CN101554998A - Method for preparing sulfur trioxide by utilizing gypsum and equipment system thereof - Google Patents

Method for preparing sulfur trioxide by utilizing gypsum and equipment system thereof Download PDF

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CN101554998A
CN101554998A CNA2008100625290A CN200810062529A CN101554998A CN 101554998 A CN101554998 A CN 101554998A CN A2008100625290 A CNA2008100625290 A CN A2008100625290A CN 200810062529 A CN200810062529 A CN 200810062529A CN 101554998 A CN101554998 A CN 101554998A
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gypsum
ammonium sulfate
ammonia
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CN101554998B (en
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陈明顺
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Hangzhou Guardian Industry Co., Ltd.
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Abstract

The invention relates to a method for preparing sulfur trioxide by utilizing gypsum and an equipment system thereof, aiming to provide a new technology which takes phosphogypsum or fluorine gypsum (also including ordinary gypsum) as raw materials to prepare the sulfur trioxide, and the matched equipment system thereof. The invention comprises the following steps: (1) double decomposition reaction: gypsum slurry is added into ammonium bicarbonate or carbonized ammonia water for reacting to obtain ammonium sulfate solution and calcium carbonate; then the steps of (2) dewater treatment, (3) concentration treatment, (4) mixing ammonia distillation treatment and (5) reductive decomposition reaction are sequentially carried out on the ammonium sulfate solution, and a sulfur trioxide gas product is obtained.

Description

Utilize gypsum to produce the method and the device systems thereof of sulphur trioxide
Technical field
The present invention relates to a kind of sulphur trioxide preparation method, specifically is a kind of method and device systems thereof that utilizes gypsum to produce sulphur trioxide.
Background technology
Phosphogypsum, fluorgypsum are the wastes of phosphorous chemical industry, are never effectively handled for a long time and utilize now qualitative become " Hazardous wastes ".And preparing the method for sulphur trioxide in the prior art, sulphur commonly used, sulfurous gas (CN1384805), oleum (ZL85109395) etc. are raw material.And the method for utilizing phosphogypsum or fluorgypsum to prepare sulphur trioxide is not appeared in the newspapers.
Summary of the invention
The technical issues that need to address of the present invention are, overcome the existing deficiency of prior art, and providing a kind of is raw material with phosphogypsum or fluorgypsum (also comprising common gypsum), produces the new technology of sulphur trioxide.
Another technical problem that the present invention need solve is, providing one, what can effectively move is raw material with phosphogypsum or fluorgypsum (also comprising common gypsum), produces the device systems of sulphur trioxide.
Gypsum of the present invention is common gypsum, phosphogypsum or fluorgypsum.Wherein (main component is CaSO to phosphogypsum 42H 2O content is more than 60%) be the waste residue of producing phosphate fertilizer, be with sulfuric acid and Rock Phosphate (72Min BPL) reaction, the waste residue that is produced during Wet-process phosphoric acid (WPPA); Fluorgypsum is with fluorite (CaF 2) and sulfuric acid (H 2SO 4) produce the waste residue in hydrofluoric acid (HF) process; Terra alba is meant the starting material of exploitation gained in the plaster of paris ore deposit, after pulverizing, is processed into dehydrated gyp-, semi-hydrated gypsum or crude original breeze etc.
The present invention utilizes gypsum to produce the method for sulphur trioxide, it is characterized in that carrying out according to the following steps:
(1) replacement(metathesis)reaction: in sealed reactor (1), water ratio is 20%～80% calcium plaster adding bicarbonate of ammonia, or gypsum adding carbonated aqueous ammonia, and fully stirring reaction obtains ammonium sulfate solution and lime carbonate;
Gypsum (dry measure): the mol ratio of bicarbonate of ammonia is 1: 1～3;
Gypsum (being generally powdery): the mol ratio of carbonated aqueous ammonia is 1: 1～3.
