CN115074164B - Method for cleaning and removing key harmful elements in hard-to-float bituminous coal - Google Patents
Method for cleaning and removing key harmful elements in hard-to-float bituminous coal Download PDFInfo
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Abstract
The invention relates to the technical field of coal processing, in particular to an integrated cleaning and removing method for key harmful elements in hard-to-float bituminous coal, which comprises the following steps: in the first step, crushed hard-to-float bituminous coal and pure water are added into an electrolytic tank, and 30% H with required quantity is added into the electrolytic tank 2 O 2 Electrolyzing for 10min to 80min under ultrasonic and stirring to obtain bituminous coal mixed solution; and secondly, filtering the bituminous coal mixed solution after the electrolysis is completed, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed. The invention adopts ultrasonic wave combined electrolysis technology, adopts clean and economical 30% H by ultrasonic electrochemical method 2 O 2 As electrolyte, the integrated effective removal of harmful substances such as sulfur, chlorine, mercury, arsenic, lead, sodium oxide in ash and the like in the hard-to-float bituminous coal is realized, and meanwhile, the moisture is obviously reduced and the heat value is improved.
Description
Technical Field
The invention relates to the technical field of coal processing, in particular to an integrated cleaning and removing method for key harmful elements in hard-to-float bituminous coal.
Background
With the increasing technical requirements of the country on the clean processing and utilization of coal. In the aspect of coal processing and utilization, the utilization ratio of coal for power generation is up to 75%. The traditional power coal for power generation is mainly obtained by a method of physically washing and easily floating raw coal, and has low sulfur, low ash, low water and high heat productivity.
The coal washing and separation are main industrial coal cleaning technological means, and the flotation, jigging and coal washing, heavy medium coal washing and the like are common wet coal separation methods, and the wind coal separation, the composite coal separation, the air heavy medium fluidized bed coal separation and the like are common dry coal separation methods. The wet coal washing technology has long application time, mature and reliable technology, needs to consume a large amount of water resources, generates a large amount of coal slime, and causes pollution due to a large amount of harmful substances in wastewater. The dry coal preparation method is simple, efficient and environment-friendly, does not need water resources, and is suitable for the north with water shortage and coldness. However, the dry coal dressing technology is relatively immature, the high-power equipment has high energy consumption, and the screening range is small, so that part of coal resources are wasted. The wet coal preparation and the dry coal preparation are essentially raw coal physical washing, separation is realized by means of density gravity difference of clean coal, medium coal, gangue and the like, and the method has a good effect of removing inorganic sulfur, elemental sulfur and ash, and is difficult to remove harmful elements in organic state coal.
As a representative wet washing method, a flotation method is mainly used for easily floating coal, and the separation of harmful elements and coal in the flotation process is realized by utilizing the hydrophobicity of the surfaces of coal particles and the hydrophilicity of part of the physical inlaid harmful elements. The flotation can effectively remove various harmful elements which are partially physically inlaid on the surfaces of coal particles, and the harmful elements in the coal are difficult to remove when the organic state is endowed. Therefore, how to realize the integrated removal of harmful elements in the coal is particularly necessary, and the removal of harmful elements in the water phase of wet-process coal washing is also important. The harmful elements existing in the organic state often need solvent extraction or chemical conversion, extraction and dissolution or conversion into an ionic state which is easy to dissolve in water, and transfer to a solvent phase or an aqueous phase to realize separation from coal. Traditional organic solvent extraction and electrochemical conversion are concentrated on removal of sulfur of a single harmful element, and reports on integrated removal of the harmful element are provided.
In a word, the research on how to effectively realize clean, economical and efficient utilization of the raw coal difficult to float, especially how to integrally remove harmful sulfur, chlorine, mercury, lead, sodium oxide in ash and the like in the raw coal, simultaneously reduce the moisture and improve the heat value is relatively lacking. In addition, the existing method for removing harmful elements in coal generates a large amount of wastewater or organic waste liquid, wherein the large amount of harmful elements cause pollution, and the treatment cost is high.
Disclosure of Invention
The invention provides an integrated cleaning and removing method for key harmful elements in hard-to-float bituminous coal, which overcomes the defects of the prior art, and can effectively solve the problem that the prior art cannot integrally remove harmful sulfur, chlorine, mercury, lead and sodium oxide in ash in raw coal.
