CN102530868A - Environmental-protection process method for removing ammonia from ammoxidation synthesis gas - Google Patents
Environmental-protection process method for removing ammonia from ammoxidation synthesis gas Download PDFInfo
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- CN102530868A CN102530868A CN2010106077901A CN201010607790A CN102530868A CN 102530868 A CN102530868 A CN 102530868A CN 2010106077901 A CN2010106077901 A CN 2010106077901A CN 201010607790 A CN201010607790 A CN 201010607790A CN 102530868 A CN102530868 A CN 102530868A
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Abstract
The invention provides an environmental-protection process method for removing ammonia from ammoxidation synthesis gas. The method is characterized in that a combined ammonia removal technological method composed of a primary ammonia removal process using phosphoric acid or ammonium dihydrogen phosphate and a fine ammonia removal process using sulfuric acid or ammonium bisulfate. In the primary ammonia removal process of ammoxidation synthesis gas, primary ammonia removal and ammonia recovery of the synthesis gas can be achieved through the repeated cycle of the following steps: phosphoric acid or ammonium dihydrogen phosphate absorbs free ammonia in the synthesis gas as a carrier in a primary ammonia removal tower, and is transformed to diammonium hydrogen phosphate; and diammonium hydrogen phosphate produces free ammonia in a desorption tower, and is transformed to ammonium dihydrogen phosphate. The ammoxidation synthesis gas enters a fine ammonia removal tower after the primary ammonia removal process, and fine ammonia removal process is achieved by using sulfuric acid or ammonium bisulfate as an absorber to absorb remaining ammonia in the synthesis gas after the primary ammonia removal process in a fine ammonia removal tower, wherein sulfuric acid or ammonium bisulfate is transformed to ammonium sulfate byproducts. The combined ammonia removal method can recover free ammonia in the ammoxidation synthesis gas to save resources and achieve real environmental protection property of the ammonia removal process, and has good economic and social benefits.
Description
Technical field
A kind of environment-protective process method that relates to the ammonia oxidation synthetic gas except that ammonia; Be meant the removal technological process for purifying of free ammonia in the reaction gas of the ammonia oxidation of carrying out for the ammonia source with ammonia after it is synthetic; Fully take into account the recycling of ammonia and the feature of environmental protection of technological process, belong to the environment-friendly clean process technological method.
Background technology
Oxidative ammonolysis is the process of knowing, and it is in the presence of ammoxidation catalyst, uses the organism pyrolytic conversion that ammonia and oxygen can ammonia oxidations to be prussiate.The technological value of oxidative ammonolysis is used such as having: by the propylene acrylonitrile production, by toluene system benzonitrile, by ortho position or paraxylene system phthalonitrile or Terephthalodinitrile, prepare prussic acid and hydrogen from methyl alcohol cyanic acid etc. by 3-picoline system 3-cyanopyridine and by methane; In these technological technological processs, the free ammonia of a great deal of is usually arranged in the synthesis gas behind the oxidative ammonolysis, after need separating or remove, these free ammonias just can carry out the purification of product or the reaction of step operation down.In existing industrial production, the removal of the free ammonia in the reaction mixture gas adopts the sulfuric acid neutralisation to remove mostly, removes respond well.But can produce a large amount of ammonium sulfate sub products owing to adopt the sulfuric acid neutralization to remove ammonia, ammonium sulfate is cheap and remove ammonia and need consume a large amount of sulfuric acid, and ammonia also has been consumed, and is ineffective; Also there are many kind and upright men to imagine the ammonia-removal method that adopts other on the industry; Try hard to ammonia is recycled: such as adopting phosphoric acid as absorption agent; Phosphoric acid is absorbed into Secondary ammonium phosphate, Secondary ammonium phosphate with free ammonia and obtains primary ammonium phosphate release ammonia through parsing again, thereby reaches the recycling of ammonia.Thisly realize as carrier the removal and the method for recycling of free ammonia in the synthetic gas can obtaining advantageous effects to a certain extent with phosphoric acid or primary ammonium phosphate, but owing to the stability of Secondary ammonium phosphate is limited; Therefore, the thoroughness that adopts phosphoric acid or primary ammonium phosphate to absorb its removal of free ammonia in the synthetic gas can't finely solve the also residual free ammonia that certain content is arranged in the synthetic gas after the processing; Especially in the temperature of the synthetic gas system after the processing under condition with higher, the content of residual free ammonia can be higher in the synthetic gas, is difficult to reach processing requirements; If the treatment temp ratio is lower, in the treatment solution system, can dissolve a certain amount of other material so, bring other unfavorable factor for parsing pre-treatment and resolving; Therefore being greatly limited property in actual production can not finely be promoted.