(2) processed: the mixture that step (1) is obtained carries out solid-liquid separation, obtains lime carbonate byproduct and ammonium sulfate solution;
(3) concentration: the ammonium sulfate solution that step (2) is obtained carries out evaporation concentration, makes ammonium sulfate solution become crystalline sulfuric acid ammonium (solid-state);
(4) mixing, ammonia still process are handled: add ferric oxide in the ammonium sulfate that step (3) obtains, the mol ratio of ammonium sulfate and ferric oxide is 1: 0.1～1, behind thorough mixing in the blender, enter among the process furnace I and react under 150 ℃～300 ℃ temperature, obtain solid-state ferric sulfate and ammonia (or become byproduct, maybe can be recycled);
(5) reduction decomposition reaction: the ferric sulfate that step (4) is obtained heat in process furnace II and carries out the reduction decomposition reaction, begins decomposition after the ferric sulfate decomposition temperature, obtains sulfur trioxide gas product and ferric oxide (can be recycled).
Step (1) calcium plaster also can be that phosphogypsum or fluorgypsum obtain through washing, and the water ratio of calcium plaster is 20%～80%.
The soup compound of the present invention after with terra alba or discarded phosphogypsum, fluorgypsum washing is raw material and bicarbonate of ammonia or carbonated aqueous ammonia generation replacement(metathesis)reaction, generates ammonium sulfate and lime carbonate, and reaction formula is as follows respectively:
React with bicarbonate of ammonia:
CaSO 4·2H 2O+2NH 4HCO 3→CaCO 3+CO 2+(NH 4) 2SO 4+3H 2O
Or and carbonated aqueous ammonia reaction:
CaSO 4·2H 2O+(NH 3·H 2O+NH 4OH)+CO 2→CaCO 3+(NH 4) 2SO 4+3H 2O。
Lime carbonate wherein forms byproduct after dehydration, oven dry; Ammonium sulfate mixes, carries out ammonia still process again and handle behind dehydration, condensing crystal with ferric oxide, generate ferric sulfate and discharge ammonia, and reaction formula is as follows:
3(NH 4) 2SO 4+Fe 2O 3→Fe 2(SO 4) 3+6NH 3+3H 2O。
The ferric sulfate that obtains carries out the reduction decomposition reaction again, is heated to decomposition temperature, generates ferric oxide and sulphur trioxide, and reaction formula is as follows:
Fe 2(SO 4) 3→Fe 2O 3+3SO 3。
The device systems that utilizes gypsum to produce sulphur trioxide of the present invention is characterized in that: reservoir I, one or more parallel connection of reactor, band filter, reservoir II, the three-effect evaporation and condensation device of being furnished with squirt pump, blender, process furnace I, process furnace II, heat exchanger II cooperates successively or connect; A carbonating tower is connected with process furnace I by heat exchanger I, also is connected with reactor by pipeline.
In the present device system,, add water and can synthesize carbonated aqueous ammonia again by carbonating tower and utilize once more from the carbonic acid gas of reactor with from the ammonia of process furnace I.Ferric oxide from the reduction decomposition reaction also can be recycled.The present invention can realize fundamentally economizing on resources with the recycle of water, ammonia and ferric oxide, reduces the production cost of sulphur trioxide.
The advantage of preparation method of the present invention is that one can digest a large amount of discarded phosphogypsums, fluorgypsum (terra alba); Two can utilize the carbonic acid gas of outside discharging to join the synthetic carbonated aqueous ammonia of carbonating tower, play the purpose that reduces Greenhouse effect; Ammonia in three bicarbonate of ammonia that add and ferric oxide can recycles, help reducing production costs; The 4th, the technology circuit is rationally ripe, helps industrialization production.