The technical scheme of the invention is realized by the following measures: the integrated cleaning and removing method for the key harmful elements in the hard-to-float bituminous coal comprises the following steps: in the first step, crushed hard-to-float bituminous coal and pure water are added into an electrolytic tank, and 30% H with required quantity is added into the electrolytic tank 2 O 2 Electrolyzing for 10min to 80min under ultrasonic and stirring to obtain bituminous coal mixed solution;
and secondly, filtering the bituminous coal mixed solution after the electrolysis is completed, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed.
The following are further optimizations and/or improvements to the above-described inventive solution:
in the first step, the mass ratio of the hard-to-float bituminous coal to the pure water is 1:5 to 1:10.
In the first step, 30% H 2 O 2 The volume-mass ratio of the coal to the hard-to-float bituminous coal is 1L/20kg to 1L/120kg.
In the first step, the electrode used for electrolysis is a platinum electrode, the electrolysis is carried out at 20-70 ℃ and the current density is 40mA/cm 2 To 160mA/cm 2 The electrolysis voltage is 10V to 60V.
In the first step, the stirring speed is 100rpm to 400rpm.
In the first step, the particle size of the pulverized hard-to-float bituminous coal is 0 to 0.2mm.
The method for integrally cleaning and removing the key harmful elements in the hard-to-float bituminous coal further comprises a third step of performing membrane filtration on the filtrate obtained by the filtration in the second step.
In the third step, the membrane filtration is performed under the conditions of a pressure of 0.1MPa to 0.5MPa, a temperature of 20 ℃ to 40 ℃ and a pH of 5 to 8.
In the third step, the filtering membrane is one of a reverse osmosis membrane combined nanofiltration membrane, a microfiltration membrane and an ultrafiltration membrane.
The invention adopts ultrasonic wave combined electrolysis technology, adopts clean and economical 30% H by ultrasonic electrochemical method 2 O 2 As electrolyte, the integrated effective removal of harmful substances such as sulfur, chlorine, mercury, arsenic, lead, sodium oxide in ash and the like in the hard-to-float bituminous coal is realized, and meanwhile, the moisture is obviously reduced and the heat value is improved. In addition, the harmful elements transferred to the water phase are subjected to membrane separation, and the water purification and the recycling of the elements are realized by utilizing reverse osmosis membrane separation.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention. The various chemical reagents and chemical supplies mentioned in the invention are all commonly known and used in the prior art unless specified otherwise; the percentages in the invention are mass percentages unless specified otherwise; the solutions in the invention are aqueous solutions in which the solvent is water unless otherwise specified, for example, the hydrochloric acid solution is hydrochloric acid aqueous solution; the room temperature and the room temperature in the present invention generally refer to temperatures ranging from 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
In the present invention, unless otherwise specified, the devices and apparatuses used are all known and commonly used in the art.
The invention is further described below with reference to examples:
example 1: the method for integrally cleaning and removing key harmful elements in the hard-to-float bituminous coal comprises the following steps:
in the first step, crushed hard-to-float bituminous coal and pure water are added into an electrolytic tank, and 30% H with required quantity is added into the electrolytic tank 2 O 2 Electrolyzing for 10min to 80min under ultrasonic and stirring to obtain bituminous coal mixed solution;
and secondly, filtering the bituminous coal mixed solution after the electrolysis is completed, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed.
The invention selects 30% H 2 O 2 As the electrolyte, a strong oxidizing electrolyte such as KMnO is used more than the prior art 4 Strongly reducing electrolytes such as KI, neutral electrolytes such as NaCl, etc., 30% H 2 O 2 The electrolyte can effectively avoid the introduction of harmful elements, and simultaneously can effectively realize the electrochemical conversion of key harmful elements in the hard-to-float bituminous coal under the action of electrolysis, and the key harmful elements are transferred to the water phase to be stripped from the raw coal.