Summary of the invention
Deficiency to the technology of ammonia oxidation synthetic gas ammonia-removal process as stated; Adopt a kind of associating ammonia-removal process method; Both can well realize the recycling of ammonia, can handle the free ammonia in the synthetic gas very thorough again, realize the sufficient feature of environmental protection of technological process.
The purpose of this invention is to provide the environment-protective process method that a kind of ammonia oxidation synthetic gas removes ammonia, it is characterized in that adopting a kind of technology method of uniting, form by phosphoric acid or the elementary meticulous ammonia that removes of ammonia and sulfuric acid or monoammonium sulfate that removes of primary ammonium phosphate except that ammonia; The elementary ammonia that removes of ammonia oxidation synthetic gas; Adopt phosphoric acid or primary ammonium phosphate as carrier; At the elementary free ammonia that absorbs in the ammonia tower in the synthetic gas that removes, phosphoric acid or primary ammonium phosphate are converted into Secondary ammonium phosphate, and Secondary ammonium phosphate parses free ammonia in Analytic Tower; Be converted into primary ammonium phosphate again, circulation has realized the elementary recovery that removes ammonia and ammonia of synthetic gas so repeatedly; The ammonia oxidation synthetic gas is through elementary meticulous except that the ammonia tower except that getting into behind the ammonia again; The meticulous ammonia that removes is to adopt sulfuric acid or monoammonium sulfate as absorption agent; Meticulous elementary except that the residual ammonia in the synthetic gas behind the ammonia except that absorbing in the ammonia tower; Sulfuric acid or monoammonium sulfate convert the ammonium sulfate sub product into, realize the meticulous ammonia that removes of ammonia oxidation synthetic gas.
A kind of ammonia oxidation synthetic gas provided by the invention removes the environment-protective process method of ammonia; Be applicable to that all relate to the oxidative ammonolysis synthetic gas and remove the ammonia process, as prepare by the propylene acrylonitrile production, by toluene system benzonitrile, by ortho position or paraxylene system phthalonitrile or Terephthalodinitrile, by 3-picoline system 3-cyanopyridine and by the methane ammonia oxidation oxidative ammonolysis synthetic gas such as prussic acid and methanol ammonoxidation hydrogen manufacturing cyanic acid except that the ammonia process; Can realize the recycling of free ammonia in the ammonia oxidation synthetic gas, promptly can economize on resources and can realize the real feature of environmental protection of ammonia-removal process extraordinary economic benefit and social benefit being arranged.
A kind of ammonia oxidation synthetic gas provided by the invention removes the environment-protective process method of ammonia, and its practical implementation step is following:
The first step: the elementary ammonia that removes of ammonia oxidation synthetic gas, realize the recycling of free ammonia.
The ammonia oxidation synthetic gas gets into the elementary ammonia tower that removes, and phosphoric acid or ammonium dihydrogen phosphate aqueous solution are converted into ammonium dibasic phosphate aqueous solution at the elementary free ammonia that absorbs in the synthetic gas in the ammonia tower that removes, and the ammonia oxidation synthetic gas is realized the elementary ammonia that removes.Reaction equation is following:
NH
3+H
3PO
4——→NH
4H
2PO
4
NH
3+NH
4H
2PO
4——→(NH
4)
2HPO
4
The absorption tower device that ammonium dihydrogen phosphate aqueous solution absorbs the free ammonia in the ammonia oxidation synthetic gas generally is divided into two sections; Primary ammonium phosphate content is higher relatively in the epimere circulating absorption solution of absorption tower, and the concentration of Secondary ammonium phosphate is higher relatively in the hypomere circulating absorption solution of absorption tower; Effusive absorption liquid is the approaching ammonium dibasic phosphate aqueous solution completely that transforms from bottom, hypomere absorption tower.After epimere circulating absorption solution circulation in absorption tower absorbs ammonia, flow to the hypomere absorption tower, in the hypomere absorption tower, continue circulation again and absorb ammonia, flow out near transforming ammonium dibasic phosphate aqueous solution completely from bottom, hypomere absorption tower at last from the bottom on epimere absorption tower.
