammonium sulfate production equipment comprises the saturex being provided with coke-oven gas import and coke-oven gas outlet, is provided with mutually through mixing zone, spray district and crystallizing field in described saturex from top to bottom successively; Described gas inlet and the outlet of described coke-oven gas are positioned at the mixing zone of described saturex, crystal solution outlet is provided with bottom the crystallizing field of described saturex, described crystal solution exports the inlet communication by crystallization pump and crystallization header tank, the outlet of described crystallization header tank is communicated with moisture eliminator by whizzer, and the liquid outlet of described whizzer is communicated with the liquid inlet being located at described saturex and spraying district;
Have a top to be provided with overflow groove that fluid inlet and bottom are provided with liquid outlet, the fluid inlet of described overflow groove is communicated with the overflow port being located at described saturex and spraying district, the liquid outlet of described overflow groove is communicated with the fluid inlet being located at described saturex top by little Recycling Mother Solution pump, described overflow groove is provided with the conduit that is stretched out its overflow groove end face, described conduit is communicated with ammoniacal liquor delivery trunk by multiple ammoniacal liquor flowrate control valve, wherein an ammoniacal liquor flowrate control valve fluid inlet with the pipeline between liquid outlet is connected with an isocon be communicated with by two ammoniacal liquor flowrate control valves, ammoniacal liquor under meter is provided with between described isocon and two described ammoniacal liquor flowrate control valves,
Comprise following operation steps:
A, coke-oven gas and be transported to saturex respectively from the ammonia that Coking Plant Wastewater is evaporated mixing zone in mix, mixed gas enters described saturex spray district and is obtained by reacting product a with the sulphuric acid soln sprayed;
B, from ammoniacal liquor delivery trunk input ammoniacal liquor import overflow groove by conduit, be obtained by reacting product b with the sulphuric acid soln in overflow groove; Described product b is transported in saturex by little Recycling Mother Solution pump, is obtained by reacting product c in described saturex spray district with the sulphuric acid soln sprayed;
The described product a and step B that C, steps A are obtained by reacting is obtained by reacting the crystallizing field that described product c enters described saturex, and in described crystallizing field, moisture evaporates along with the rising of temperature, the ammonium sulfate crystallization gradually in described product a and product c;
D, crystal solution containing ammonium sulfate crystallization are transported in crystallization header tank from the crystal solution outlet bottom the crystallizing field of described saturex by crystallization pump;
E, be separated being delivered to whizzer containing the crystal solution of described ammonium sulfate crystallization in crystallization header tank, separating obtained supernatant liquor returns in saturex, is separated the throw out obtained and is delivered to moisture eliminator and carries out being drying to obtain ammonium sulfate.
In such scheme, scheme is more specifically: the concentration of ammoniacal liquor described in step B is 9% ~ 15%, and the concentration of described sulphuric acid soln is 2% ~ 3%; The flow importing the ammoniacal liquor of overflow groove from described conduit is 2m 3/ h ~ 3m 3/ h.
Further, the liquid outlet of the described conduit of described ammonium sulfate production equipment is positioned at lower 0.7 meter ~ 0.9 meter of the liquid level of described overflow groove sulphuric acid soln.
Owing to have employed technique scheme, the present invention compared with prior art has following beneficial effect:
1, the present invention original with coke-oven gas be preparing ammonium sulfate basis on increase ammoniacal liquor again as raw materials for production, phosphoric acid is washed the unnecessary ammoniacal liquor importing overflow groove that ammonia operation produces, and react with the sulphuric acid soln in overflow groove and generate ammonium sulfate, not only improve the output of ammonium sulfate, and solve the problem of ammoniacal liquor excess production capacity; Use ammoniacal liquor under meter monitoring ammoniacal liquor flow simultaneously, guarantee the stable of the ammonia vol importing overflow groove and ammonium sulfate crystallization, normally the carrying out of discharging; 2, invention increases coke-oven gas quality, and reduce production cost, current Liu Gang coke-oven plant ammonium sulfate stable yield, and can according to Production requirement flexible at about 2800 tons/month.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention.
