CN111686635B - Integrated granulation drying method for coking desulfurization sulfur foam and desulfurization waste liquid - Google Patents
Integrated granulation drying method for coking desulfurization sulfur foam and desulfurization waste liquid Download PDFInfo
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Abstract
The invention belongs to the technical field of desulfurization waste liquid and sulfur foam treatment, and discloses an integrated granulation and drying method for coking desulfurization sulfur foam and desulfurization waste liquid, which comprises the steps of adding food colloid into a mixed solution of sulfur foam and desulfurization waste liquid with a certain solid content to form a stable suspension; dripping the obtained suspension into cold water or electrolyte solution with certain concentration in a dripping or spraying manner to form gel balls, and solidifying in the solution for a certain time; drying the solidified gel spheres at a certain temperature to obtain saliferous coarse sulfur spherical particles which are free from agglomeration and moisture absorption and uniform in particles. The invention adopts a dropping ball method or a spraying method to prepare gel balls, and then the gel balls are dried to obtain coarse sulfur spherical particles containing salt. The technology has the advantages of simple process flow, low operation requirement, low equipment investment cost, simple maintenance and lower operation cost. The salt-containing coarse sulfur spherical particles prepared by the process can be dried at a higher temperature, and the production efficiency is favorably improved.
Description
Technical Field
The invention belongs to the technical field of desulfurization waste liquid and sulfur foam treatment, and particularly relates to an integrated granulation and drying method for coking desulfurization sulfur foam and desulfurization waste liquid.
Background
At present, desulfurization waste liquid and sulfur foam are byproducts in a desulfurization process of a coking enterprise by adopting a wet oxidation method (HPF method). The pollutants are not treated and directly discharged into the environment, so that the pollutants can release irritating odor, cause serious pollution to the surrounding environment, influence the respiration of animals and the growth of plants and cause serious resource waste.
Because the desulfurization waste liquid contains a large amount of inorganic salt, the components are complex and the desulfurization waste liquid has strong corrosivity; the sulfur foam also contains a large amount of salt impurities, the purity is not high, and the comprehensive utilization efficiency is low, so the desulfurization waste liquid and the sulfur foam are the most difficult industrial wastes to treat at present, and the long-term development of coking enterprises is severely restricted. At present, the comprehensive utilization ways of coking desulfurization and sulfur foam mainly comprise the following types.
(1) Burning the sulfur foam directly into SO2And (5) further processing the gas to prepare industrial sulfuric acid. The core of the technology is that the sulfur foam and the desulfurization waste liquid thereof are burnt and decomposed at high temperature, and then SO is recovered2A gas. The method has the advantages of short process flow, continuous production process, simultaneous treatment of the sulfur foam and the desulfurization waste liquid, and realization of waste treatment and sulfur recycling. This technique also has significant drawbacks that are difficult to overcome. On one hand, the heat energy consumption is extremely high, and the operation cost is very high; another one isOn the other hand, a large amount of moisture is vaporized in the incineration process, and the water vapor needs to be removed in the purification process, so that energy is repeatedly consumed, and therefore, the method is unreasonable in economy; in addition, a large amount of water vapor is generated in the process, together with a small amount of SO3And SO2Dilute sulfuric acid and sulfurous acid are generated by contact, and equipment and process pipelines are seriously corroded, so that the investment cost of the device is very high; finally, the technology relates to foreign technical patents, the patent use cost is high, key equipment and catalysts need to be imported, the technology is restricted by people, foreign technical maintenance needs to be relied on for a long time, and troubleshooting and overhauling are troublesome.
(2) Firstly, the coke oven gas is desulfurized by adopting a vacuum potassium carbonate method, and then the resolved H is separated by utilizing a Topsoe technology2S gas is burnt to generate SO2Finally, sulfuric acid is prepared by a condensation technology. This technique need construct complete set's desulfurization system sour device, and not only the investment is big, has still appeared a lot of drawbacks moreover in the actual motion process, if: in the vacuum potassium carbonate method desulfurization section, the desulfurization efficiency is not high, the desulfurization is not thorough, the discharge standard requirements of national environmental protection regulation cannot be met, the hidden danger of producing a highly toxic substance potassium cyanide exists, the serious harm is brought to the health of workers and the water and soil pollution, and the sewage treatment difficulty is high and becomes a new environmental protection problem; h desorbed from incineration station2SO generated from S gas2Low gas content and conversion to SO3When acid is made, the self-heating balance is difficult to maintain, and the intangible supplementary heat also increases the production cost and the equipment investment.