Ammonium dibasic phosphate aqueous solution is resolved release ammonia and is converted primary ammonium phosphate in Analytic Tower, primary ammonium phosphate returns the elementary ammonia tower that removes again and recycles repeatedly; The ammonia water that discharges absorbs and obtains the recycling that ammoniacal liquor is used for ammonia.Reaction equation is following:
(NH
4)
2HPO
4——→NH
4H
2PO
4+NH
3↑
Ammonium dibasic phosphate aqueous solution is resolved release ammonia and is obtained ammonia soln in Analytic Tower; Ammonia soln is through the ammonia separating and reclaiming device; Obtain directly to be used for the raw material ammonia of ammonia oxidation building-up reactions, realized the recycling and the cleaner production of ammonia oxidation synthesis technique of free ammonia.
The ammonia oxidation synthetic gas can remove in the reaction gas 95% or above free ammonia through the elementary ammonia that removes, and adopts this technical matters, can recycle 95% or above ammonia.
The elementary residual volume except that ammonia behind the ammonia of ammonia oxidation synthetic gas determines with removing factors such as ammonia temperature, pressure environment and ammonium dibasic phosphate solution stability, and is not fairly obvious with free ammonia content relation in the ammonia oxidation synthetic gas; Even there is more free ammonia also can well be reclaimed in the synthetic gas through the elementary ammonia that removes.Therefore in implementing the actual production of ammonia oxidation building-up reactions; Can be on the reaction raw materials proportioning ratio of suitable increase ammonia; The side reaction that can suppress very effectively in the ammonia oxidation building-up reactions takes place; Improve overall yield and quality product, solved the consumption of ammonia and the contradiction of quality product and product yield well.
Second step: the meticulous ammonia that removes of ammonia oxidation synthetic gas obtains removing ammonia ammonia oxidation synthetic gas comparatively completely.
Get into the meticulous ammonia tower that removes again through the elementary ammonia oxidation synthetic gas that removes behind the ammonia, adopt sulfuric acid or monoammonium sulfate as absorption agent, at the meticulous ammonia that absorbs the remnants in the synthetic gas in the ammonia tower that removes, sulfuric acid or monoammonium sulfate convert the ammonium sulfate sub product into.Reaction equation is following:
2NH
3+H
2SO
4——→(NH
4)
2SO
4
NH
3+NH
4HSO
4——→(NH
4)
2SO
4
Because ammonium sulfate is highly stable in system, can obtain our needed synthetic gas system with realizing the meticulous ammonia that removes except that free ammonia remaining in the ammonia oxidation synthetic gas behind the ammonia absorbs more completely through phosphate system is elementary, be used for going on foot down and handle with synthetic.Since in the elementary synthetic gas system of removing behind the ammonia amount of remaining free ammonia have only handle before the free ammonia amount 5% or below; So the amount of producing ammonium sulfate byproduct have only simple 5% when handling with sulfuric acid absorption or below; This just greatly reduces the market pressure and the vitriolic consumption of producing ammonium sulfate byproduct; Also greatly reduce simultaneously the treatment capacity of producing ammonium sulfate byproduct, practiced thrift energy consumption, realized cleaning technique production.
Technical matters provided by the invention has following characteristic:
1. the present invention is divided into two steps with the removal of the middle free ammonia of ammonia oxidation synthetic gas and carries out, and two combination of steps are removed the thorough removal that ammonia is realized free ammonia in recycling and the synthetic gas of free ammonia; Practice thrift raw material ammonia and raw material sulphuric acid, practiced thrift material cost.