Embodiment
Below in conjunction with Fig. 1 and specific examples, the invention will be further described:
Embodiment 1:
A kind of production method of ammonium sulfate, use a kind of ammonium sulfate production equipment as shown in Figure 1, this ammonium sulfate production equipment comprises ammonium sulfate production equipment and comprises the saturex 1 being provided with coke-oven gas import 101 and coke-oven gas outlet 103, is provided with mutually through mixing zone 107, spray district 108 and crystallizing field 109 in saturex 1 from top to bottom successively; The coke-oven gas import 101 of saturex 1 is positioned at the sidewall of the mixing zone 107 of saturex 1, the coke-oven gas outlet 103 of saturex 1 is positioned at the top of the mixing zone 107 of saturex 1, bottom the crystallizing field 109 of saturex 1, be provided with two crystal solution outlet 106, crystal solution outlet 106 is by pipeline and crystallization pump 6 inlet communication with crystallization header tank 8; The outlet of crystallization header tank 8 is communicated with moisture eliminator 10 with whizzer 7 by pipeline, and whizzer 7 is provided with liquid outlet and crystallization outlet, and the liquid outlet of whizzer 7 is communicated with the liquid inlet 104 being contained in saturex 1 and spraying district 108 by pipeline; Overflow groove 2 is provided with top and is provided with fluid inlet 201 and bottom liquid outlet 202, and fluid inlet 201 is communicated with the overflow port being located at saturex 1 and spraying district 108 sidewall by pipeline; The liquid outlet 202 of overflow groove 2 is communicated with the fluid inlet 102 being located at saturex 1 top with little Recycling Mother Solution pump 3 by pipeline, is also provided with the fluid inlet 105 be communicated with the ammonia output tube 17 evaporated from coking plant wastewater at the top of saturex 1; Overflow groove 2 is provided with the conduit 11 that is stretched into overflow groove 2 inside, and the liquid outlet of the conduit 11 of the present embodiment is positioned at lower 0.7 meter of liquid level, with guarantee to enter ammoniacal liquor in overflow groove 2 can with the sulphuric acid soln complete reaction of overflow groove 2; The present embodiment conduit 11 is communicated with ammoniacal liquor delivery trunk 16 by two ammoniacal liquor flowrate control valves, wherein an ammoniacal liquor flowrate control valve 13 fluid inlet with the pipeline between liquid outlet is connected with an isocon 14 be communicated with by two ammoniacal liquor flowrate control valves 12, the isocon 14 between two ammoniacal liquor flowrate control valves 12 is equipped with ammoniacal liquor under meter 15.
The production of ammonium sulfate comprises following operation steps:
A, coke-oven gas and be transported to saturex respectively from the ammonia that Coking Plant Wastewater is evaporated mixing zone in mix, it is that 2% sulphuric acid soln is obtained by reacting product a with the concentration sprayed that mixed gas enters saturex spray district;
B, from ammoniacal liquor delivery trunk input concentration be that the ammoniacal liquor of 9% is with 2m 3the flow of/h imports overflow groove by conduit, then with the concentration in overflow groove be 2% sulphuric acid soln be obtained by reacting product b, product b is transported in saturex by little Recycling Mother Solution pump, and the sulphuric acid soln being 2% with the concentration sprayed in saturex spray district is obtained by reacting product c;
Be obtained by reacting the crystallizing field that product c enters saturex in the product a be obtained by reacting in C, steps A and step B, in crystallizing field, moisture evaporates along with the rising of temperature, the ammonium sulfate crystallization gradually in product a and product c;
D, crystal solution containing ammonium sulfate crystallization are transported in crystallization header tank from the crystal solution outlet bottom the crystallizing field of saturex by crystallization pump;
E, be separated being delivered to whizzer containing the crystal solution of ammonium sulfate crystallization in crystallization header tank, separating obtained supernatant liquor returns in saturex, is separated the throw out obtained and is delivered to moisture eliminator and carries out being drying to obtain ammonium sulfate.
Embodiment 2:
The production of ammonium sulfate comprises following operation steps:
A, coke-oven gas and be transported to saturex respectively from the ammonia that Coking Plant Wastewater is evaporated mixing zone in mix, mixed gas enters the sulphuric acid soln that saturex spray district and the concentration sprayed are 3% and is obtained by reacting product a;
B, from ammoniacal liquor delivery trunk input concentration be that the ammoniacal liquor of 15% is with 3m 3the flow of/h imports overflow groove by conduit, the sulphuric acid soln being 3% with the concentration in overflow groove is obtained by reacting product b, product b is transported in saturex by little Recycling Mother Solution pump, and the sulphuric acid soln being 3% with the concentration sprayed in saturex spray district is obtained by reacting product c;
Be obtained by reacting the crystallizing field that product c enters saturex in the product a be obtained by reacting in C, steps A and step B, in crystallizing field, moisture evaporates along with the rising of temperature, the ammonium sulfate crystallization gradually in product a and product c;
D, crystal solution containing ammonium sulfate crystallization are transported in crystallization header tank from the crystal solution outlet bottom the crystallizing field of saturex by crystallization pump;
E, be separated being delivered to whizzer containing the crystal solution of ammonium sulfate crystallization in crystallization header tank, separating obtained supernatant liquor returns in saturex, is separated the throw out obtained and is delivered to moisture eliminator and carries out being drying to obtain ammonium sulfate.
The liquid outlet of the conduit 11 of the present embodiment ammonium sulfate production equipment is positioned at lower 0.9 meter of liquid level, and other features are identical with embodiment 1.

