CN110404525B - Catalyst with sulfur resistance for catalytic oxidation of NO, preparation method and application thereof - Google Patents
Catalyst with sulfur resistance for catalytic oxidation of NO, preparation method and application thereof Download PDFInfo
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- 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
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention relates to a catalyst with sulfur resistance for catalytic oxidation of NO, a preparation method and application thereof, wherein the catalyst is boric acid modified activated carbon, and the mass content of boron is 0.01-2%. The catalyst is obtained by mixing aqueous solution of boric acid and activated carbon powder, performing rotary evaporation, calcining in nitrogen atmosphere, and cooling. The preparation method disclosed by the invention is simple in process flow, simple and convenient to operate, low in cost and easy for mass production; the required raw materials are clean and environment-friendly, have no harmful substances, do not generate secondary pollution, and accord with the concept of green chemistry; the prepared modified activated carbon has good sulfur resistance when being used for NOCO, and the activation time is extended by 25-300% compared with that before modification.
Description
Technical Field
The invention relates to the field of industrial waste gas treatment, in particular to a catalyst with sulfur resistance for catalytic oxidation of NO, a preparation method and application thereof.
Background
In recent years, nitrogen oxide pollution in the atmosphere has been receiving much attention, and is considered to be one of important causes of environmental problems such as photochemical smog, greenhouse effect, haze, ozone depletion and the like. With the rapid development of national economy, the consumption of fossil fuels in China is rising year by year, and the problem of accompanying explosive increase of nitrogen oxide emission needs to be solved by a new removal method. The technology of Catalytic Oxidation of nitric oxide (NOCO) assisted by absorption and removal of alkali liquor draws more and more attention due to low price, greenness and lasting conversion efficiency, and provides support for developing a new denitration technology.
The NOCO is based on the principle that low-concentration NO stably existing in flue gas is catalytically oxidized into nitrogen dioxide (NO) by utilizing catalytic media such as metal oxide, molecular sieve, porous carbon material and the like 2 ) Thereafter, the water-insoluble NO is reacted with NO 2 After combination, N which is easy to dissolve in water can be generated 2 O 3 Thereby being removed. The core of this technology is the development of efficient and inexpensive catalysts. Of the many catalytic materials available for NOCOOsCompared with metal oxides, molecular sieve catalysts and high-end carbon materials, the carbon material has good application prospect due to simple manufacturing process, relatively low cost and good catalytic activity under low temperature. However, activated carbon is extremely susceptible to poisoning by sulfur-containing fumes, so that the activity of NOCO is lost, and therefore, the activated carbon needs to be modified to improve the sulfur resistance of the activated carbon. The existing research on improving the sulfur resistance of the activated carbon in the NOCO process is very limited, and no reference solution is available at present.
Disclosure of Invention
The invention aims to overcome the defect that the existing catalyst is easy to inactivate due to sulfur-containing gas in the NOCO process, and provides a catalyst with sulfur resistance for catalytic oxidation of NO, wherein the sulfur resistance is improved by 25-300% compared with that of unmodified activated carbon.
The invention also provides a preparation method of the catalyst for catalyzing and oxidizing NO with sulfur resistance, and the technological process can be briefly described as follows: firstly, ultrasonically dipping vacuum-dried activated carbon in a boric acid solution, and then carrying out rotary evaporation on the boric acid solution and the activated carbon to realize uniform distribution of boric acid solids on the surface and pore channels of the activated carbon; and (3) carrying out high-temperature calcination on the solid obtained after rotary evaporation in a nitrogen atmosphere to prepare the boron-doped modified activated carbon which has good sulfur resistance under low-temperature catalytic oxidation of NO.
The present invention also provides a catalyst for catalytic oxidation of NO having sulfur resistance, in which a boron (B) atom has a lower electronegativity than a carbon (C) atom, and thus a C active site pair polar substance such as SO is reduced to be bonded thereto 2 The binding ability of the compound can be used for doping the activated carbon so as to improve the sulfur resistance of the activated carbon at low temperature NOCO.
