WO2018142651A1 - 酸性ガス処理剤 - Google Patents

酸性ガス処理剤 Download PDF

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Publication number
WO2018142651A1
WO2018142651A1 PCT/JP2017/028719 JP2017028719W WO2018142651A1 WO 2018142651 A1 WO2018142651 A1 WO 2018142651A1 JP 2017028719 W JP2017028719 W JP 2017028719W WO 2018142651 A1 WO2018142651 A1 WO 2018142651A1
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Prior art keywords
acid gas
less
median diameter
diameter
agent
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PCT/JP2017/028719
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English (en)
French (fr)
Japanese (ja)
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恵一 水品
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栗田工業株式会社
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Priority to CN201780074442.2A priority Critical patent/CN110022970B/zh
Priority to KR1020197013783A priority patent/KR102124792B1/ko
Publication of WO2018142651A1 publication Critical patent/WO2018142651A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/81—Solid phase processes
    • B01D53/83—Solid phase processes with moving reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size

Definitions

  • the present invention relates to an acid gas treating agent. More specifically, the present invention provides an acidic gas such as hydrogen chloride and sulfur oxide contained in combustion exhaust gas discharged from facilities for incineration, firing or melting of general waste and industrial waste, biomass power generation boilers, and the like.
  • the present invention relates to an acid gas treating agent to be summed.
  • sodium compounds such as sodium hydrogen carbonate are also commonly used as acid gas treating agents and are widely used.
  • the amount of sodium bicarbonate used is less than that of the slaked lime.
  • Patent Document 1 proposes an acidic component removing agent containing sodium hydrogen carbonate having a volume-based average particle diameter measured by a laser diffraction scattering method of 1 to 9 ⁇ m. According to this remover, acidic components such as hydrogen chloride, sulfur oxide, and nitrogen oxide can be efficiently removed from the exhaust gas, and the disposal process is easy and the amount of waste can be reduced.
  • the volume-based average particle diameter measured by the laser diffraction scattering method is 1 to 9 ⁇ m, and the pore diameter in the pore diameter range of 1 to 10 ⁇ m in the pore distribution by the mercury intrusion method of the powder layer.
  • An acidic component remover containing sodium hydrogen carbonate having a volume of 0.4 cm 3 / g or more has been proposed. According to this removing agent, hydrogen chloride gas can be sufficiently removed by adsorption with a small amount of acidic component removing agent.
  • JP 2000-218128 A Japanese Patent Laid-Open No. 2006-239689
  • the average particle size of sodium hydrogen carbonate is preferably 10 ⁇ m or less.
  • sodium hydrogen carbonate is a fine particle, there are problems that the fine particles are easily aggregated and solidified, and that a pulverization cost and a pulverization time for making the fine particle are required.
  • the present invention has been made in view of such problems, and the problem is that acid gas can be efficiently processed even with a small amount, and the caking property and the differential pressure increase in the bag filter are greatly improved. It is possible to provide an acid gas treating agent that is also excellent in cost.
  • the present inventors pay attention to the ratio of the mode diameter (D m ) to the median diameter (D m / D 50 ), and the range of this ratio is kept constant. By making it within the range, it was found that the above problems could be solved at once, and the present invention was completed. Specifically, the present invention provides the following.
  • the present invention is a sodium hydrogen carbonate having a median diameter (D 50 ) of 11 ⁇ m or more and 25 ⁇ m or less, and a ratio of the mode diameter (D m ) to the median diameter (D m / D 50 ) of 2.0 or less.
  • the median diameter (D 50 ) is a particle diameter at which the integrated value on the mass basis in the particle size distribution measured by the laser diffraction / scattering particle size distribution measuring device is 50%.
  • the mode diameter (D m ) is a particle diameter at which the relative particle amount in the particle size distribution measured by the laser diffraction / scattering particle size distribution measuring device is maximized.
  • the difference between the median diameter (D 50 ) of the sodium hydrogen carbonate and the accumulated weight 30% diameter (D 30 ) is 15 ⁇ m or less
  • the accumulated weight 70% diameter of the sodium hydrogen carbonate The acid gas treating agent according to (1), wherein a difference between (D 70 ) and the median diameter (D 50 ) is 15 ⁇ m or less.
