A method for synergistic concentration of sulfur foam by gradient centrifugation and microwave drying
By employing a sulfur foam gradient centrifugation-microwave drying synergistic concentration method, utilizing foam modifiers and microwave drying technology, the problems of high viscosity and water content of sulfur foam were solved, achieving efficient concentration and dehydration effects.
Patent Information
- Application Number
- CN202511029001.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-25
- Publication Date
- 2026-01-30
- Estimated Expiration
- 2045-07-25
AI Technical Summary
Sulfur foam has a high viscosity and high water content, which affects its dehydration effect and makes subsequent processing difficult.
A sulfur foam gradient centrifugation-microwave drying co-concentration method was adopted, which includes adding a foam modifier, solid-liquid separation and microwave drying. 1-Ethyl-3-methylimidazolium betaine salt was used for modification to reduce viscosity and destroy colloidal structure. Dehydration was carried out by combining centrifugation and microwave technology.
It effectively reduces the viscosity and water content of sulfur foam, promotes water separation, improves the concentration and dehydration effect of sulfur foam, and simplifies subsequent processing steps.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] This invention belongs to the field of sulfur foam separation technology, specifically relating to a method for the synergistic concentration of sulfur foam by gradient centrifugation and microwave drying. Background Technology
[0002] In the wet desulfurization and regeneration process of coke oven gas, a large amount of sulfur foam is generated through flotation. The concentration of this sulfur foam varies greatly, and its high liquid content is detrimental to subsequent processing. Furthermore, the sulfur foam generated during the wet desulfurization process can be used in sulfuric acid production, effectively recovering and utilizing sulfur resources. This also solves the problem of saline wastewater discharge during desulfurization, reducing environmental pollution and representing a promising development direction in the field of coking desulfurization. Currently, the pretreatment of sulfur foam in this process—namely, the effective concentration and separation of sulfur foam—is a prerequisite for the subsequent combustion of sulfuric acid feedstock to produce sulfuric acid feedstock gas.
[0003] Sulfur foam concentration refers to increasing the sulfur content in sulfur foam through specific methods during the sulfur recovery process, enabling more efficient recovery and treatment. Currently, sulfur foam is generally treated using plate and frame filtration and centrifugal separation processes, or directly fed into an incinerator for sulfuric acid production. The purpose of plate and frame filtration is to filter out the sulfur particles from the sulfur foam and press it into sulfur paste for sulfur production. The clarified liquid after filtration is used for desulfurization and is generally returned to the reaction tank of the desulfurization system. The desulfurization liquid in the desulfurization tower is continuously circulated in the desulfurization tower through countercurrent contact with the coal gas for desulfurization via a circulating pump. Centrifugal separation uses a centrifuge, which sends the separated sulfur particles into a filter press or sulfur melting kettle. The clarified liquid after centrifugation is returned to the desulfurization tower.
[0004] It is evident that sulfur foam concentration is a crucial step in the sulfur recovery process. By employing physical, chemical, and thermal methods, the sulfur content in the sulfur foam can be increased, recovery efficiency optimized, impurity content reduced, and the process ensured to be both efficient and safe. Summary of the Invention
[0005] To address the aforementioned technical problems, this invention provides a method for the synergistic concentration of sulfur foam through gradient centrifugation and microwave drying. This method effectively solves the problem that the high viscosity and high water content of sulfur foam affect the drying effect of the dehydrating agent.
[0006] This invention provides a method for the synergistic concentration of sulfur foam through gradient centrifugation and microwave drying, comprising the following steps:
[0007] (1) Take the sulfur foam to be treated, add foam modifier, stir and mix well to obtain sulfur foam liquid;
[0008] (2) The sulfur foam liquid is filtered to perform the first solid-liquid separation and remove some water;
[0009] (3) Continue to centrifuge the sulfur foam liquid for a second solid-liquid separation to further remove moisture;
[0010] (4) Collecting the solid part for microwave drying treatment.
[0011] In some preferred embodiments, in the step (2), the first solid-liquid separation step comprises gravity sedimentation or plate-frame pressure filtration.
[0012] In some preferred embodiments, in the step (3), the centrifugal speed of the second solid-liquid separation step is 5000-8000 rpm.
[0013] In some preferred embodiments, in the step (4), the microwave frequency of the microwave drying step is 900-1200 MHz.