The research of the inventor shows that the main causes of the poisoning of the activated carbon under the action of sulfur-containing flue gas mainly include the destruction of catalytic active sites and the blockage of nano-pores. The NO is combined with the catalytic sites on the surface of the carbon and concentrated by the nanometer pore channels when in the activated carbon, so that the surface dispersity and the local concentration in the pore channels are respectively improved, and the NO is converted into the NO in the forms of surface catalytic oxidation and gas-phase direct oxidation 2 . Due to SO 2 The polarity of the molecule is higher than NO 2 Polarity of molecules, SO when the flue gas contains SO 2 In the process, the active sites on the surface of the carbon are combined preferentially, and the carbon is difficult to desorb at normal temperature, so that the active sites are occupied and nanopores are blocked, and the NOCO cannot be carried out continuously.
Catalytic materials for NOCOs have a higher degree of surface oxidation and a specific nanoporous distribution than conventional materials that adsorb organic gases. Due to NO 2 The catalytic material is more active than NO and is easily combined with the defects and reducing groups on the surface of the activated carbon, so that the catalytic material shows a higher surface oxidation state. In order to provide the activated carbon with better initial catalytic effect and reaction stability, the oxidizing groups on the surface of the activated carbon need to be increased in the preparation process. Research of the inventor shows that micropores of 0.6-0.7 nm in the activated carbon have excellent NOCO activity, and the performance of the catalytic material can be remarkably improved through a corresponding pore channel adjusting process.
The catalyst prepared by the invention is different from an SCR denitration catalyst, ammonia gas is not used, the working temperature is room temperature, and partial NO is catalytically oxidized into NO by using the existing oxygen in flue gas as an oxidant 2 Therefore, the method removes the nitrogen oxides through the alkaline solution, achieves the purposes of environmental protection, energy conservation and economy, and is beneficial to providing a new implementation form for the research and development of the denitration catalyst.
In the catalyst for catalytic oxidation of NO with the sulfur resistance, the mass content of boron is 0.01-2%, the doping amount is less than 0.01%, and the improvement of the sulfur resistance is not obvious; the mass content of boron higher than 2% leads to a significant reduction in the initial activity of the catalyst, which is not favorable for improving the overall performance thereof.
In the preparation method provided by the invention, the specific surface area is selected as the raw material>800m 2 The catalyst can normally work under the condition of high airspeed, and smoke is prevented from being blocked by overlarge pressure.
The ultrasonic soaking method is adopted to achieve the purpose that boric acid solution fully soaks the activated carbon, so that uneven distribution of borate ions on the surface and in pore channels of the activated carbon caused by capillary effect is avoided, and compared with conventional mixed soaking, the ultrasonic soaking method has the advantages of good soaking effect and high speed.
The rotary evaporation is a key step in the preparation of the invention, and because B atoms are difficult to be uniformly distributed on an active surface and a pore channel, the catalytic performance of the catalyst is unstable. By adopting a rotary evaporation technology, boric acid is more fully diffused at 70-90 ℃ and gradually enters doping sites, so that the effect of uniformly distributing boric acid particles on the surface of the activated carbon and in pore channels is realized.
The calcining temperature in the calcining step is 800-1200 ℃, and the effective realization of the B atoms from H 3 BO 3 Migration into the C-skeleton. The preferred calcination temperature is 1200 ℃. The calcining atmosphere is inert gas environment such as nitrogen, argon and the like.
The specific scheme is as follows:
the catalyst for catalytic oxidation of NO with sulfur resistance is boric acid modified active carbon, wherein the mass content of boron is 0.01-2%.
Further, the catalyst for catalytic oxidation of NO with sulfur resistance is obtained by mixing an aqueous solution of boric acid and activated carbon powder, performing rotary evaporation and calcination in a nitrogen atmosphere, and then cooling.
Further, the preparation method of the catalyst for catalyzing and oxidizing NO with the sulfur resistance performance comprises the following steps:
step 1: vacuum drying the activated carbon powder;
step 2: adding the activated carbon powder after vacuum drying into a boric acid aqueous solution for ultrasonic impregnation to obtain a mixture;
and step 3: carrying out rotary evaporation on the mixture obtained in the step 2 to obtain activated carbon with uniform boric acid particles distributed on the surface and in the pore channels;
and 4, step 4: calcining the product obtained in the step 3 in a nitrogen atmosphere;
and 5: and (4) cooling the calcined product in the step (4) to room temperature in a nitrogen atmosphere to obtain the catalyst for catalytic oxidation of NO with sulfur resistance.