Taking sulfur element in hard-to-float bituminous coal as an example, sulfur (such as pyrite sulfur, alcohol sulfur and thiophene sulfur) in different forms in the hard-to-float bituminous coal is converted into water-soluble SO after ultrasonic electrolysis 4 2- . OH in hydrogen peroxide under hydrogen peroxide electrolyte as shown in formulas 1 to 5 - And H + Respectively carrying out oxidation reaction and reduction reaction on the anode and the cathode, and the anode OH - Electrolytic production of O 2 FeS which is inorganic can be used 2 S in (C) is converted into SO 4 2- And simple substance S, which converts organic sulfur alkoxide and thiophenic sulfur into SO 4 2- . Other harmful elements are transferred to the water phase after ultrasonic electrolysis and exist in the water phase in an ionic state. Wherein, chlorine element in the coal is mainly added in sodium salt, potassium salt and organic chlorine, lead element in the coal is mainly added in silicon aluminum compound, and chlorine and lead are transferred to water phase after ultrasonic electrolytic decomposition. Mercury and arsenic are mainly contained in sulfides, and are removed by stripping of sulfur. In addition, after ultrasonic electrolysis treatment, the moisture in the treated bituminous coal is reduced due to the electrochemical dehydration in the bituminous coal difficult to float; and the amount of heat generated by the bituminous coal is increased to a certain extent after the treatment due to the increase of the carbon content in the coal caused by the dissociation of partial inorganic matters and organic matters in the electrochemical conversion.
Anode:
2O 2 +FeS 2 ——→FeSO 4 +S (2)
And (3) cathode:
example 2: as an optimization of the above embodiment, in the above first step, the mass ratio of the hard-to-float bituminous coal to the pure water is 1:5 to 1:10.
Example 3: as an optimization of the above example, in the above first step, 30% H 2 O 2 The volume-mass ratio of the coal to the hard-to-float bituminous coal is 1L/20kg to 1L/120kg.
Example 4: as an optimization of the above embodiment, in the above first step, the electrode used for electrolysis is a platinum electrode, the electrolysis is performed at 20℃to 70℃and the current density is 40mA/cm 2 To 160mA/cm 2 The electrolysis voltage is 10V to 60V.
Example 5: as an optimization of the above embodiment, in the above first step, the stirring speed was 100rpm to 400rpm.
Example 6: as an optimization of the above embodiment, in the above first step, the particle size of the hard-to-float bituminous coal after pulverization is 0 to 0.2mm.
Example 7: as an optimization of the above embodiment, the method for integrally cleaning and removing the key harmful elements in the hard-to-float bituminous coal further includes a third step of performing membrane filtration on the filtrate obtained by the filtration in the second step.
In the invention, sulfur, chlorine, lead, mercury, arsenic and the like in the bituminous coal are in ionic state to be in the water phase of the bituminous coal mixed liquid after ultrasonic electrolysis. Therefore, the separation of harmful elements in the aqueous phase and the purification treatment of water are particularly necessary. This patent carries out the purification treatment of filtrate through reverse osmosis membrane separation, gets rid of sulfur, chlorine, plumbum, mercury, arsenic in the aqueous phase, realizes the purification utilization of water. Meanwhile, sulfur, chlorine, lead, mercury and arsenic can be enriched and recovered, and part of metal ions can be recovered through subsequent treatment, so that lead, mercury and arsenic elements can be recovered and reused.
Example 8: as an optimization of the above embodiment, in the above third step, the membrane filtration is performed under the conditions of a pressure of 0.1MPa to 0.5MPa, a temperature of 20℃to 40℃and a pH of 5 to 8.
Example 9: as an optimization of the above embodiment, in the third step, the filtration membrane is one of a reverse osmosis membrane combined nanofiltration membrane, a microfiltration membrane, and an ultrafiltration membrane.
Example 10: the method for integrally cleaning and removing key harmful elements in the hard-to-float bituminous coal comprises the following steps:
firstly, adding crushed hard-to-float bituminous coal (bituminous coal of certain power plant in Xinjiang) and pure water into an electrolytic tank according to a mass ratio of 1:7, and adding 30% H into the electrolytic tank 2 O 2 30% H is added to the hard-to-float bituminous coal at the ratio of 1L/40kg 2 O 2 Electrolyzing for 60min under ultrasonic and stirring to obtain bituminous coal mixed solution; electrolysis was carried out at 25℃using platinum electrodes with a current density of 125mA/cm 2 The electrolysis voltage was 30V and the stirring speed was 180rpm.
