CN103073027A - Environment-friendly clean production method for high purity sodium cyanide - Google Patents
Environment-friendly clean production method for high purity sodium cyanide Download PDFInfo
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- CN103073027A CN103073027A CN 201110326860 CN201110326860A CN103073027A CN 103073027 A CN103073027 A CN 103073027A CN 201110326860 CN201110326860 CN 201110326860 CN 201110326860 A CN201110326860 A CN 201110326860A CN 103073027 A CN103073027 A CN 103073027A
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- ammonia
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Abstract
The invention provides an environment-friendly clean production method for high purity sodium cyanide. The production method comprises the following steps that: without removal of ammonia, hydrocyanic acid synthetic gas synthesized through ammoxidation is directly absorbed by and reacts with an aqueous sodium hydroxide solution to obtain a high purity aqueous sodium cyanide solution, and free ammonia remains in tail gas; the aqueous sodium cyanide solution is cooled and blended to obtain a high purity liquid sodium cyanide product, the high purity liquid sodium cyanide product undergoes condensation, crystallization and centrifugation to obtain a high purity solid sodium cyanide product, and mother liquor is indiscriminately used in liquid alkali absorption liquor; phosphoric acid or ammonium biphosphate is employed as a carrier for repeated cyclic indiscriminate application of ammonia so as to recover ammonia in the tail gas; and after recovery of ammonia, the tail gas is purified and absorbed with water or the aqueous sodium hydroxide solution, a small amount of the aqueous hydrocyanic acid solution or a crude aqueous sodium cyanide solution product is obtained while the tail gas is purified, the purified tail gas is burned with a tail gas boiler, and the aqueous hydrocyanic acid solution or the crude aqueous sodium cyanide solution product is indiscriminately used in the liquid alkali absorption liquor.
Description
Technical field
A kind of production method that relates to sodium cyanide, refer to that and aqueous sodium hydroxide solution reaction direct at the synthetic prussic acid mixed gas of the ammonia oxidation of carrying out as the ammonia source take ammonia obtains the environment-friendly clean process production method of high-purity sodium cyanide, fully take into account the recycle and reuse of ammonia and the feature of environmental protection of technological process, belong to recycling economy environment-protecting clean production technology method.
Background technology
The reaction of the synthetic prussic acid of ammonia oxidation is the process of knowing, and it is in the presence of ammoxidation catalyst, and organism pyrolytic conversion that can ammonia oxidation with ammonia and oxygen is prussic acid; The technological value of the synthetic prussic acid of ammonia oxidation is used more extensive: mainly contain the methane prepared by ammoxidation and prepare prussic acid, the standby prussic acid of light oil cracking prepared by ammoxidation etc. for prussic acid, methanol ammonoxidation; The synthetic prussic acid mixed gas of ammonia oxidation obtains sodium cyanide with the aqueous sodium hydroxide solution reaction again.The free ammonia that a great deal of is usually arranged in the synthesis gas behind the oxidative ammonolysis in existing technical matters process of producing sodium cyanide, adopts to separate first or remove and just carries out aqueous sodium hydroxide solution behind the free ammonia absorption reaction of prussic acid is obtained sodium cyanide.Because except also having a certain amount of carbonic acid gas in the prussic acid mixed gas behind the ammonia, in absorption process, inevitably sneak in the sodium cyanide solution with sodium hydroxide reaction generation yellow soda ash, the yellow soda ash separating difficulty that is mixed with in the sodium cyanide is large, therefore has a strong impact on the quality of sodium cyanide product; Be mixed with the sodium cyanide product of yellow soda ash, in the process of synthetic derived product, affect product yield on the one hand, also having a strong impact on the quality of sodium cyanide derived product.For obtaining high-purity sodium cyanide, also have after separating or removing free ammonia, contained prussic acid in the water absorption of gases carries out rectifying to absorption liquid again and obtains high purity liquid prussic acid, obtains the high purity liquid sodium cyanide with the aqueous sodium hydroxide solution reaction again.This technique has increased plant investment, energy consumption and consumption of raw materials.
Summary of the invention
For the deficiency of Sodium Cyanide Production Technology as mentioned above, adopt a kind of new producing and manufacturing technique, not only can obtain carbonate content enough trace high-purity sodium cyanide product but also can well realize the recycling of ammonia, realize that resource takes full advantage of the environment-friendly clean process production of Mode of Circular.