The application of the catalyst with the sulfur resistance for catalyzing and oxidizing NO is used for catalyzing and oxidizing NO at room temperature to 70 ℃.
Further, compared with unmodified activated carbon, the sulfur resistance of the catalyst for catalytic oxidation of NO with the sulfur resistance at room temperature is improved by 25-300%.
A preparation method of the catalyst with the sulfur-resistant performance for catalyzing and oxidizing NO comprises the following steps:
step 1: vacuum drying the activated carbon powder;
step 2: adding the activated carbon powder after vacuum drying into a boric acid aqueous solution for ultrasonic impregnation to obtain a mixture;
and step 3: carrying out rotary evaporation on the mixture obtained in the step 2 to obtain activated carbon with uniform boric acid particles distributed on the surface and in the pore channels;
and 4, step 4: calcining the product obtained in the step 3 in a nitrogen atmosphere;
and 5: and (4) cooling the calcined product in the step (4) to room temperature in a nitrogen atmosphere to obtain the catalyst for catalytic oxidation of NO with sulfur resistance.
Further, in the step 1, the activated carbon powder is at least one of wood activated carbon powder, coal activated carbon powder or coconut shell activated carbon powder, and the specific surface area of the activated carbon powder is more than 800m 2 The mesh number is 20-80 meshes; the temperature of vacuum drying is 60-110 ℃, the time is 8-12 h, and the vacuum degree is-0.4-0.8 MPa.
Further, the mass concentration of the aqueous solution of boric acid in the step 2 is 0.020-2.0 wt.%; the ultrasonic power is 400-1000W, the dipping time is 10-50 min, and the dipping method is an isometric dipping method.
Further, the rotary evaporation temperature in the step 3 is 70-90 ℃, the time is 1-2 h, and the vacuum degree is-0.01 to-0.2 MPa.
Further, in the step 4, the purity of nitrogen is more than 99.99 vol.%, the flow rate is 0.01-0.1L/min, the calcining temperature is 800-1200 ℃, the calcining time is 1-2 h, and the heating rate during calcining is 5-20 ℃/min;
optionally, in the step 5, the purity of the nitrogen is more than 99.99 vol.%, the flow rate is 0.01-0.1L/min, and the cooling rate during cooling is 5-20 ℃/min.
Has the advantages that:
the preparation method disclosed by the invention is simple in process flow, simple and convenient to operate, low in cost and easy for mass production; the required raw materials are clean and environment-friendly, have no harmful substances, do not generate secondary pollution, and accord with the concept of green chemistry; the prepared modified activated carbon has good sulfur resistance when being used for NOCO, and the activation time is extended by 25-300% compared with that before modification.
Drawings
In order to illustrate the technical solution of the present invention more clearly, the drawings will be briefly described below, and it is apparent that the drawings in the following description relate only to some embodiments of the present invention and are not intended to limit the present invention.
FIG. 1 shows a catalyst prepared by the method of the present invention in the presence of SO 2 Deactivation curve of catalytic oxidation NO under conditions.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. In the following examples, "%" means weight percent, unless otherwise specified.
Example 1
The specific surface area is 1200m 2 And putting the coconut shell activated carbon with the granularity of 40-60 meshes in a vacuum drying oven, drying for 12 hours at the temperature of 80 ℃ under the vacuum degree of-0.6 MPa, and marking as a sample AC.
Taking 5g of sample AC, placing the sample AC in a porcelain boat, moving the sample AC into a tube furnace, and introducing 50mL of N 2 (99.99 vol.%), heating to 800 deg.C at 5 deg.C/min, and calcining for 2 hr; then the temperature is reduced to room temperature at the speed of 5 ℃/min, and a sample is taken and recorded as AC-800 ℃.