2. unite except that ammonia can make the envrionment conditions of ammonia oxidation synthetic gas in removing the ammonia operation and becoming friendly relatively, material has obtained good improvement to equipment corrosion, when practicing thrift facility investment, can prolong the work-ing life of equipment.
3. unite except that ammonia under the prerequisite that economizes on resources, can be very effective the realization environment-protecting clean produce, well solved the environmental protection difficult problem in the existing ammonia oxidation synthesis and production process, broken through the environmental technology barrier of ammonia oxidation synthesis and production process industrialized development.
4. adopt and unite the efficient recovery that to realize ammonia except that ammonia; Can be in ammonia oxidation building-up reactions proportioning raw materials the ratio of suitable increase ammonia; Can effectively suppress the side reaction in the ammonia oxidation building-up reactions; Improve overall yield and quality product, well solved the consumption of ammonia and the contradiction of quality product.
Description of drawings
Figure of description is that the oxidative ammonolysis synthetic gas that the present invention relates to is united the schematic flow sheet except that ammonia.
Embodiment
Illustrate in greater detail the present invention through embodiment below, but scope of the present invention does not receive the restriction of embodiment.
Embodiment: prussic acid is synthesized in the ammonia oxidation of iS-One method Sweet natural gas, and reacting synthesis gas is not contained ammonia or contains the reacting synthesis gas body of constant ammonia through uniting except that ammonia.
Component such as the following table of certain synthetic gas before removing ammonia:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 0.08092 | 6 | N 2 | 0.54328 |
| 2 | NH 3 | 0.01508 | 7 | CO 2 | 0.00503 |
| 3 | H 2O | 0.25513 | 8 | CO | 0.04705 |
| 4 | CH 4 | 0.00462 | 9 | H 2 | 0.04765 |
| 5 | O 2 | 0.00020 | 10 | Other | 0.00104 |
Synthetic gas is realized obtaining the elementary ammonia synthesis gas that removes, elementary component such as the following table of removing ammonia synthesis gas after the recycling of free ammonia through the elementary ammonia that removes:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 0.089855 | 6 | N 2 | 0.608716 |
| 2 | NH 3 | 0.000679 | 7 | CO 2 | 0.005631 |
| 3 | H 2O | 0.182415 | 8 | CO | 0.052714 |
| 4 | CH 4 | 0.005181 | 9 | H 2 | 0.053388 |
| 5 | O 2 | 0.000225 | 10 | Other | 0.001196 |
The elementary ammonia that removes is 95.497% except that the ammonia rate.Ammonium dihydrogen phosphate absorbs ammonia and is converted into ammonium hydrogen phosphate solution, through the recovery of parsing with ammonia; The ammonium dihydrogen phosphate circulation that parses is used for the absorption of ammonia, reclaims ammonia and is used for the ammonia oxidation raw material; The elementary recycling that has realized ammonia except that ammonia.
The elementary ammonia synthesis gas that removes obtains the meticulous ammonia synthesis gas that removes, meticulous component such as the following table of removing ammonia synthesis gas through meticulous after removing ammonia by-product sulfate of ammoniac again:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 0.091558 | 6 | N 2 | 0.621532 |
| 2 | NH 3 | 0.000012 | 7 | CO 2 | 0.005853 |
| 3 | H 2O | 0.166567 | 8 | CO | 0.053628 |
| 4 | CH 4 | 0.005225 | 9 | H 2 | 0.054168 |
| 5 | O 2 | 0.000231 | 10 | Other | 0.001226 |
Meticulous remove ammonia to remove the ammonia rate be 98.233%; Monoammonium sulfate or sulphuric acid soln absorb ammonia and are converted into ammoniumsulphate soln, and ammoniumsulphate soln obtains the ammonium sulfate sub product through purifying treatment and condensing crystal.
The ammonia oxidation synthetic gas removes the ammonia step through two and realizes uniting except that ammonia, has not only realized the recycling of ammonia but also realized the removal of ammonia in the synthetic gas.