  • the cumulative weight 30% diameter (D 30 ) is a particle diameter at which the cumulative value on the mass basis in the particle size distribution measured by the laser diffraction / scattering particle size distribution measuring device is 30%.
  • the cumulative weight 70% diameter (D 70 ) is a particle diameter at which the cumulative value on the mass basis in the particle size distribution measured by the laser diffraction / scattering particle size distribution measuring device is 70%.
  • the present invention further includes an anti-caking agent, and the anti-caking agent includes at least one selected from a hydrophilic substance, a hydrophobic substance, and a clay mineral, (1) Or it is an acidic gas processing agent as described in (2).
  • the anti-caking agent is one or more of wet silica, calcium stearate, zeolite, hydrophobic silica, hydrophilic fumed silica, white carbon, basic magnesium carbonate, and carbon black. It is an acidic gas processing agent as described in (3) containing.
  • this invention is an acid gas processing method of collecting fly ash after adding the acid gas processing agent in any one of (1) to (4) to acid gas.
  • the present invention it is possible to efficiently process acid gas even in a small amount, and to significantly improve the caking property and the differential pressure increase in the bag filter, and to provide an acid gas treating agent excellent in cost. Can do.
  • the schematic structure of the acidic gas processing apparatus 10 used by the present Example is shown.
  • the schematic structure of the load test apparatus 30 used in order to evaluate the caking property of an acidic gas processing agent is shown.
  • the acidic gas treating agent of this embodiment contains sodium hydrogen carbonate.
  • Sodium bicarbonate functions as a neutralizing agent for acid gas.
  • the acid gas treating agent preferably further contains an anti-caking agent as required.
  • Sodium bicarbonate obtained by pulverizing crude sodium bicarbonate is preferably used.
  • the lower limit of the median diameter (D 50 ) of sodium hydrogen carbonate is 11 ⁇ m or more, preferably 12.5 ⁇ m or more, more preferably 15 ⁇ m or more, and particularly preferably 17 ⁇ m or more. If the median diameter (D 50 ) is too small, the sodium hydrogen carbonate fine particles are likely to aggregate and solidify, which is not preferable. Moreover, since the grinding
  • the upper limit of the median diameter (D 50 ) of sodium hydrogen carbonate is 25 ⁇ m or less, preferably 21 ⁇ m or less, and more preferably 19.5 ⁇ m or less.
  • the amount of sodium carbonate required for treating the acid gas is within a range of a suitable equivalent ratio with respect to the concentration of the acid gas at the bag filter inlet (for example, 1.0 or more and 5. 0 or less), which is not preferable.
  • the ratio of the mode diameter to the median size of the sodium hydrogen carbonate (D 50) (D m) (D m / D 50) is 2.0 or less, preferably 1.5 or less, 1.3 or less More preferably. If the ratio (D m / D 50 ) is large, the acidic gas cannot be sufficiently treated even if the median diameter (D 50 ) is within an appropriate range.
  • the lower limit of the ratio (D m / D 50 ) is not particularly limited, but since the mode diameter (D m ) is larger than the median diameter (D 50 ), the lower limit of the ratio (D m / D 50 ) is It is 1.00 or more.
  • the upper limit of the difference (D 50 -D 30 ) between the median diameter (D 50 ) of sodium hydrogen carbonate and the 30% cumulative weight diameter (D 30 ) is preferably 15 ⁇ m or less, more preferably 10 ⁇ m or less. preferable.
  • the lower limit of the difference (D 50 -D 30 ) is not particularly limited as long as it exceeds 0 ⁇ m. However, in order to increase the product yield and provide an acid gas treating agent excellent in cost, the difference (D 50 The lower limit of ⁇ D 30 ) is preferably 1 ⁇ m or more, and more preferably 3 ⁇ m or more.
  • the upper limit of the difference (D 70 -D 50 ) between the 70% cumulative weight (D 70 ) and median diameter (D 50 ) of sodium hydrogen carbonate is preferably 15 ⁇ m or less, and more preferably 10 ⁇ m or less.