Description of drawings
Fig. 1 is that the present invention adds ammonium bicarbonate method and produces the sulphur trioxide process route view;
Fig. 2 is that the present invention adds the carbonated aqueous ammonia legal system and gets the sulphur trioxide process route view;
Fig. 3 is that the present invention produces sulphur trioxide device systems synoptic diagram.Major equipment and basic role thereof in the system:
Reactor 1---carry out replacement(metathesis)reaction, obtain ammonium sulfate solution and lime carbonate;
Band filter 2---carry out processed, isolate the lime carbonate byproduct, get ammonium sulfate solution;
Reservoir I 3---the solution (containing a spot of ammonium sulfate solution) behind the lime carbonate is cleaned in storage, can add water to reactor;
Reservoir II 4---storage ammonium sulfate solution;
Squirt pump 5---make evaporation concentrator 6 be in negative pressure state, improve dewatering efficiency;
Evaporation concentrator 6---make ammonium sulfate solution become the crystalline sulfuric acid ammonium;
Blender 7---crystalline sulfuric acid ammonium and ferric oxide are carried out uniform mixing;
Process furnace I 8---carry out ammonia still process and handle, ammonium sulfate is decomposed, produce ammonia and ferric sulfate;
Heat exchanger I 9---the high temperature ammonia is carried out thermal exchange, cooling;
Carbonating tower 10---system is in negative pressure under the state of bleeding, and carries out the synthetic of carbonated aqueous ammonia (being ammonia, carbonic acid gas and water);
Process furnace II 11---carry out the reduction decomposition reaction, make ferric sulfate be decomposed into sulfur trioxide gas and ferric oxide.
Heat exchanger II 12---sulfur trioxide gas is cooled off, reclaims.
Embodiment
Below by embodiment technical scheme of the present invention is described in further detail.
It is as follows that phosphogypsum of the present invention, fluorgypsum are washed the processing general step: (adopting terra alba not need to wash processing)
(a) washing process of phosphogypsum, fluorgypsum carries out twice cleaning in the cement pond, mainly removes the water-soluble P in phosphogypsum and the fluorgypsum 2O 5, F -With the organism that is suspended on the water surface, by the phosphogypsum post precipitation, take out top liquid, obtain the soup compound (controlling moisture content≤50%) of sedimentary phosphogypsum and water.
(b) adopt a plurality of cement pond to clean, circulating water treatment technology causes the P in the aqueous solution after long-time water treatment 2O 5, F -Bring up to one regularly with organic concentration, available lime neutralizes, and utilizes [Ca 3(PO 4) 2] and the precipitation principle of CaF, purifying, the water after the purification can be reused.
The general step of preparation method of the present invention is as follows:
(1) replacement(metathesis)reaction: replacement(metathesis)reaction is carried out in the reactor of sealing, working temperature is under 30 ℃～50 ℃ state, calcium plaster of post precipitation (controlling moisture content≤50%) and bicarbonate of ammonia (or carbonated aqueous ammonia) are added in molar ratio, adopt slurry formula alr mode, mixing speed is at 30～80 rev/mins, and the reaction times was at 0.5～2 hour.Obtain ammonium sulfate [(NH 4) 2SO 4] the aqueous solution and lime carbonate (CaCO 3), the carbonic acid gas (CO that reaction generates 2) the gas carbonating tower that enters the back carries out the synthetic of carbonated aqueous ammonia, so carbonic acid gas (CO 2) gas do not have loss.
(2) processed: the mixture after the replacement(metathesis)reaction is put into band filter, carry out processed, reach solid-liquid separation; After the processed, form lime carbonate byproduct and ammonium sulfate solution.
(3) concentration: the ammonium sulfate solution after the processed is joined in the evaporation concentrator, utilize steam heating, vacuumize, quicken concentration process, shorten concentration time, make ammonium sulfate become crystallization with the venturi vacuum device.