Claims (3)
1. an ammonia oxidation synthetic gas removes the environment-protective process method of ammonia, it is characterized in that adopting a kind of technology method of uniting except that ammonia, removes by phosphoric acid or primary ammonium phosphate are elementary that ammonia and sulfuric acid or monoammonium sulfate are meticulous to be formed except that ammonia; The elementary ammonia that removes of ammonia oxidation synthetic gas; Adopt phosphoric acid or primary ammonium phosphate as carrier; At the elementary free ammonia that absorbs in the ammonia tower in the synthetic gas that removes, phosphoric acid or primary ammonium phosphate are converted into Secondary ammonium phosphate, and Secondary ammonium phosphate parses free ammonia in Analytic Tower; Be converted into primary ammonium phosphate again, circulation has realized the elementary recovery that removes ammonia and ammonia of synthetic gas so repeatedly; The ammonia oxidation synthetic gas is through elementary meticulous except that the ammonia tower except that getting into behind the ammonia again; The meticulous ammonia that removes is to adopt sulfuric acid or monoammonium sulfate as absorption agent; Meticulous elementary except that the residual ammonia in the synthetic gas behind the ammonia except that absorbing in the ammonia tower; Sulfuric acid or monoammonium sulfate convert the ammonium sulfate sub product into, realize the meticulous ammonia that removes of ammonia oxidation synthetic gas.
2. the said a kind of ammonia oxidation synthetic gas of claim 1 removes the environment-protective process method of ammonia; It is characterized in that being applicable to that all relate to the ammonia process of removing of oxidative ammonolysis synthetic gas, as prepare by the propylene acrylonitrile production, by toluene system benzonitrile, by ortho position or paraxylene system phthalonitrile or Terephthalodinitrile, by 3-picoline system 3-cyanopyridine and by the methane ammonia oxidation oxidative ammonolysis synthetic gas such as prussic acid and methanol ammonoxidation hydrogen manufacturing cyanic acid except that the ammonia process.
3. the described elementary ammonia-removal method of claim 1; The absorption tower device that it is characterized in that the free ammonia in the ammonium dihydrogen phosphate aqueous solution absorption ammonia oxidation synthetic gas generally is divided into two sections; Primary ammonium phosphate content is higher relatively in the epimere circulating absorption solution of absorption tower; The concentration of Secondary ammonium phosphate is higher relatively in the hypomere circulating absorption solution of absorption tower, and effusive absorption liquid is the approaching ammonium dibasic phosphate aqueous solution completely that transforms from bottom, hypomere absorption tower; After absorption tower epimere circulating absorption solution circulation absorbed ammonia, from the inflow hypomere absorption tower, bottom on epimere absorption tower, the continuation circulation absorbed ammonia in the hypomere absorption tower again, at last from the approaching ammonium dibasic phosphate aqueous solution completely that transforms of bottom, hypomere absorption tower outflow.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864105A (en) * | 2012-12-18 | 2014-06-18 | 英威达科技公司 | Enhanced methane control for Andrussow process |
| CN106698344A (en) * | 2015-11-16 | 2017-05-24 | 宁夏琪凯节能设备有限公司 | Energy saving technical process for ammonia removal of ammonia oxidation synthesis gas |
| CN110280104A (en) * | 2019-06-24 | 2019-09-27 | 天华化工机械及自动化研究设计院有限公司 | A kind of phosphorus ammonium method processing catalyst ammonia-contaminated gas and ammonia reclaiming process |
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2010
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Patent Citations (2)
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| CN101027252A (en) * | 2004-07-22 | 2007-08-29 | 伊内奥斯美国公司 | Process for recovery and recycle of ammonia from a vapor stream |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864105A (en) * | 2012-12-18 | 2014-06-18 | 英威达科技公司 | Enhanced methane control for Andrussow process |
| CN103864105B (en) * | 2012-12-18 | 2018-04-17 | 英威达纺织（英国）有限公司 | Methane control for the enhancing of Andrussow methods |
| CN106698344A (en) * | 2015-11-16 | 2017-05-24 | 宁夏琪凯节能设备有限公司 | Energy saving technical process for ammonia removal of ammonia oxidation synthesis gas |
| CN110280104A (en) * | 2019-06-24 | 2019-09-27 | 天华化工机械及自动化研究设计院有限公司 | A kind of phosphorus ammonium method processing catalyst ammonia-contaminated gas and ammonia reclaiming process |
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