  • the lower limit of the difference (D 70 -D 50 ) is not particularly limited as long as it exceeds 0 ⁇ m.
  • the difference (D 70 The lower limit of ⁇ D 50 ) is preferably 1 ⁇ m or more, more preferably 3 ⁇ m or more, and further preferably 5 ⁇ m or more.
  • the processing performance of acid gas is enhanced by the sharp particle size distribution. Further, since the particle size distribution is sharp, solidification of the acid gas treating agent can be suppressed, and as a result, the handling performance of the apparatus is enhanced.
  • the acidic gas treating agent preferably contains sodium hydrogen carbonate and an anti-caking agent.
  • the anti-caking agent preferably contains at least one selected from a hydrophilic substance, a hydrophobic substance, and a clay mineral.
  • hydrophilic means a property that is insoluble in water but has a hydrophilic group on the surface of the substance, and the surface of the substance is easily wetted with water (does not form water droplets or repels).
  • a substance having Examples of the hydrophilic substance include hydrophilic silica (hydrophilic fumed silica and the like).
  • hydrophobic refers to a substance that is insoluble in water and does not have a hydrophilic group on the surface of the substance.
  • examples of the hydrophobic substance include calcium stearate and hydrophobic silica.
  • clay minerals include zeolite, diatomaceous earth, and activated clay.
  • the anti-caking agent preferably contains calcium stearate.
  • anti-caking agents such as white carbon, basic magnesium carbonate, carbon black, calcium carbonate, magnesium carbonate, magnesium hydroxide, ammonium citrate, anhydrous magnesium sulfate, anhydrous sodium phosphate, blast furnace slag, aluminum oxide, etc. It may be included.
  • the lower limit of the content is not particularly limited as long as the acid gas treating agent can be caking and preventing fluidity from being lowered.
  • the content of the anti-caking agent is preferably 0.1 parts by mass or more and more preferably 0.2 parts by mass or more with respect to 100 parts by mass of sodium bicarbonate.
  • the upper limit of the content is not particularly limited as long as it does not affect the treatment of the desalted residue.
  • the content of the anti-caking agent is preferably 3.0 parts by mass or less, more preferably 1.0 part by mass or less, and 0.8 parts by mass with respect to 100 parts by mass of sodium bicarbonate. Or less, more preferably 0.6 parts by mass or less.
  • the preparation of the acid gas treating agent can be obtained through the following steps. (1) Grinding of crude baking soda (sodium bicarbonate with a large particle size) (2) Mixing of ground baking soda (sodium bicarbonate) with an anti-caking agent as required
  • the crude baking soda is pulverized, and the median diameter (D 50 ), the ratio of the mode diameter (D m ) to the median diameter (D 50 ) (D m / D 50 ), and the like are adjusted within specified ranges.
  • the median diameter (D 50 ) and the like are adjusted by adjusting the setting values of the grinding rotor and classification rotor in the grinder based on the particle size of the raw material of crude sodium bicarbonate and the raw material supply amount of the crude sodium bicarbonate.
  • the acid gas treating agent is added to exhaust gas containing acid gas to perform exhaust gas treatment.
  • the acid gas treating agent is supplied to the flue, and the acid gas treating agent is brought into contact with the exhaust gas containing the acid gas.
  • the type of exhaust gas is not particularly limited, and examples thereof include exhaust gas containing acidic gas such as hydrogen chloride and sulfur oxide generated in a waste treatment facility, a combustion facility such as a biomass boiler and a coal boiler.
  • the timing of supplying the acid gas treating agent is not particularly limited as long as it is before dust collection by the dust collector.
  • the timing of incineration of waste in an incinerator, the exhaust gas generated by incineration is smoke
  • the timing between passing the road and reaching the temperature reduction tower that reduces the temperature of the exhaust gas, after cooling the exhaust gas in the temperature reduction tower, until the exhaust gas after cooling reaches the bag filter provided in front of the dust collector The timing of this is mentioned.
  • the supply amount of the acid gas treating agent is not particularly limited. To avoid both excessive and excessive, adjust the concentration of acid gas passing through the flue while monitoring it appropriately and supply it to satisfy the management target value for each target combustion facility. Is preferred.