(4) mix, ammonia still process handles: being content 70%～99% crystalline sulfuric acid ammonium adds ferric oxide according to 1: 0.34 mol ratio, behind the mixing tank thorough mixing, in Reaktionsofen (with electrically heated, inflammable gas heating, coal heating, coke heating etc.), controlled temperature is under 150 ℃～300 ℃ state, ammonium sulfate is decomposed, produce ammonia and ferric sulfate; Wherein ammonia is behind heat exchanger, makes the ammonia cooling, forms the liquefied ammonia byproduct through pressurization and/or freezing back, and remaining is solid-state ferric sulfate.
(5) reduction decomposition reaction: the solid-state ferric sulfate heating that obtains, temperature is under 350 ℃～600 ℃ state, ferric sulfate is decomposed, produce sulfur trioxide gas and ferric oxide, sulfur trioxide gas is recycled into product after heat exchanger cooling, ferric oxide can come back to step (4) mixing, ammonia still process is made starting material usefulness in handling, so ferric oxide does not have loss.
The present invention produces embodiment (according to mass parts).
Embodiment 1---and phosphogypsum is produced sulphur trioxide (using ammonium bicarbonate method)
See Fig. 1, Fig. 3.Phosphogypsum carries out twice cleaning in the cement pond, mainly remove the solubility P in the phosphogypsum 2O 5, F -With the organism that is suspended on the water surface, phosphogypsum post precipitation, take out top liquid, obtain the calcium plaster (controlling moisture content is≤50%) that sedimentary phosphogypsum and water mix.
(1) replacement(metathesis)reaction: in the reactor 1 of band paddle agitator, (main component is CaSO through 1 part of phosphogypsum after the washing 42H 2O content is 82%, and is not moisture), add bicarbonate of ammonia (NH 4HCO 3Content is 98%) 1.2 parts, reaction is 1 hour under 30 ℃～50 ℃ temperature, obtains lime carbonate and ammonium sulfate [(NH 4) 2SO 4] the aqueous solution.
(2) processed: filter with band filter 2, carry out solid, liquid two-phase and separate, separate the lime carbonate byproduct, ammonium sulfate solution enters reservoir II 4.
(3) concentration: after ammonium sulfate solution concentrates with the evaporation concentrator 6 of being furnished with squirt pump 5, obtain 0.6 part of the crystallization of ammonium sulfate.
(4) mixing, ammonia still process are handled: the ammonium sulfate crystallization that obtains adds ferric oxide (Fe 2O 3Content is 95%) 0.3 part in blender 7, mix after, advance among the process furnace I 8 and react, controlled temperature is 150 ℃～300 ℃, the reaction times is 0.5 hour, obtains ammonia (byproduct) and ferric sulfate [Fe 2(SO 4)] 0.606 part.
(5) reduction decomposition reaction: the ferric sulfate [Fe that obtains 2(SO 4)], use heat again at process furnace II 11, impel ferric sulfate to decompose.All decompose at 480 ℃～600 ℃, obtain 0.36 part of ferric oxide (can move into blender 7 recycles) and sulfur trioxide gas, through heat exchanger II 12 cool off reclaim product.
Embodiment 2---and terra alba is produced sulphur trioxide (using ammonium bicarbonate method)
(1) replacement(metathesis)reaction: 1 part of plaster of paris breeze (CaSO 42H 2O content is 88%), particle diameter is below 50um), add bicarbonate of ammonia (NH 4HCO 3Content is 98%) 1.2 parts.In the reactor 1 of band paddle agitator, reaction is 1 hour under 30 ℃～50 ℃ the temperature, obtains lime carbonate and ammonium sulfate [(NH 4) 2SO 4] the aqueous solution.
(2) processed: filter with band filter 2, carry out solid, liquid two-phase and separate, separate the lime carbonate byproduct, ammonium sulfate solution enters reservoir II 4.
(3) concentration: after ammonium sulfate solution concentrates with the evaporation concentrator 6 of being furnished with squirt pump 5, obtain 0.68 part of the crystallization of ammonium sulfate.