(3) Claus sulfur recovery process. The process uses absorption method to desulfurize and then desorb H2S gas is combusted in a Claus furnace to produce a portion H2Oxidation of S to SO2，SO2Then with the remaining unreacted H2S reacts on a catalyst to generate sulfur. The sulfur recovered by the process has high purity, can reach the quality index of commercial-grade industrial sulfur, and can be directly used for producing industrial sulfuric acid by using the traditional acid preparation technology. However, the method has complex process flow, high operation requirement, high equipment investment cost and high operation cost.
(4) The technology for preparing acid by simultaneously solidifying desulfurized waste liquid and sulfur foam and directly burning solid crude sulfur is a method for preparing acid by utilizing sulfur-containing waste materials. The key technologies of the process mainly comprise a sulfur foam curing, drying and recycling technology, a solid crude sulfur direct burning technology, a waste heat recycling, an acid cleaning and purifying technology, a '3 + 2' two-conversion and two-absorption technology and the like.
The invention patent (CN201410820970.6) discloses a method for drying coking desulfurization sulfur foam and desulfurization waste liquid. The method is characterized in that a spray drying tower is used for simultaneously carrying out spray drying on the desulfurization waste liquid and the sulfur foam to obtain salt-containing crude sulfur powder. However, this method has disadvantages in that, on the one hand, the temperature during spray drying is high, so that elemental sulfur in the sulfur foam is easily melted, and wall sticking occurs in the drying tower. Although a blowing device (or an air hammer) can be arranged in the tower body, the fine powder adsorbed on the inner wall of the tower body is blown off by adopting compressed air, so that the wall sticking problem can be relieved to a certain extent. However, the blowing device can not remove accumulated materials in time, the time is long, the accumulated materials are in a high-temperature area for a long time, and the accumulated materials can turn yellow, coke and deteriorate, fall into products and cause pollution to the materials, and even scrap the products when the accumulated materials are serious, so that great waste is caused; on the other hand, since elemental chalcogen is a combustible substance, during the spray drying process, sulfur powder is liable to form static electricity due to mutual friction, thereby causing a risk of spontaneous combustion and even explosion in the spray drying tower.
Through the above analysis, the problems and disadvantages of the prior art are: because the components in the desulfurization waste liquid and the sulfur foam are complex, and many components have strong toxicity and corrosiveness. On one hand, the existing treatment method has complex process, large energy consumption, serious equipment corrosion phenomenon and high operation cost; on the other hand, the product obtained after treatment contains more impurities, has low added value and small market space. More importantly, the treatment process has higher flammable and explosive risks, the sulfur circulation is increased, and secondary pollution is caused. Therefore, the coking industry does not have an economical, safe, feasible and universal technology for integrated harmless treatment of the desulfurization waste liquid and the sulfur foam at present, which becomes a significant bottleneck for restricting the benign development and the technical upgrading of the current coking industry.
The invention aims to solve the technical problem of providing an integrated drying method of coking desulfurization sulfur foam and desulfurization waste liquid, which has universality, simplicity, high efficiency, low cost and no flammable and explosive risks. The method can dry the desulfurization waste liquid and the sulfur foam together to obtain the coarse sulfur spherical particles with uniform particles and salt, is easy to store and transport, provides a brand new solution for the treatment and utilization of the desulfurization waste liquid and the sulfur foam, and is beneficial to the sustainable green development of the coking industry.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an integrated granulation and drying method for coking desulfurization sulfur foam and desulfurization waste liquid.
The invention is realized in this way, an integrated granulating and drying method for coking desulfurization sulfur foam and desulfurization waste liquid, comprising the following steps:
adding the food colloid into a mixed solution of sulfur foam with a certain solid content and desulfurization waste liquid to form a stable suspension;
dripping the obtained suspension into cold water or electrolyte solution with certain concentration in a dripping or spraying manner to form gel balls, and solidifying in the solution for a certain time;
and drying the solidified gel spheres at a certain temperature to obtain the coarse saliferous sulfur spherical particles which are not agglomerated, do not absorb moisture and are uniform in particles.
Further, the food gel comprises: one or more of gelatin, agar, xanthan gum, carrageenan, alginate, locust bean gum, guar gum, konjac gum and pectin.
Adding into the mixture of sulfur foam with solid content less than 55 wt% and desulfurized waste liquid to form stable suspension.
Dripping the obtained suspension into cold water at 5-35 ℃ or electrolyte solution with the concentration of 0.2-15 wt% in a dripping or spraying mode.