Respectively carrying out room-temperature catalytic oxidation NO test on a sample AC and a sample AC-800 ℃ in sulfur-containing flue gas, wherein the method comprises the following steps: a0.300 g sample was charged into a quartz reaction tube having an inner diameter of 1cm, and 800ppm NO and 20 vol.% O were introduced thereinto at room temperature 2 、N 2 (99.99 vol.%) balanced gas mixture, space velocity 120000h -1 . Measuring NO and NO every 2h 2 The concentration of (c); after stabilization, 50ppm SO is introduced 2 Keeping the assay until NO 2 The concentration is lower than the initial concentration in the mixed gas, and the activity time of the catalyst in the sulfur-containing flue gas is recorded, as shown in figure 1. The vertical axis in the figure represents the relative activity of the catalyst, activity at time t of the catalyst/initial activity of the catalyst 100%, wherein the activity at time t of the catalyst η can be calculated according to equation (1):
wherein, C (NO) 0 -the concentration of NO in the flue gas at the initial moment, ppm; c (NO) 2 ) 0 -the concentration of NO in the flue gas at the initial moment, ppm; c (NO) t -the concentration of NO in the flue gas at the initial moment, ppm; c (NO) 2 ) t -concentration of NO in flue gas at initial time, ppm.
The performance of the sample AC is similar to that of the sample AC-800 ℃ in the catalytic oxidation of NO at room temperature in the sulfur-containing flue gas, which shows that the activated carbon is very easy to inactivate in the sulfur-containing flue gas, so that the effect of the catalytic oxidation of NO is difficult to exert for a long time; while the drying and high-temperature calcination can not change the chemical property of the catalytic active sites on the surface of the activated carbon, SO 2 Can quickly occupy active sites and block nano-pore channels, so that the sulfur resistance of the catalyst is not improved.
Example 2
The specific surface area is 1200m 2 And putting the coconut shell activated carbon with the granularity of 40-60 meshes in a vacuum drying oven, and drying for 12 hours at the temperature of 80 ℃ and the vacuum degree of-0.6 MPa. 5.00g of dried activated carbon was placed in a flask and 200mL of 0.15 wt.% H was added 3 BO 3 And (4) uniformly mixing the solution. The flask was placed in an ultrasonic cleaner at a power of 1000W and a temperature of 30 deg.CSubjecting to ultrasonic oscillation for 30min, introducing into rotary evaporator, evaporating and drying in water bath at 80 deg.C and vacuum degree of-0.01 MPa to obtain surface and pore canal with uniformly distributed H 3 BO 3 The activated carbon is placed in a porcelain boat and moved into a tube furnace, and 50mL of N is introduced 2 (99.99 vol.%), heating to 800 ℃ at a rate of 5 ℃/min, and calcining for 2 h; then cooling to room temperature at the speed of 5 ℃/min, and taking out to obtain the B-doped active carbon BAC1-800 ℃.
The prepared catalyst BAC1-800 deg.C, 0.300g is filled into a quartz reaction tube with an inner diameter of 1cm, and 800ppm NO and 20 vol.% O are introduced at room temperature 2 、N 2 (99.99 vol.%) balanced gas mixture, space velocity 120000h -1 . Measuring NO and NO every 2h 2 The concentration of (c); after stabilization, 50ppm SO is introduced 2 Keeping the assay until NO 2 The concentration is lower than the initial concentration in the gas mixture. The catalyst activity time in sulfur-containing flue gas was recorded at 10h, which is 25% longer than 8h before modification, as shown in fig. 1.
Example 3
Keeping the other conditions in example 1 unchanged, adding H 3 BO 3 The concentration of the solution was changed to 0.30 wt.%, and the prepared catalyst BAC 2% -800 ℃ was evaluated under the same test conditions as in example 1. The activity time of the catalyst in sulfur-containing flue gas is 20h, and is prolonged by 150% compared with that before modification as shown in figure 1.
Example 4
The catalyst prepared with the calcination temperature changed to 1000 ℃ was evaluated at 2-1000 ℃ under the same test conditions as in example 1, while keeping the other conditions in example 2 unchanged. The activity time of the catalyst in sulfur-containing flue gas is 28h, and is prolonged by 250% compared with that before modification as shown in figure 1.