  • the lower limit of the supply amount of the acidic gas treating agent is preferably 0.1 g / m 3 or more, more preferably 1 g / m 3 or more, and 10 g / m 3 or more. More preferably.
  • the lower limit of the supply amount of the acidic gas treating agent is preferably 1.0 or more, more preferably 1.2 or more in terms of equivalent ratio with respect to the concentration of acidic gas at the bag filter inlet, More preferably, it is 1.4 or more.
  • the upper limit of the supply amount of the acid gas treatment agent is preferably within a range of 200 g / m 3 or less, and a range of 150 g / m 3 or less. More preferably, it is within.
  • the upper limit of the supply amount of the acidic gas treating agent is preferably 5.0 or less, more preferably 3.0 or less in terms of equivalent ratio with respect to the concentration of acidic gas at the bag filter inlet, More preferably, it is 2.0 or less.
  • the fly ash containing the reaction product of the acid gas and the acid gas treating agent and the unreacted material as components is collected.
  • the fly ash may be collected by a known dust collector such as a bag filter.
  • Example 1 Relationship between particle size of sodium hydrogen carbonate, acid gas treatment performance and solidification [comparison of acid gas treatment performance] [Test conditions] The acid gas treatment performance of the six types of sodium carbonate listed in Table 1 was compared using the acid gas treatment apparatus 10 shown in FIG. The diameter of sodium carbonate was measured using SALD-7500 nano manufactured by Shimadzu Corporation.
  • FIG. 1 shows a schematic configuration of an acid gas treatment apparatus 10 used in this example.
  • the acid gas treatment device 10 includes a heater 11 that heats the acid gas, an acid gas treatment agent supplier 13 that supplies the acid gas treatment agent to the acid gas that is output from the heater 11, and a reaction between the acid gas and the acid gas treatment agent.
  • a bag filter 15 that collects the product and unreacted material, a cooling tower 17 that cools the dust collected by the bag filter 15, a neutralization tower 18 that neutralizes the cooled dust collection, And an induction blower 19 for discharging the neutralized product neutralized by the neutralization tower 18 to the outside of the system.
  • a pressure gauge P1 and a hydrogen chloride concentration measuring device are provided at a location corresponding to the inlet of the bag filter 15 in the pipe 12 from the heater 11 to the acidic gas treating agent supply machine 13.
  • the pressure gauge P1 and the hydrogen chloride concentration measuring device can measure the inlet pressure of the bag filter 15 and the concentration of hydrogen chloride contained in the acid gas.
  • a pressure gauge P2 and a hydrogen chloride concentration measuring device are provided at a location corresponding to the outlet of the bag filter 15.
  • the outlet pressure of the bag filter 15 and the hydrogen chloride concentration contained in the collected dust collected by the bag filter 15 can be measured by the pressure gauge P2 and the hydrogen chloride concentration measuring device.
  • an ion electrode type hydrogen chloride meter HL-22 manufactured by Kyoto Electronics Co., Ltd. was used as the hydrogen chloride measuring device.
  • Example 1 The test conditions in Example 1 are as follows. Exhaust gas amount: 0.28 Nm 3 -dry / min Hydrogen chloride concentration at the inlet of the bag filter 15: 250 ppm (407 mg / Nm 3 ) Moisture content: 10% Bag filter temperature: 170 ° C Amount of acid gas treatment agent added: 1.5 equivalent ratio to the inlet hydrogen chloride concentration Acid gas treatment agent addition time: 90 minutes with continuous addition
  • the load test apparatus 30 includes a frame-shaped rod 31 of 100 mm ⁇ 100 mm and a 10 kg weight 32 for applying a load to a sample (acid gas treatment agent) accommodated in the frame-shaped rod 31.
  • the acid gas treating agent S is mixed with the first sieve and the second sieve.
  • the ratio of the sieve residue to the weight of the acid gas treating agent S used for the test (unit: weight) %) was calculated. It shows that the caking property of an acidic gas processing agent is so small that the ratio of this sieve residue is small. Using the ratio of the sieve residue as an index, the caking property of each acid gas treating agent was evaluated.