The electrolyte solution comprises a solution containing K+、Na+、Ca2+、Mg2+、Fe2+、Fe3+One or more ions of (a).
Further, the gel beads are cured in the solution for 10min to 60 min.
Drying the solidified gel balls at 100-250 ℃ to obtain the crude salt-containing sulfur spherical particles which are not agglomerated, do not absorb moisture and have uniform particles.
The invention also aims to provide the integrated granulation and drying equipment for the coking desulfurization sulfur foam and the desulfurization waste liquid, which is used for implementing the integrated granulation and drying method for the coking desulfurization sulfur foam and the desulfurization waste liquid.
From the technical principle, the invention and the utility model thereof are completely different from the existing treatment schemes of domestic and foreign desulfurized sulfur foam and desulfurized waste liquid, can effectively avoid the technical barriers of foreign patents, and overcome the problems that people are restricted in the technology, the long-term dependence on the foreign technical maintenance is required, the trouble is eliminated and the maintenance is troublesome, etc. The integral scheme is feasible, the method is universal, simple, efficient, low in cost and free of inflammable and explosive risks, and the coking desulfurization sulfur foam and desulfurization waste liquid integrated drying method is beneficial to sustainable green development of the coking industry.
By combining all the technical schemes, the positive effects of the dry tail gas emission of the invention are shown in the following table 1:
TABLE 1
| Serial number | Contaminant item | GB16171-2012 | Control index |
| 1 | Sulfur dioxide | 30mg/m3 | <30mg/m3 |
| 3 | Nitrogen oxides | 150mg/m3 | <100mg/m3 |
| 4 | Particulate matter | 15mg/m3 | <10mg/m3 |
The invention adopts a continuous production process, thereby having higher production efficiency and being beneficial to the industrial scale treatment of the desulfurization waste liquid and the sulfur foam.
The desulfurization waste liquid and the sulfur foam are directly mixed, and are dripped into gel balls by adopting a dripping ball method or a spraying method, and then the gel balls are dried to obtain coarse sulfur spherical particles containing salt. The technology has the advantages of simple process flow, low operation requirement, low equipment investment cost, simple maintenance and lower operation cost. On the other hand, the prepared salt-containing coarse sulfur particles are uniform in particle size, and because the elemental sulfur is wrapped by the gel film, the phenomena of melting, bonding and pulverization cannot occur in the subsequent drying process due to overhigh temperature, and the problem of friction and spontaneous combustion of the elemental sulfur is effectively avoided.
The method can dry the desulfurization waste liquid and the sulfur foam together to obtain the coarse sulfur spherical particles with uniform particles and salt, realize closed-loop treatment and realize zero emission.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
FIG. 1 shows an embodiment of the present invention providing an integrated method and system for granulating and drying coked desulfurized sulfur foam and desulfurized waste liquid
FIG. 2 is a graph showing the effect of saliferous coarse sulfur spherical particles provided in example 1 of the present invention.
FIG. 3 is a graph showing the effect of the salt-containing coarse spherical sulfur granules provided in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides an integrated granulation and drying method and system for coking desulfurization sulfur foam and desulfurization waste liquid, and the invention is described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the integrated granulation and drying method for the coked desulfurized sulfur foam and the desulfurized waste liquid provided by the invention comprises the following steps:
firstly, adding food colloid (one or more of gelatin, agar, xanthan gum, carrageenan, alginate, locust bean gum, guar gum, konjac gum and pectin) to a certain solid content<55 wt%) of sulfur foam and desulfurized waste liquid to form a stable suspension. Then dripping the obtained suspension into cold water (5-35 ℃) or electrolyte solution (containing K) with certain concentration (0.2-15 wt%) by a dripping or spraying mode+、Na+、Ca2+、Mg2+、Fe2+、Fe3+One or more ions of (a), gel spheres are formed and cured in solution for a certain time (10min-60 min). And finally, drying the solidified gel spheres at a certain temperature (100-250 ℃) to obtain the salt-containing coarse sulfur spherical particles which are not agglomerated and absorb moisture and have uniform particles.
The present invention provides an integrated granulation and drying method and system for coking desulfurization sulfur foam and desulfurization waste liquid, and those skilled in the art can also use other steps to implement, and the invention of fig. 1 is provided only as an embodiment.
The invention is further described with reference to specific examples.
Example 1:
firstly, 0.5 wt% of carrageenan powder is dissolved in a mixed solution of sulfur foam with the solid content of 40% and desulfurized waste liquid to form a stable suspension. Then, the resulting suspension was dropped dropwise into a 0.6 wt% KCl curing solution with a dropper to form gel beads, and cured in the curing solution for 60 min. Finally, drying the solidified gel spheres at 150 ℃ to obtain the salt-containing coarse sulfur spherical particles with the particle size of about 1.6-2mm, which are not agglomerated and absorb moisture and have uniform particles (figure 2).