The environment-friendly clean process production method that the purpose of this invention is to provide a kind of high-purity sodium cyanide, it is characterized in that adopting the synthetic prussic acid reactant gases of ammonia oxidation directly and the aqueous sodium hydroxide solution absorption reaction obtain the environment-friendly clean process production method of high-purity sodium cyanide, the prussic acid reactant gases that contain free ammonia synthetic by ammonia oxidation obtaining high-purity sodium cyanide solution without removing the ammonia process with regard to direct and aqueous sodium hydroxide solution absorption reaction, obtains high purity liquid sodium cyanide product by cooling off allotment; High-purity sodium cyanide solution obtains high purity solid sodium cyanide product by concentrated, crystallization, centrifugation, and mother liquid recycle is in sodium hydroxide absorption reaction liquid; Absorb free ammonia and remain in the tail gas, again tail gas is carried out the recycling of ammonia; Tail gas behind the recovery ammonia purifies rear burning again.
The environment-friendly clean process production method of a kind of high-purity sodium cyanide provided by the invention, its implementation step is as follows:
The first step: the prussic acid in aqueous sodium hydroxide solution or sodium hydroxide and sodium cyanide crude product (prussic acid) the mixed aqueous solution absorbing ammonia oxidation synthetic gas, produce high purity liquid sodium cyanide or high purity solid sodium cyanide.
The ammonia oxidation synthetic gas enters reactor, and the prussic acid in the synthetic gas and the reaction of the sodium hydroxide in the absorption liquid generate sodium cyanide; Reaction equation is as follows:
NaOH+HCN→NaCN+H
2O
As above contain free ammonia in the ammonia oxidation synthetic gas of reaction, the ammonia oxidation synthetic gas is in the absorption process that does not have through the prussic acid that directly carries out except the ammonia operation; Free ammonia in the ammonia oxidation synthetic gas remains in behind absorption reaction in the tail gas, carries out the recycling of free ammonia when vent gas treatment again.
This process is a simple absorption reaction process, but key is that what how to guarantee to obtain is high-purity sodium cyanide solution; The inventor herein is according to the nature and characteristic of such prussic acid building-up reactions gas, what propose pointedly environmental stress that this absorption reaction process system adopts suitable control absorption reaction system and temperature cooperates to realize this purpose: absorption reaction environmental system pressure is 0.0-0.08MPa (gauge pressure), and temperature is 60 ℃-200 ℃.Experimental results show that at this patent and describe the reaction that absorption reaction system absorption reaction under pressure and temperature environment as above can suppress carbonic acid gas and sodium hydroxide, carbonate content in the sodium cyanide solution that obtains is effectively controlled, thereby provides foundation for producing high-purity sodium cyanide solution.
The inventor herein also finds in the aqueous sodium hydroxide solution to carry out in the absorption reaction process under absorption reaction system environment as above when containing a certain amount of carbonate, and carbonate can be replaced by hydrogen root or hydroxide radical and be formed release of carbonate dioxide out; Therefore, the aqueous sodium hydroxide solution that this absorption reaction adopts allows and suitable contain yellow soda ash and do not affect the high-quality performance of product that is to say can be relatively loose to the specification of quality of sodium hydroxide raw material; As everyone knows, always contain a certain amount of yellow soda ash in the sodium hydroxide raw material of supplying on the market (no matter being liquid product or solid phase prod).
Above-mentioned absorption reaction has obtained highly purified sodium cyanide solution, obtains high purity liquid sodium cyanide product by the cooling allotment; Obtain high-purity sodium cyanide solid phase prod by concentrated, crystallization, centrifugal, drying, crystalline mother solution directly or after purifying cover use in the sodium hydroxide absorption reaction liquid.
Second step: phosphoric acid or ammonium dihydrogen phosphate aqueous solution are being converted into ammonium dibasic phosphate aqueous solution except the free ammonia in the absorption tail gas in the ammonia tower, and tail gas is realized the recycle and reuse of ammonia.Reaction equation is as follows:
NH
3+H
3PO
4→NH
4H
2PO
4
NH
3+NH
4H
2PO
4→(NH
4)
2HPO
4
The absorption tower device of the free ammonia in phosphoric acid or the ammonium dihydrogen phosphate aqueous solution absorption tail gas generally is divided into two sections; Determining ammonium biphosphate content is relatively high in the epimere circulating absorption solution of absorption tower, and the relative concentration of Secondary ammonium phosphate is higher in the hypomere circulating absorption solution of absorption tower; The absorption liquid that flows out from bottom, hypomere absorption tower transforms completely ammonium dibasic phosphate aqueous solution for approaching.Behind the absorption tower epimere circulating absorption solution circulation absorbing ammonia, flow to the hypomere absorption tower from the bottom on epimere absorption tower, in the hypomere absorption tower, continue again the circulation absorbing ammonia, flow out to approach from bottom, hypomere absorption tower at last and transform completely ammonium dibasic phosphate aqueous solution.