Step two, after the electrolysis is completed, filtering the bituminous coal mixed solution, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed;
and thirdly, carrying out membrane filtration on the filtrate obtained by the filtration in the second step by adopting a nanofiltration membrane combined with a reverse osmosis membrane, and removing sulfur, chlorine, lead, mercury and arsenic in the filtrate. The membrane filtration was carried out at a pressure of 2.0MPa, a temperature of 40℃and a pH of 6.8.
Harmful element analysis and industrial analysis were performed on the hard-to-float bituminous coal before and after the treatment, and the results are shown in table 1. As can be seen from Table 1, the sulfur, chlorine, mercury, arsenic, lead and sodium oxide in the hard-to-float bituminous coal are reduced by 81.1%, 71.9%, 62.7%, 75.0%, 60.0%, 46.1% in order, and the air-dried base moisture (M ad ) The reduction is 65.3 percent. In addition, the method for measuring the heating value of GB/T213-2008 coal is used for the treatment before and afterThe refractory bituminous coal was tested with a heating value increased from 23.64MJ/kg before treatment to 26.15MJ/kg after treatment.
Example 11: the method for integrally cleaning and removing key harmful elements in the hard-to-float bituminous coal comprises the following steps:
firstly, adding crushed hard-to-float bituminous coal (Xinjiang bituminous coal I) and pure water into an electrolytic tank according to a mass ratio of 1:7, and adding 30% H into the electrolytic tank 2 O 2 30% H is added to the hard-to-float bituminous coal at the ratio of 1L/80kg 2 O 2 Electrolyzing for 40 min under ultrasonic and stirring to obtain bituminous coal mixed solution; electrolysis was carried out at 30℃using platinum electrodes with a current density of 83mA/cm 2 The electrolysis voltage was 40V and the stirring speed was 150rpm.
Step two, after the electrolysis is completed, filtering the bituminous coal mixed solution, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed;
and thirdly, carrying out membrane filtration on the filtrate obtained by the filtration in the second step by adopting a nanofiltration membrane combined with a reverse osmosis membrane, and removing sulfur, chlorine, lead, mercury and arsenic in the filtrate. The membrane filtration was carried out at a pressure of 2.0MPa, a temperature of 40℃and a pH of 6.5.
The harmful element analysis was performed on the hard-to-float bituminous coal before and after the treatment, and the results are shown in table 2. As can be seen from Table 2, the sulfur, chlorine, mercury, arsenic, lead and sodium oxide in the hard-to-float bituminous coal are sequentially reduced by 76.7%, 73.3%, 81.1%, 75.0%, 83.3%, 42.0% and the air-dried base moisture (M) ad ) The reduction is 84.9%. In addition, the refractory bituminous coal before and after treatment was tested according to the calorific value measurement method of GB/T213-2008 coal, and the calorific value was increased from 26.11MJ/kg before treatment to 27.62MJ/kg after treatment.
Example 12: the method for integrally cleaning and removing key harmful elements in the hard-to-float bituminous coal comprises the following steps:
firstly, adding crushed hard-to-float bituminous coal (Xinjiang bituminous coal II) and pure water into an electrolytic tank according to a mass ratio of 1:10, and adding 30% H into the electrolytic tank 2 O 2 Adding 30% H at a ratio of 1L/48kg to refractory bituminous coal 2 O 2 Electrolyzing for 40 min under ultrasonic and stirring to obtain bituminous coal mixed solution; electrolysis was carried out at 50℃using platinum electrodes with a current density of 63mA/cm 2 The electrolysis voltage was 40V and the stirring speed was 200rpm.
Step two, after the electrolysis is completed, filtering the bituminous coal mixed solution, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed;
and thirdly, carrying out membrane filtration on the filtrate obtained by the filtration in the second step by adopting a nanofiltration membrane combined with a reverse osmosis membrane, and removing sulfur, chlorine, lead, mercury and arsenic in the filtrate. The membrane filtration was carried out at a pressure of 2.0MPa, a temperature of 40℃and a pH of 6.3.