Example 2:
firstly, 1.5 wt% of agar powder is dissolved in a mixed solution of sulfur foam with the solid content of 40% and desulfurization waste liquid to form a stable suspension. Then, the resulting suspension was atomized and dropped into 1 wt% FeCl with a centrifugal atomizer3Forming gel balls in the solution, and curing for 10min in the curing liquid. Finally, drying the solidified gel spheres at 150 ℃ to obtain the salt-containing coarse sulfur spherical particles with the particle size of about 0.1-1mm, which are not agglomerated and absorb moisture and have uniform particles (figure 3).
Example 3:
firstly, 2 wt% of xanthan gum and konjac gum mixed powder (mass ratio of xanthan gum to konjac gum is 6:4) is dissolved in a mixed solution of sulfur foam with a solid content of 30% and desulfurization waste liquid to form a stable suspension. Then, the resulting suspension was dropped dropwise into a 2 wt% KCl solution using a centrifugal atomizer to form gel beads, and cured in the curing solution for 30 min. And finally, drying the solidified gel spheres at 220 ℃ to obtain the salt-containing coarse sulfur spherical particles with the particle size of about 0.1-0.4mm, which are not agglomerated and absorb moisture and have uniform particles.
Example 4:
firstly, 4 wt% of sodium alginate powder is dissolved in the solution with the solid content of 30%And forming stable suspension in the mixed solution of the sulfur foam and the desulfurization waste liquid. Then, the resulting suspension was dropwise added with 15 wt% MgCl using a centrifugal atomizer2In the solution, gel balls are formed, and the gel balls are solidified in the solidifying liquid for 10 min. And finally, drying the solidified gel spheres at 250 ℃ to obtain the saliferous coarse sulfur spherical particles with the particle size of about 0.1-0.3mm, which do not cake and absorb moisture and are uniform in particles.
The drying methods of examples 5-6 were the same as those of examples 1-4, and the specific parameters are shown in Table 2.
TABLE 2
In the description of the present invention, "a plurality" means two or more unless otherwise specified; the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The integrated granulation and drying method for the coking desulfurization sulfur foam and the desulfurization waste liquid is characterized by comprising the following steps of:
adding food colloid into a mixed solution of sulfur foam with a certain solid content and desulfurization waste liquid to form a stable turbid liquid;
dripping the obtained suspension into cold water or electrolyte solution with certain concentration in a dripping or spraying manner to form gel balls, and solidifying in the solution for a certain time;
drying the solidified gel spheres at a certain temperature to obtain salt-containing coarse sulfur spherical particles which are not agglomerated and absorb moisture and have uniform particles;
the solid content of the mixed liquid of the desulfurized sulfur foam and the desulfurized waste liquid is less than 55 wt%.
2. The integrated process for granulation and drying of coked desulfurization sulfur foam and desulfurization waste liquid according to claim 1, wherein the food colloid comprises: one or more of gelatin, agar, xanthan gum, carrageenan, alginate, locust bean gum, guar gum, konjac gum, and pectin.
3. The integrated granulation and drying method of coked desulfurization sulfur foam and desulfurization waste liquid as claimed in claim 1, wherein the obtained suspension is dripped into cold water at 5-35 ℃ or an electrolyte solution with a concentration of 0.2-15 wt% in a dripping or spraying manner.
4. The integrated process of granulation and drying of coked desulfurization sulfur foam and desulfurization waste liquid of claim 1, wherein the electrolyte solution comprises K-containing+、Na+、Ca2+、Mg2+、Fe2+、Fe3+One or more ions of (a).
5. The integrated granulation drying method of coking desulfurization sulfur foam and desulfurization waste liquid as described in claim 1, wherein the gel beads are solidified in the solution for 10min to 60 min.
6. The integrated granulation drying method of coking desulfurization sulfur foam and desulfurization waste liquid as described in claim 1, wherein the solidified gel spheres are dried at 100 ℃ to 250 ℃ to obtain salt-containing coarse sulfur spherical particles which are non-caking, non-hygroscopic and uniform in particle size.
7. An integrated granulation drying apparatus for coking desulfurization sulfur foam and desulfurization waste liquid, which implements the integrated granulation drying method for coking desulfurization sulfur foam and desulfurization waste liquid according to claims 1 to 6.
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