Claims (3)

1. a production method for ammonium sulfate, is characterized in that:
Use a kind of ammonium sulfate production equipment, this ammonium sulfate production equipment comprises the saturex being provided with coke-oven gas import and coke-oven gas outlet, is provided with mutually through mixing zone, spray district and crystallizing field in described saturex from top to bottom successively; Described gas inlet and the outlet of described coke-oven gas are positioned at the mixing zone of described saturex, crystal solution outlet is provided with bottom the crystallizing field of described saturex, described crystal solution exports the inlet communication by crystallization pump and crystallization header tank, the outlet of described crystallization header tank is communicated with moisture eliminator by whizzer, and the liquid outlet of described whizzer is communicated with the liquid inlet being located at described saturex and spraying district;
Have a top to be provided with overflow groove that fluid inlet and bottom are provided with liquid outlet, the fluid inlet of described overflow groove is communicated with the overflow port being located at described saturex and spraying district, the liquid outlet of described overflow groove is communicated with the fluid inlet being located at described saturex top by little Recycling Mother Solution pump, described overflow groove is provided with the conduit that is stretched out its overflow groove end face, described conduit is communicated with ammoniacal liquor delivery trunk by multiple ammoniacal liquor flowrate control valve, wherein an ammoniacal liquor flowrate control valve fluid inlet with the pipeline between liquid outlet is connected with an isocon be communicated with by two ammoniacal liquor flowrate control valves, ammoniacal liquor under meter is provided with between described isocon and two described ammoniacal liquor flowrate control valves,
Comprise following operation steps:
A, coke-oven gas and be transported to saturex respectively from the ammonia that Coking Plant Wastewater is evaporated mixing zone in mix, mixed gas enters described saturex spray district and is obtained by reacting product a with the sulphuric acid soln sprayed;
B, from ammoniacal liquor delivery trunk input ammoniacal liquor import overflow groove by conduit, be obtained by reacting product b with the sulphuric acid soln in overflow groove; Described product b is transported in saturex by little Recycling Mother Solution pump, is obtained by reacting product c in described saturex spray district with the sulphuric acid soln sprayed;
The described product a and step B that C, steps A are obtained by reacting is obtained by reacting the crystallizing field that described product c enters described saturex, and in described crystallizing field, moisture evaporates along with the rising of temperature, the ammonium sulfate crystallization gradually in described product a and product c;
D, crystal solution containing ammonium sulfate crystallization are transported in crystallization header tank from the crystal solution outlet bottom the crystallizing field of described saturex by crystallization pump;
E, be separated being delivered to whizzer containing the crystal solution of described ammonium sulfate crystallization in crystallization header tank, separating obtained supernatant liquor returns in saturex, is separated the throw out obtained and is delivered to moisture eliminator and carries out being drying to obtain ammonium sulfate.
2. the production method of a kind of ammonium sulfate according to claim 1, is characterized in that: the concentration of ammoniacal liquor described in step B is 9% ~ 15%, and the concentration of described sulphuric acid soln is 2% ~ 3%; The flow importing the ammoniacal liquor of overflow groove from described conduit is 2m 3/ h ~ 3m 3/ h.
3. the production method of a kind of ammonium sulfate according to claim 1, is characterized in that, the liquid outlet of the described conduit of described ammonium sulfate production equipment is positioned at lower 0.7 meter ~ 0.9 meter of the liquid level of described overflow groove sulphuric acid soln.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105197962A (en) * 2015-09-30 2015-12-30 芜湖新兴铸管有限责任公司 Ammonium sulfate crystallization equipment
CN105271305A (en) * 2015-09-29 2016-01-27 山东钢铁股份有限公司 Method for treating ammonia water obtained after ammonia distillation of residual ammonia water
CN105329868A (en) * 2015-10-30 2016-02-17 东华工程科技股份有限公司 Method for recycling ammonia and hydrogen from ammonia synthesizing tail gas
CN105833705A (en) * 2016-05-19 2016-08-10 泰州百力化学股份有限公司 Saturated-reactor-process ammonia waste gas treatment device and process thereof
CN108658096A (en) * 2017-03-31 2018-10-16 上海宝钢化工有限公司 Ammonium sulfate production method using coke oven gas as raw material
CN113044856A (en) * 2021-03-23 2021-06-29 李文娟 Method for preparing ammonium sulfate by using coke oven gas

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CN102951657A (en) * 2012-12-10 2013-03-06 张卫东 Process and equipment for producing ammonium sulfate by taking sulfur pulp and ammonia water as raw materials
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271305A (en) * 2015-09-29 2016-01-27 山东钢铁股份有限公司 Method for treating ammonia water obtained after ammonia distillation of residual ammonia water
CN105197962A (en) * 2015-09-30 2015-12-30 芜湖新兴铸管有限责任公司 Ammonium sulfate crystallization equipment
CN105329868A (en) * 2015-10-30 2016-02-17 东华工程科技股份有限公司 Method for recycling ammonia and hydrogen from ammonia synthesizing tail gas
CN105833705A (en) * 2016-05-19 2016-08-10 泰州百力化学股份有限公司 Saturated-reactor-process ammonia waste gas treatment device and process thereof
CN108658096A (en) * 2017-03-31 2018-10-16 上海宝钢化工有限公司 Ammonium sulfate production method using coke oven gas as raw material
CN108658096B (en) * 2017-03-31 2021-11-05 宝武炭材料科技有限公司 Ammonium sulfate production method using coke oven gas as raw material
CN113044856A (en) * 2021-03-23 2021-06-29 李文娟 Method for preparing ammonium sulfate by using coke oven gas

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