(4) mixing, ammonia still process are handled: the ammonium sulfate crystallization that obtains adds ferric oxide (Fe 2O 3Content is 95%) 0.33 part, after in blender 7, mixing, advance among the process furnace I 8 and react, controlled temperature is 150 ℃～300 ℃, the reaction times is 0.5 hour, obtains ammonia (byproduct) and ferric sulfate [Fe 2(SO 4)] 0.687 part.
(5) reduction decomposition reaction: the ferric sulfate [Fe that obtains 2(SO 4)], use heat again at process furnace II 11, impel ferric sulfate to decompose.All decompose at 480 ℃～600 ℃, obtain 0.41 part of ferric oxide (can move into blender 7 recycles) and sulfur trioxide gas, through heat exchanger II 12 cool off reclaim product.
Embodiment 3---and terra alba is produced sulphur trioxide (adding the carbonated aqueous ammonia method)
See Fig. 2, Fig. 3.Add 1 part of 2 parts of ammonia, carbonic acid gas by carbonating tower 10 and become saturated solution (unsaturated solution can make speed of response slow down) with hydration; 1 part of plaster of paris breeze (CaSO 42H 2O content is 90%), particle diameter is below 50um) get the raw materials ready.
(1) replacement(metathesis)reaction: 1 part of plaster of paris breeze and 3.7 parts of carbonated aqueous ammonias, in the reactor 1 of band paddle agitator, reaction is 2 hours under 30 ℃～50 ℃ temperature, obtains lime carbonate (byproduct separation) and ammonium sulfate [(NH 4) 2SO 4] aqueous solution.
(2) processed: filter with band filter 2, carry out solid, liquid two-phase and separate, separate the lime carbonate byproduct, ammonium sulfate solution enters reservoir II 4.
(3) concentration: after ammonium sulfate solution concentrates with the evaporation concentrator 6 of being furnished with squirt pump 5, obtain 0.66 part of the crystallization of ammonium sulfate.
(4) mixing, ammonia still process are handled: the ammonium sulfate crystallization that obtains adds ferric oxide (Fe 2O 3Content is 95%) 0.32 part in blender 7, mix after, advance among the process furnace I 8 and react, controlled temperature is 150 ℃～300 ℃, the reaction times is 0.5 hour, obtains ammonia (delivering to carbonating tower 10 through heat exchanger I 9) and ferric sulfate [Fe 2(SO 4)] 0.667 part.
(5) reduction decomposition reaction: the ferric sulfate [Fe that obtains 2(SO 4)], use heat again at process furnace II 11, impel ferric sulfate to decompose.All decompose at 480 ℃～600 ℃, obtain 0.40 part of ferric oxide (can move into blender 7 recycles) and sulfur trioxide gas, through heat exchanger II 12 cool off reclaim product.

Claims (3)

1, a kind of method of utilizing gypsum to produce sulphur trioxide is characterized in that carrying out according to the following steps:
(1) replacement(metathesis)reaction: in sealed reactor (1), water ratio is 20%～80% calcium plaster adding bicarbonate of ammonia, or gypsum adding carbonated aqueous ammonia, and fully stirring reaction obtains ammonium sulfate solution and lime carbonate;
Gypsum: the mol ratio of bicarbonate of ammonia is 1: 1～3;
Gypsum: the mol ratio of carbonated aqueous ammonia is 1: 1～3.
(2) processed: the mixture that step (1) is obtained carries out solid-liquid separation, obtains lime carbonate byproduct and ammonium sulfate solution;
(3) concentration: the ammonium sulfate solution that step (2) is obtained carries out evaporation concentration, makes ammonium sulfate solution become the crystalline sulfuric acid ammonium;
(4) mixing, ammonia still process are handled: add ferric oxide in the ammonium sulfate that step (3) obtains, the mol ratio of ammonium sulfate and ferric oxide is 1: 0.1～1, behind the thorough mixing of blender (7) lining, enters process furnace I (8), under temperature of reaction, react, obtain solid-state ferric sulfate and ammonia;
(5) reduction decomposition reaction: the ferric sulfate that step (4) is obtained heat among process furnace II (11) and carries out reduction decomposition and react, and begins decomposition after the ferric sulfate decomposition temperature, obtains sulfur trioxide gas product and ferric oxide.