Ammonium dibasic phosphate aqueous solution is resolved release ammonia and is converted to primary ammonium phosphate in Analytic Tower, primary ammonium phosphate returns elementary except the use of ammonia tower iterative cycles again; The ammonia water that discharges absorbs and obtains the recycling that ammoniacal liquor is used for ammonia.Reaction equation is as follows:
(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 by the ammonia separating and reclaiming device, obtain to be directly used in the raw material ammonia of ammonia oxidation building-up reactions, realized the recycling of free ammonia and the cleaner production of high-purity sodium cyanide.
Because the tail gas temperature out is relatively low, the free ammonia in the tail gas can be absorbed comparatively thoroughly, can reach the recovery requirement of environmental protection fully, and the rate of recovery of free ammonia reaches more than 99%.
The 3rd step: the tail gas after ammonia reclaims adopts water or aqueous sodium hydroxide solution to purify absorption again, and remaining prussic acid is purified and gathers in the crops simultaneously a small amount of hydrocyanic acid aqueous solution or the sodium cyanide crude product aqueous solution in the tail gas, and the tail gas after the purification burns with the tail gas boiler.
NaOH+HCN→NaCN+H
2O
Although the amount of remaining free hydrogen cyanic acid is very limited in the tail gas system, because prussic acid belongs to highly toxic substance; We must carry out purifying treatment to tail gas, also can gather in the crops a small amount of hydrocyanic acid aqueous solution or the sodium cyanide crude product aqueous solution simultaneously; The hydrocyanic acid aqueous solution that obtains or the sodium cyanide crude product aqueous solution directly cover are used in the absorbing by liquid caustic soda liquid, and the tail gas after the purifying treatment send the tail gas burning boiler to burn again.
Tail gas clean-up is processed in the crude product sodium cyanide solution that obtains and is contained a certain amount of yellow soda ash, the crude product sodium cyanide solution is blended in the absorbing by liquid caustic soda liquid jointly as absorption reaction liquid, in the absorption reaction process of under the first step absorption reaction system environment, carrying out, carbonate can be replaced by cyanogen root or hydroxide radical and be formed release of carbonate dioxide out, can not affect the quality of sodium cyanide solution.
By as above three steps, finished the environment-friendly clean process production method of a kind of high-purity sodium cyanide provided by the invention.Its step process is that the employing ammonia oxidation is synthesized the prussic acid synthetic gas directly and aqueous sodium hydroxide solution reacts the environment-friendly clean process production method that obtains high-purity sodium cyanide: the synthetic prussic acid synthetic gas of ammonia oxidation is just directly obtaining high-purity sodium cyanide solution by the aqueous sodium hydroxide solution absorption reaction without removing the ammonia process, and free ammonia remains in the tail gas; High-purity sodium cyanide solution obtains high purity liquid sodium cyanide product by the cooling allotment, and high-purity sodium cyanide solution obtains high purity solid sodium cyanide product by concentrated, crystallization, centrifugation, and mother liquid recycle is in absorbing by liquid caustic soda liquid; Adopt phosphoric acid or primary ammonium phosphate as carrier, free ammonia in the absorption tower in the absorption tail gas, 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 again primary ammonium phosphate, iterative cycles has realized that the ammonia of tail gas reclaims; Tail gas after ammonia reclaims is water or aqueous sodium hydroxide solution purification absorption again, remaining prussic acid is purified and gathers in the crops simultaneously a small amount of hydrocyanic acid aqueous solution or crude product sodium cyanide solution in the tail gas, tail gas after the purification burns with the tail gas boiler, and hydrocyanic acid aqueous solution or crude product sodium cyanide solution cover are used in the absorbing by liquid caustic soda liquid.
The environment-friendly clean process production method of a kind of high-purity sodium cyanide provided by the invention, be applicable to relate to the process that the synthetic prussic acid synthetic gas of all ammonia oxidations is produced sodium cyanide, such as the process of producing sodium cyanide by synthetic gas such as the standby prussic acid of methane prepared by ammoxidation, methanol ammonoxidation hydrogen manufacturing cyanic acid, the standby prussic acid of light oil cracking prepared by ammoxidation; Present method both provided the production method of high-purity sodium cyanide product, and the recycle and reuse that can realize the synthetic gas free ammonia, the environment-protecting clean producing and manufacturing technique of realizing the Mode of Circular of comprehensive utilization of resources are provided again.