  • Sodium hydrogen carbonate having a median diameter (D 50 ) of 11 ⁇ m or more and 25 ⁇ m or less and a ratio of the mode diameter (D m ) to the median diameter (D m / D 50 ) of 2.0 or less is a high acid gas. It had processing performance (Examples 1-1 to 1-3). Because of its excellent acid treatment performance, it is expected to reduce the environmental burden such as extending the life of the final disposal site by reducing the amount of dust and reducing the COD of leachate.
  • the sodium hydrogen carbonate is also excellent in anti-caking property (Examples 1-1 to 1-3).
  • the anti-caking property is further improved (Examples 1-2 and 1-3), and when it is 17 ⁇ m or more, the anti-caking property is further improved (implementation).
  • Example 1-3 when the median diameter (D 50 ) is 15 ⁇ m or more, the anti-caking property is further improved (Examples 1-2 and 1-3), and when it is 17 ⁇ m or more, the anti-caking property is further improved (implementation).
  • the manufacturing cost is reduced.
  • the grinding time of the crude baking soda can be shortened and the amount of grinding can be increased, so that the acidic gas treating agent can be stably supplied.
  • Example 2 Comparison of anti-caking agents [caking property of acid gas treating agent]
  • the anti-caking agent shown in Table 2 was mixed in the proportion shown in Table 2 with respect to 100% by weight of sodium hydrogen carbonate having the particle size shown in Table 2 to obtain various acid gas treating agents. Then, the acid gas treating agent was consolidated by the same method as in Example 1. The results are shown in Table 2.
  • an anti-caking agent When an anti-caking agent is added to sodium bicarbonate having a median diameter (D 50 ) of 11 ⁇ m or more and 25 ⁇ m or less and a ratio of the mode diameter (D m ) to the median diameter (D m / D 50 ) of 2.0 or less Compared with the case where no anti-caking agent is added, the anti-caking property is more excellent (Examples 2-2 to 2-5, 2-12 to 2-15, 2-22 to 2-25). In particular, when the anti-caking agent contains calcium stearate, it has particularly excellent anti-caking properties (Examples 2-4, 2-5, 2-14, 2-15, 2-24, 2-25). ).
  • Sodium bicarbonate having a median diameter (D 50 ) of 11 ⁇ m or more and 25 ⁇ m or less and a ratio of the mode diameter (D m ) to the median diameter (D m / D 50 ) of 2.0 or less is a kind of anti-caking agent.
  • the pressure loss of the bag filter reaches 0.5 kPa, the number of times of automatic backwashing is small, the acid gas treatment agent is excellent in peelability from the bag filter, and the increase in the pressure loss of the bag filter is prevented. It was confirmed that it was possible (Examples 2-1 to 2-5, 2-11 to 2-15, 2-21 to 2-25). This is presumably because sodium bicarbonate particles and anti-caking agent particles were prevented from entering the filter cloth, and a stable filtration layer was formed on the filter cloth surface.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Biomedical Technology (AREA)
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  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Processing Of Solid Wastes (AREA)
PCT/JP2017/028719 2017-02-01 2017-08-08 酸性ガス処理剤 WO2018142651A1 (ja)

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Application Number Priority Date Filing Date Title
CN201780074442.2A CN110022970B (zh) 2017-02-01 2017-08-08 酸性气体处理剂
KR1020197013783A KR102124792B1 (ko) 2017-02-01 2017-08-08 산성가스 처리제

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JP2017016548A JP6350690B1 (ja) 2017-02-01 2017-02-01 酸性ガス処理剤
JP2017-016548 2017-02-01

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KR101996926B1 (ko) * 2018-11-27 2019-07-05 한국화학연구원 산성오염물질 제거용 비드 및 이의 제조방법
KR102234692B1 (ko) * 2019-05-28 2021-04-02 한국화학연구원 오염물질 제거용 스마트 비드
KR102043186B1 (ko) * 2019-05-15 2019-11-12 한국화학연구원 무기산 제거용 비드 및 이의 제조방법
KR20240003494A (ko) 2022-07-01 2024-01-09 (주)청해소재 산성가스 중화제 조성물

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