2, the method for utilizing gypsum to produce sulphur trioxide according to claim 1 is characterized in that described calcium plaster is that phosphogypsum or fluorgypsum obtain through washing.
3, a kind of device systems that utilizes gypsum to produce sulphur trioxide is characterized in that: reservoir I (3), one or more parallel connection of reactor (1), band filter (2), reservoir II (4), the three-effect evaporation and condensation device (6) of being furnished with squirt pump (5), blender (7), process furnace I (8), process furnace II (11), heat exchanger II (12) cooperates successively or connect; A carbonating tower (10) is connected with process furnace I (8) by heat exchanger I (9), also is connected with reactor (1) by pipeline.
CN2008100625290A 2008-06-20 2008-06-20 Method for preparing sulfur trioxide by utilizing gypsum and equipment system thereof Expired - Fee Related CN101554998B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102564890A (en) * 2011-12-27 2012-07-11 浙江天蓝环保技术股份有限公司 Method for detecting content of sulfur trioxide in gypsum
CN102976645A (en) * 2012-12-13 2013-03-20 泰山石膏股份有限公司 Pretreatment method of phosphogypsum for production of thistle board
CN110697731A (en) * 2019-11-05 2020-01-17 浙江浙能技术研究院有限公司 Method for preparing ammonium sulfate and calcium carbonate from desulfurized gypsum
CN113731113A (en) * 2021-09-15 2021-12-03 北京工大环能科技有限公司 System for reducing blockage of ammonium bisulfate of air preheater of coal-fired power plant
CN115124062A (en) * 2022-06-23 2022-09-30 国能(山东)能源环境有限公司 Desulfurization gypsum resource comprehensive utilization system and process

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES478382A1 (en) * 1978-04-02 1979-11-01 Abdel Fattah Sabry Hosein Kame Process for recovering sulphuric acid from natural gypsum or phospho-gypsum.
CN1095055A (en) * 1993-05-08 1994-11-16 曾繁威 Produce the novel process of vitriolate of tartar and ammonium chloride with the phosphogypsum conversion method
CN1099723A (en) * 1993-08-31 1995-03-08 张智新 Decomposition for ammonium sulfate

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102564890A (en) * 2011-12-27 2012-07-11 浙江天蓝环保技术股份有限公司 Method for detecting content of sulfur trioxide in gypsum
CN102564890B (en) * 2011-12-27 2013-09-04 浙江天蓝环保技术股份有限公司 Method for detecting content of sulfur trioxide in gypsum
CN102976645A (en) * 2012-12-13 2013-03-20 泰山石膏股份有限公司 Pretreatment method of phosphogypsum for production of thistle board
CN102976645B (en) * 2012-12-13 2016-03-02 泰山石膏股份有限公司 A kind of pretreatment process of phosphogypsum for production of thistle board
CN110697731A (en) * 2019-11-05 2020-01-17 浙江浙能技术研究院有限公司 Method for preparing ammonium sulfate and calcium carbonate from desulfurized gypsum
CN113731113A (en) * 2021-09-15 2021-12-03 北京工大环能科技有限公司 System for reducing blockage of ammonium bisulfate of air preheater of coal-fired power plant
CN115124062A (en) * 2022-06-23 2022-09-30 国能(山东)能源环境有限公司 Desulfurization gypsum resource comprehensive utilization system and process
CN115124062B (en) * 2022-06-23 2023-12-01 国能(山东)能源环境有限公司 Desulfurization gypsum recycling comprehensive utilization system and process

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