Technical matters provided by the invention has following feature:
1, the present invention adopts the synthetic prussic acid synthetic gas of ammonia oxidation without just directly obtaining high-purity sodium cyanide solution by the aqueous sodium hydroxide solution absorption reaction except the ammonia process, obtains very easily our needed high purity product, has saved loaded down with trivial details purification process.
2, the recovery of ammonia adopts phosphoric acid or primary ammonium phosphate as carrier in the tail gas, has realized the recycling of ammonia in the tail gas, has realized simultaneously the utilization of absorption carrier iterative cycles, has realized the Mode of Circular of resource comprehensive recycle.
3, the recovery of ammonia adopts phosphoric acid or primary ammonium phosphate as carrier in the tail gas, and envrionment conditions is relatively friendly, and material has obtained good improvement to equipment corrosion, work-ing life that can extension device when saving facility investment.
4, present technique technique can be produced by very effective realization environment-protecting clean, has well solved the difficult problem of environmental protection in the synthetic Sodium Cyanide Production technique of existing ammonia oxidation, has broken through the environmental technology barrier of the synthetic Sodium Cyanide Production technique industrialized development of ammonia oxidation.
5, adopt the high-purity sodium cyanide of present technique explained hereafter, to raw-material require relatively low; Demonstrate fully the practicality of Technology provided by the invention, and can reduce the raw material quality cost.
Description of drawings
Figure of description is that the synthetic prussic acid mixed gas of the ammonia oxidation of carrying out as the ammonia source take ammonia that the present invention relates to directly reacts the environment-friendly clean process production method schematic flow sheet that obtains high-purity sodium cyanide with aqueous sodium hydroxide solution.
Embodiment
Illustrate in greater detail the present invention below by embodiment, but scope of the present invention is not subjected to the restriction of embodiment.
Embodiment: the synthetic prussic acid synthetic gas of iS-One method Sweet natural gas ammonia oxidation is just directly obtaining high-purity sodium cyanide solution by the aqueous sodium hydroxide solution absorption reaction without removing the ammonia process, and free ammonia remains in the tail gas;
Component such as the following table of certain synthetic gas before absorption reaction:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 8.092 | 6 | N 2 | 54.328 |
| 2 | NH 3 | 1.508 | 7 | CO 2 | 0.503 |
| 3 | H 2O | 25.513 | 8 | CO | 4.705 |
| 4 | CH 4 | 0.462 | 9 | H 2 | 4.765 |
| 5 | O 2 | 0.020 | 10 | Other | 0.104 |
The sodium cyanide solution quality table:
| Outward appearance | Sodium cyanide (%) | CO 3 2- | NH 3 + | Other |
| Water white transparency | 30.78 | 0.021 | 0.012 | Water, trace impurity |
Obtain high purity liquid sodium cyanide product by the cooling allotment; High-purity sodium cyanide solution obtains high purity solid sodium cyanide product by concentrated, crystallization, centrifugation;
Solid sodium cyanide quality product table:
| Outward appearance | Sodium cyanide (%) | CO 3 2- | NH 3 + | Other |
| Water white transparency | 99.58 | 0.068 | 0.008 | Water, trace impurity |
Tail gas component such as following table:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 0.2246 | 6 | N 2 | 60.8716 |
| 2 | NH 3 | 1.6818 | 7 | CO 2 | 0.5631 |
| 3 | H 2O | 25.6069 | 8 | CO | 5.2714 |
| 4 | CH 4 | 0.5181 | 9 | H 2 | 5.3388 |
| 5 | O 2 | 0.0225 | 10 | Other | 0.0012 |
Tail gas carries out the recovery of ammonia, adopts phosphoric acid or primary ammonium phosphate as absorbing carrier; Tail gas composition such as following table behind the recovery ammonia:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 0.2655 | 6 | N 2 | 74.7016 |
| 2 | NH 3 | 0.0679 | 7 | CO 2 | 0.6910 |
| 3 | H 2O | 10.4429 | 8 | CO | 6.4691 |
| 4 | CH 4 | 0.6358 | 9 | H 2 | 6.5518 |
| 5 | O 2 | 0.0276 | 10 | Other | 0.1468 |
The ammonium dihydrogen phosphate absorbing ammonia is converted into ammonium hydrogen phosphate solution, by the recovery of parsing with ammonia; The ammonium dihydrogen phosphate that parses is cycled to used in the absorption of ammonia, reclaims ammonia and is used for the recycling that the ammonia oxidation raw material has been realized ammonia.