[0014] In some preferred embodiments, in the step (1), the stirring speed is 200-400 rpm.
[0015] In some preferred embodiments, the foam modifier comprises an ionic liquid demulsifier.
[0016] In some preferred embodiments, the foam modifier comprises a betaine salt.
[0017] In some preferred embodiments, the foam modifier comprises 1-ethyl-3-methylimidazolium betaine [EMIM][Betaine].
[0018] In some preferred embodiments, the addition amount of the foam modifier based on the sulfur foam slurry is 5-10 wt%.
[0019] In some preferred embodiments, the foam modifier further comprises an esterase microcapsule.
[0020] The embodiments of the present application have the following technical effects:
[0021] The sulfur foam gradient centrifugation-microwave drying synergistic concentration method of the present application utilizes the selected foam modifier to modify the sulfur foam, which not only effectively reduces the bubbles of the sulfur foam and the viscosity performance of the slurry, but also effectively destroys the colloid system formed by the bubbles and sulfur particles in the sulfur foam, promotes the separation of water in the sulfur foam, further strengthens the dehydration effect, so that the treated sulfur foam only needs conventional physical dehydration treatment to realize the dehydration and drying treatment of high water content sulfur foam.
[0022] The sulfur foam gradient centrifugal-microwave drying synergistic concentration method of the present application adopts 1-ethyl-3-methyl imidazole betaine salt [EMIM][betaine] to modify the sulfur foam, and compared with general betaine salt or 1-ethyl-3-methyl imidazole salt, the modification effect is more optimal, especially suitable for the modification treatment of sulfur foam, which can effectively improve the foam and viscosity of the sulfur foam itself, is more conducive to the filtration step, and can destroy the colloidal structure between sulfur particles, reduce the influence of polymerization water, effectively improve the concentration and dehydration effect, and solve the current problem of difficult dehydration of sulfur foam. DETAILED DESCRIPTION
[0023] To make the objectives, technical solutions, and advantages of the present application clearer, the technical solutions of the present application will be clearly and completely described below. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work belong to the present application.
[0024] In the following embodiments of the present application, a sulfur foam gradient centrifugal-microwave drying synergistic concentration method is provided, which specifically comprises the following steps:
[0025] (1) The sulfur foam to be treated is added with a foam modifier, stirred and mixed to obtain a sulfur foam slurry;
[0026] (2) The sulfur foam slurry is subjected to first solid-liquid separation by filtration to remove part of the water;
[0027] (3) The sulfur foam slurry is further subjected to second solid-liquid separation by centrifugation to further remove water;
[0028] (4) The solid part is collected for microwave drying treatment, and the sulfur foam is obtained.
[0029] The sulfur foam gradient centrifugal-microwave drying synergistic concentration method of the present application utilizes the selected foam modifier to modify the sulfur foam, which not only can effectively reduce the bubbles of the sulfur foam and the viscosity performance of the slurry, but also can effectively destroy the colloidal system formed by the bubbles and sulfur particles in the sulfur foam, promote the separation of water in the sulfur foam, and further strengthen the dehydration effect, so that the treated sulfur foam only needs conventional physical dehydration treatment to realize the dehydration and drying treatment of the sulfur foam with high water content.
[0030] In some feasible embodiments, in the step (2), the first solid-liquid separation step adopts a general physical filtration method, such as gravity sedimentation or plate and frame filter pressing.
[0031] In some possible implementation forms, in the second solid-liquid separation step, a general centrifugal filtration method is used, for example, the centrifugal speed is controlled to be 5000-8000 rpm.
[0032] In some possible implementation forms, in the microwave drying step, the microwave frequency is 900-1200 MHz.
[0033] In some possible implementation forms, in the stirring step, the stirring speed is 200-400 rpm, so that the foam modifier can be in better contact with the sulfur foam, and thus the modification treatment can be sufficient.
[0034] In some possible implementation forms, the foam modifier comprises an ionic liquid demulsifier.
[0035] In some possible implementation forms, the foam modifier comprises a betaine salt.
[0036] In some possible implementation forms, the foam modifier comprises 1-ethyl-3-methyl imidazole betaine salt [EMIM][Betaine].
[0037] In some possible implementation forms, the foam modifier is added in an amount of 5-10 wt% based on the sulfur foam liquid, when the amount is low, the modification effect is not ideal, and when the amount is higher, the enhanced improvement effect is not obvious.