The harmful element analysis was performed on the hard-to-float bituminous coal before and after the treatment, and the results are shown in table 3. As can be seen from Table 3, the sulfur, chlorine, mercury, arsenic, lead and sodium oxide in the hard-to-float bituminous coal are reduced by 74.4%, 83.5%, 71.9%, 76.7%, 75.0%, 52.6% in sequence, and the air-dried base moisture (M ad ) The reduction is 62.3 percent. In addition, the refractory bituminous coal before and after treatment is tested according to the calorific value measuring method of GB/T213-2008 coal, and the calorific value is increased from 26.79MJ/kg before treatment to 27.48MJ/kg after treatment.
The invention adopts ultrasonic wave combined electrolysis technology, adopts clean and economical 30% H by ultrasonic electrochemical method 2 O 2 As electrolyte, the integrated effective removal of harmful substances such as sulfur, chlorine, mercury, arsenic, lead, sodium oxide in ash and the like in the hard-to-float bituminous coal is realized, wherein the removal rate of sulfur and chlorine can reach more than 70%, the removal rate of mercury, arsenic and lead can reach more than 60%, the sodium oxide in ash is reduced by more than 40%, and meanwhile, the moisture is obviously reduced, and the heat value is improved. In addition, the invention carries out membrane separation on the harmful elements transferred to the water phase, and realizes water purification and element recycling by using reverse osmosis membrane separation.
As described above, the present invention employs clean, economical 30% H by the ultrasonic electrochemical method 2 O 2 As electrolyte, the method effectively solves the problems of removing harmful sulfur, chlorine, mercury, lead and sodium oxide in ash in raw coal, and simultaneously remarkably reduces water content and improves the quality of the raw coalThe heat value, the solution is clean and environment-friendly, and is convenient for industrial application.
The technical characteristics form the embodiment of the invention, have stronger adaptability and implementation effect, and can increase or decrease unnecessary technical characteristics according to actual needs so as to meet the requirements of different situations.
TABLE 1
TABLE 2
TABLE 3 Table 3
Claims (5)
1. The integrated cleaning and removing method for the key harmful elements in the hard-to-float bituminous coal is characterized by comprising the following steps of: firstly, adding crushed hard-to-float bituminous coal and pure water into an electrolytic tank, and adding a required amount of H with the mass fraction of 30% into the electrolytic tank 2 O 2 Electrolyzing for 10min to 80min under ultrasonic and stirring to obtain bituminous coal mixed solution; step two, after the electrolysis is completed, filtering the bituminous coal mixed solution, and drying filter residues obtained by filtering to obtain the refractory bituminous coal from which the sulfur, chlorine, lead, mercury, arsenic and sodium oxide in ash are removed; wherein in the first step, the electrode adopted for electrolysis is a platinum electrode, the electrolysis is carried out at 20-70 ℃ and the current density is 40mA/cm 2 Up to 160mA/cm 2 The electrolysis voltage is 10V to 60V, and the stirring speed is 100rpm to 400rpm.
2. The integrated cleaning and removing method for key harmful elements in hard-to-float bituminous coal according to claim 1, wherein in the first step, the mass ratio of the hard-to-float bituminous coal to pure water is 1:5 to 1:10, and the mass fraction of H is 30 percent 2 O 2 The volume-mass ratio of the coal to the hard-to-float bituminous coal is 1L/20kg to 1L/120kg.
3. The method for integrated cleaning and removing of key and harmful elements in hard-to-float bituminous coal according to claim 1 or 2, wherein the method for integrated cleaning and removing of key and harmful elements in hard-to-float bituminous coal further comprises a third step of membrane filtration of the filtrate obtained by the filtration in the second step.
4. The integrated cleaning and removing method for key harmful elements in hard-to-float bituminous coal according to claim 3, wherein in the third step, the membrane filtration is performed under the conditions of 0.1MPa to 0.5MPa, 20 ℃ to 40 ℃ and pH 5 to 8.
5. The method for integrated cleaning and removing key harmful elements in hard-to-float bituminous coal according to claim 3, wherein in the third step, the filtering membrane is one of a reverse osmosis membrane combined nanofiltration membrane, a microfiltration membrane and an ultrafiltration membrane.
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