Tail gas after ammonia reclaims is again by the de-salted water absorption cleaning, and remaining prussic acid is purified and gathers in the crops simultaneously a small amount of hydrocyanic acid aqueous solution in the tail gas;
The hydrocyanic acid aqueous solution quality table:
| Prussic acid (%) | CO 3 2-(％) | NH 3 +(％) | Other |
| 2.78 | 0.78 | 0.58 | Water, trace impurity |
The hydrocyanic acid aqueous solution cover is used in the sodium hydroxide absorption liquid;
The component of cleaning of off-gas such as following table:
| Sequence number | The component title | Component ratio % | Sequence number | The component title | Component ratio % |
| 1 | HCN | 0.0058 | 6 | N 2 | 80.1532 |
| 2 | NH 3 | 0.0012 | 7 | CO 2 | 0.7414 |
| 3 | H 2O | 4.2440 | 8 | CO | 6.9477 |
| 4 | CH 4 | 0.6828 | 9 | H 2 | 7.0366 |
| 5 | O 2 | 0.0296 | 10 | Other | 0.1577 |
Tail gas after the purification burns with the tail gas boiler.
Claims (5)
1. the environment-friendly clean process production method of a high-purity sodium cyanide, it is characterized in that adopting the synthetic prussic acid reactant gases of ammonia oxidation directly and the aqueous sodium hydroxide solution absorption reaction obtain the environment-friendly clean process production method of high-purity sodium cyanide, the prussic acid reactant gases that contain free ammonia synthetic by ammonia oxidation obtaining high-purity sodium cyanide solution without removing the ammonia process with regard to direct and aqueous sodium hydroxide solution absorption reaction, obtains high purity liquid sodium cyanide product by cooling off allotment; High-purity sodium cyanide solution obtains high purity solid sodium cyanide product by concentrated, crystallization, centrifugation, and mother liquid recycle is in sodium hydroxide absorption reaction liquid; Free ammonia remains in the tail gas, tail gas is carried out the recycling of ammonia again; Tail gas behind the recovery ammonia purifies rear burning again.
The described prussic acid reactant gases of claim 1 directly and the aqueous sodium hydroxide solution absorption reaction, its absorption reaction feature is: the absorption reaction system pressure is 0.0-0.08MPa (gauge pressure), temperature is 60 ℃-200 ℃.
3. applying mechanically of the described high purity solid crystallization of nacn of claim 1 mother liquor is characterized in that: crystalline mother solution directly or after purifying cover use in the sodium hydroxide absorption reaction liquid.
4. the recovery of ammonia in the described tail gas of claim 1, it is characterized in that: adopt phosphoric acid or primary ammonium phosphate as carrier, free ammonia in the absorption tower in the absorption tail gas, phosphoric acid or primary ammonium phosphate are converted into Secondary ammonium phosphate, Secondary ammonium phosphate parses free ammonia in Analytic Tower, be converted into again primary ammonium phosphate, iterative cycles has realized that the ammonia of tail gas reclaims.
5. the tail gas clean-up behind the described recovery ammonia of claim 1, it is characterized in that: adopt water or aqueous sodium hydroxide solution to purify and absorb, remaining prussic acid is purified and gathers in the crops simultaneously a small amount of hydrocyanic acid aqueous solution or the sodium cyanide crude product aqueous solution in the tail gas, hydrocyanic acid aqueous solution or the sodium cyanide crude product aqueous solution directly cover are used in the absorbing by liquid caustic soda liquid, and the tail gas after the purifying treatment send the tail gas burning boiler to burn again.
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| CN107434253A (en) * | 2017-08-06 | 2017-12-05 | 河北诚信有限责任公司 | A kind of continuous production technology and its production system of high-quality cyanide solution |
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| US11905179B2 (en) | 2015-06-18 | 2024-02-20 | Cyplus Gmbh | Efficient method for decontaminating waste gases and waste water containing cyanide in a method for producing alkali metal cyanides |
| CN107750235B (en) * | 2015-06-18 | 2021-03-19 | Epc工程与技术有限公司 | Effective method for detoxifying cyanide-containing waste gases and waste waters in a process for producing alkali metal cyanides |
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Application publication date: 20130501 |