[0038] In some possible implementation forms, the foam modifier further comprises an esterase microcapsule, the esterase microcapsule can be obtained by using a conventional microencapsulation method in the art, and the selection of a wall material and the like has little effect on the modification of the esterase, and a person skilled in the art can reasonably select according to the concentration and other properties of the sulfur foam.
[0039] In the following embodiments of the present application, 1-ethyl-3-methyl imidazole betaine salt [EMIM][Betaine] is selected as an example of the foam modifier for foam modification treatment, the 1-ethyl-3-methyl imidazole betaine salt is an ionic liquid known in the art, and a commercially available product or a conventional method can be used for synthesis.
[0040] In the following embodiments of the present application, the sulfur foam generated in a coke oven gas wet desulfurization process is taken as an example, which contains sulfur particles, salt and other components, and the water content is 65% and the viscosity is 198.43 cp after detection.
[0041] Example 1
[0042] Take the sulfur foam, add 8wt% of 1-ethyl-3-methylimidazolium betaine salt [EMIM][Betaine], mix well, and stir at a speed of 300 rpm for 10 min to obtain a foam mixture liquid.
[0043] Place the foam mixture liquid in a plate and frame filter press for filtration treatment, and collect the first filtrate.
[0044] Centrifuge the filter cake at a speed of 6000 rpm for 10 min, and collect the second filtrate.
[0045] Place the second filtrate in a microwave dryer, control 1000 MHz, and microwave dry for 1 h to obtain the dry product.
[0046] Example 2
[0047] Take the sulfur foam, add 5wt% of 1-ethyl-3-methylimidazolium betaine salt [EMIM][Betaine], mix well, and stir at a speed of 400 rpm for 10 min to obtain a foam mixture liquid.
[0048] Place the foam mixture liquid in a plate and frame filter press for filtration treatment, and collect the first filtrate.
[0049] Centrifuge the filter cake at a speed of 8000 rpm for 10 min, and collect the second filtrate.
[0050] Place the second filtrate in a microwave dryer, control 1200 MHz, and microwave dry for 1 h to obtain.
[0051] Example 3
[0052] Take the sulfur foam, add 10wt% of 1-ethyl-3-methylimidazolium betaine salt [EMIM][Betaine], mix well, and stir at a speed of 200 rpm for 10 min to obtain a foam mixture liquid.
[0053] Place the foam mixture liquid in a plate and frame filter press for filtration treatment, and collect the first filtrate.
[0054] Centrifuge the filter cake at a speed of 5000 rpm for 10 min, and collect the second filtrate.
[0055] Place the second filtrate in a microwave dryer, control 900 MHz, and microwave dry for 1 h to obtain.
[0056] Example 4
[0057] Take the sulfur foam, add 3wt% of 1-ethyl-3-methylimidazolium betaine salt [EMIM][Betaine], mix well, and fully stir at a speed of 300 rpm for 10 min to obtain a foam mixture liquid.
[0058] Place the foam mixture liquid in a plate and frame filter press for filtration treatment, and collect a first filtrate.
[0059] Centrifuge the filter cake at a speed of 6000 rpm for 10 min, and collect a second filtrate.
[0060] Place the second filtrate in a microwave dryer, and control the microwave drying at 1000 MHz for 1 h to obtain the product.
[0061] Example 5
[0062] Take the sulfur foam, add 12wt% of 1-ethyl-3-methylimidazolium betaine salt [EMIM][Betaine], mix well, and fully stir at a speed of 300 rpm for 10 min to obtain a foam mixture liquid.
[0063] Place the foam mixture liquid in a plate and frame filter press for filtration treatment, and collect a first filtrate.
[0064] Centrifuge the filter cake at a speed of 6000 rpm for 10 min, and collect a second filtrate.
[0065] Place the second filtrate in a microwave dryer, and control the microwave drying at 1000 MHz for 1 h to obtain the product.
[0066] Example 6
[0067] Take the sulfur foam, add 8wt% of 1-ethyl-3-methylimidazolium betaine salt [EMIM][Betaine] and 5wt% of esterase microcapsules, mix well, and fully stir at a speed of 300 rpm for 10 min to obtain a foam mixture liquid.