Example 5
The calcination temperature was changed to 1200 ℃ keeping the other conditions in example 2, and the prepared catalyst BAC2-1200 ℃ was evaluated under the same test conditions as in example 1. The activity time of the catalyst in sulfur-containing flue gas is 32h, and is prolonged by 300% compared with that before modification as shown in figure 1.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (9)
1. A catalyst having sulfur resistance for the catalytic oxidation of NO, characterized by: the catalyst for sulfur-resistant catalytic oxidation of NO is boric acid modified activated carbon, wherein the mass content of boron is 0.01-2%;
the preparation method of the catalyst with the sulfur resistance for catalyzing and oxidizing NO comprises the following steps:
step 1: vacuum drying the activated carbon powder;
step 2: adding the activated carbon powder after vacuum drying into a boric acid aqueous solution for ultrasonic impregnation to obtain a mixture;
and step 3: carrying out rotary evaporation on the mixture obtained in the step 2 to obtain activated carbon with uniform boric acid particles distributed on the surface and in the pore channels; the temperature of rotary evaporation is 70-90 ℃;
and 4, step 4: calcining the product obtained in the step 3 in a nitrogen atmosphere, wherein the calcining temperature is 800-1200 ℃;
and 5: cooling the calcined product in the step 4 to room temperature in a nitrogen atmosphere to obtain a catalyst with sulfur resistance for catalytic oxidation of NO;
compared with unmodified activated carbon, the sulfur resistance of the catalyst for catalytic oxidation of NO with the sulfur resistance is improved by 25-300%.
2. A catalyst for the catalytic oxidation of NO with sulphur resistance according to claim 1, characterized in that: the catalyst for catalytic oxidation of NO with sulfur resistance is obtained by mixing a boric acid aqueous solution and activated carbon powder, then carrying out rotary evaporation and calcination in a nitrogen atmosphere, and then cooling.
3. Use of a catalyst for the catalytic oxidation of NO with sulphur resistance as defined in claim 1 or 2 for the catalytic oxidation of NO at room temperature to 70 ℃.
4. Use of a catalyst for the catalytic oxidation of NO with sulphur resistance according to claim 3, characterized in that: compared with unmodified activated carbon, the catalyst for catalytic oxidation of NO with sulfur resistance at room temperature has the sulfur resistance improved by 25-300%.
5. A process for the preparation of a catalyst for the catalytic oxidation of NO with sulphur resistance as claimed in claim 1 or 2, characterized in that: the method comprises the following steps:
step 1: vacuum drying the activated carbon powder;
step 2: adding the activated carbon powder after vacuum drying into a boric acid aqueous solution for ultrasonic impregnation to obtain a mixture;
and step 3: carrying out rotary evaporation on the mixture obtained in the step 2 to obtain the activated carbon with uniform boric acid particles distributed on the surface and in the pore canal;
and 4, step 4: calcining the product obtained in the step 3 in a nitrogen atmosphere;
and 5: and (4) cooling the calcined product in the step (4) to room temperature in a nitrogen atmosphere to obtain the catalyst for catalytic oxidation of NO with sulfur resistance.
6. The method of claim 5 for preparing a catalyst for the catalytic oxidation of NO with sulfur resistance, wherein: the activated carbon powder in step 1Is at least one of wood activated carbon powder, coal activated carbon powder or coconut shell activated carbon powder, and has a specific surface area of more than 800m 2 The mesh number is 20-80 meshes; the temperature of vacuum drying is 60-110 ℃, the time is 8-12 h, and the vacuum degree is-0.4-0.8 MPa.
7. The method of claim 5 for preparing a catalyst for the catalytic oxidation of NO with sulfur resistance, wherein: the mass concentration of the aqueous solution of boric acid in the step 2 is 0.020-2.0 wt.%; the ultrasonic power is 400-1000W, the dipping time is 10-50 min, and the dipping method is an isometric dipping method.
8. The method of claim 5 for preparing a catalyst for the catalytic oxidation of NO with sulfur resistance, wherein: the time of rotary evaporation in the step 3 is 1-2 h, and the vacuum degree is-0.01-0.2 MPa.
9. The method of claim 5 for preparing a catalyst for the catalytic oxidation of NO with sulfur resistance, wherein: in the step 4, the purity of nitrogen is more than 99.99 vol.%, the flow rate is 0.01-0.1L/min, the calcining temperature is 800-1200 ℃, the calcining time is 1-2 h, and the heating rate during calcining is 5-20 ℃/min;
optionally, in the step 5, the purity of the nitrogen is more than 99.99 vol.%, the flow rate is 0.01-0.1L/min, and the cooling rate during cooling is 5-20 ℃/min.
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