[0068] Place the foam mixture liquid in a plate and frame filter press for filtration treatment, and collect a first filtrate.
[0069] Centrifuge the filter cake at a speed of 6000 rpm for 10 min, and collect a second filtrate.
[0070] Place the second filtrate in a microwave dryer, and control the microwave drying at 1000 MHz for 1 h to obtain the product.
[0071] Comparative Example 1
[0072] The treatment method of the sulfur foam in the present comparative example is the same as that in Example 1, and the only difference is that the foam modifier is selected as betaine chloride salt.
[0073] Comparative Example 2
[0074] The treatment method of the sulfur foam in the present comparative example is the same as that in Example 1, and the only difference is that the foam modifier is selected as betaine sulfate salt.
[0075] Comparative Example 3
[0076] The treatment method of the sulfur foam in the present comparative example is the same as that in Example 1, and the only difference is that the foam modifier is selected as 1-ethyl-3-methylimidazole chloride salt.
[0077] Comparative Example 4
[0078] The treatment method of the sulfur foam in the present comparative example is the same as that in Example 1, and the only difference is that the foam modifier is selected as 1-ethyl-3-methylimidazole hexafluorophosphate.
[0079] Comparative Example 5
[0080] The treatment method of the sulfur foam in the present comparative example is the same as that in Example 1, and the only difference is that the sulfur foam is not modified.
[0081] Experimental Example
[0082] The foam mixture liquid collected in the above-mentioned schemes of Example 1 and Comparative Examples 1-5 is respectively subjected to viscosity monitoring, and the first filter and the second filter are subjected to water content rate testing, and the specific test results are shown in Table 1 below.
[0083] The initial viscosity of the sulfur foam to be treated is 198.43 cp, and the water content rate is 65%.
[0084] Table 1
[0085]
[0086] It can be seen that, after the sulfur foam is treated by using the selected foam modifier according to the gradient centrifugation-microwave drying synergistic concentration method of the present application, the foam and viscosity of the sulfur foam can be effectively improved, which is more conducive to the filtration step, and the colloidal structure between sulfur particles can be destroyed, the influence of polymerized water can be reduced, the concentration and dehydration effects can be effectively improved, and the current problem of difficult dehydration of sulfur foam can be solved.
[0087] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not intended to limit the present application; although the present application has been described in detail with reference to the above embodiments, those skilled in the art should understand that the technical solutions recorded in the above embodiments can still be modified, or some or all of the technical features can be replaced by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the embodiments of the present application.
Claims
1. A sulfur foam gradient centrifuge-microwave drying synergistic concentration method, characterized in that, The method comprises the following steps: (1) taking the sulfur foam to be treated and adding a foam modifier, and stirring and mixing to obtain a sulfur foam slurry; (2) performing first solid-liquid separation on the sulfur foam slurry by filtration to remove part of the water; (3) continuing to perform second solid-liquid separation on the sulfur foam slurry by centrifugation to continue to remove water; (4) collecting the solid part for microwave drying treatment; The foam modifier comprises 1-ethyl-3-methylimidazolium betaine salt.
2. The method of claim 1, wherein the sulfur foam gradient centrifuge-microwave drying synergistic concentration method is characterized by, In the step (2), the first solid-liquid separation step comprises gravity sedimentation or plate and frame filter pressing.
3. The method of claim 2, wherein the sulfur foam gradient centrifuge-microwave drying synergistic concentration method is characterized by, In the step (3), the centrifugal speed of the second solid-liquid separation step is 5000-8000 rpm.
4. The method of claim 3, wherein the sulfur foam gradient centrifuge-microwave drying synergistic concentration method is characterized by, In the step (4), the microwave frequency of the microwave drying step is 900-1200 MHz.
5. The method of claim 4, wherein the sulfur foam gradient centrifuge-microwave drying synergistic concentration method is characterized by, In the step (1), the stirring speed is 200-400 rpm.
6. The method of gradient centrifugal-microwave drying synergistic concentration of sulphur foams according to any one of claims 1 to 5, characterized in that, The addition amount of the foam modifier based on the sulfur foam slurry is 5-10 wt%.
7. The method of gradient centrifugal-microwave drying synergistic concentration of sulphur foams according to any one of claims 1 to 5, characterized in that, The foam modifier further comprises esterase microcapsules.
Citation Information
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