CN108658056B - Preparation method of biochar with good electrical property - Google Patents
Preparation method of biochar with good electrical property Download PDFInfo
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- CN108658056B CN108658056B CN201810505223.1A CN201810505223A CN108658056B CN 108658056 B CN108658056 B CN 108658056B CN 201810505223 A CN201810505223 A CN 201810505223A CN 108658056 B CN108658056 B CN 108658056B
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Abstract
The invention discloses a preparation method of biochar with good electrical property, which comprises the following steps: (1) the method comprises the following steps of (1) cooking treatment, (2) oxidation soaking treatment, (3) steam explosion treatment, (4) activation treatment, (5) modification treatment and (6) carbonization treatment. The invention provides a preparation method of biochar, which has standard integral process and is convenient for batch production, the prepared biochar has excellent electrical property, the discharge capacity and the cycle stability are obviously improved, the quality of the biochar serving as a lithium battery cathode material is enhanced, and the biochar has high market competitiveness and popularization and application values.
Description
Technical Field
The invention belongs to the technical field of biological carbon processing, and particularly relates to a preparation method of biological carbon with good electrical property.
Background
The crop straw is a general term of the stem and leaf parts of the mature crops. Generally refers to the remainder of wheat, rice, corn, potatoes, oilseed rape, cotton, sugar cane and other crops after harvesting the seeds. More than half of the products of crop photosynthesis exist in the straws, and the straws are rich in carbon, nitrogen, phosphorus, potassium, calcium, magnesium, organic matters and the like, and are a multipurpose renewable biological resource. A part of crop straws are used for manufacturing biochar.
With the rapid development of social economy, the dependence of human society on energy is continuously improved. However, the excessive development of human beings causes energy exhaustion and serious environmental pollution. In order to solve the current energy problem, people aim at renewable clean energy. However, they also have their own limitations, such as large total volume, randomness, low energy density, etc., which make them difficult to use. Therefore, high-efficiency energy storage technology becomes a research hotspot.
The rechargeable battery system mainly comprising lead-acid batteries, nickel-cadmium batteries and lithium ion batteries is an important member of the large-capacity electrochemical energy storage technology, and the lead-acid batteries and the nickel-cadmium batteries which have low energy density and seriously pollute the environment are bound to gradually exit the historical stage. In contrast, outstanding as a new energy storage technology, the lithium ion battery has the advantages of open circuit voltage, high specific energy, excellent safety performance, environmental friendliness and the like, and the excellent performance of the lithium ion battery must also replace lead-acid batteries and nickel-cadmium batteries. In addition, the lithium ion battery has low price and high safety performance, and is a green battery with great potential. In recent years, lithium ion batteries have been widely used in electric vehicles and the like.
The negative electrode material is one of the cores of the lithium ion battery, and the most widely researched negative electrode materials of the lithium ion battery at present mainly comprise two types, one is a carbon-based negative electrode material, such as graphite; one class is non-carbon based anode materials such as tin based anode materials and transition metal oxides (sulfides). The biochar belongs to a carbon-based negative electrode material, and in recent years, another heat tide in the field of energy storage materials is brought up by research on biochar materials. The biochar has unique physicochemical properties, and has the advantages of rich resources, low price, renewability, environmental friendliness and the like, so that the biochar becomes a very good material with great development potential in non-graphitized carbon materials, and has attracted the wide interest of researchers. However, the biochar material prepared by the prior art mostly has the problems of poor and unstable electrical property and the like, and needs to be improved.
Disclosure of Invention
The invention aims to provide a preparation method of biochar with good electrical property aiming at the existing problems.
The invention is realized by the following technical scheme:
a preparation method of biochar with good electrical property comprises the following steps:
(1) and (3) cooking treatment:
putting crop straws into a sodium hydroxide solution, heating to boil, boiling for 20-30 min, and taking out the crop straws for later use;
(2) oxidation soaking treatment:
soaking the crop straws treated in the step (1) in a hydrogen peroxide solution with the volume fraction of 20-25% for 4-6 h, taking out, washing with deionized water to be neutral for later use;
(3) and (3) steam explosion treatment:
putting the crop straws treated in the step (2) into a steam explosion tank for steam explosion treatment, taking out the crop straws after the steam explosion treatment is finished, drying and crushing the crop straws, and sieving the crop straws with 100 meshes to obtain crop straw powder for later use;
(4) activation treatment:
putting the crop straw powder obtained in the step (3) into a tartaric acid solution, soaking for 5-7 min, taking out, washing with deionized water to be neutral, and drying for later use;
(5) modification treatment:
a. introducing argon into a reaction kettle, mixing methyltriethoxysilane and diisopropanolamine according to the weight ratio of 1: 2-2.4, heating to keep the temperature in the reaction kettle at 118-124 ℃, stirring for reaction for 5-7 hours, and then performing suction filtration, reduced pressure and distillation treatment to obtain a mixture A for later use; reacting chlorine atoms in methyltriethoxysilane with amino groups in diisopropanolamine to prepare a mixture A which is modified silane;
b. introducing argon into the reaction kettle, and then mixing the mixture A prepared in the operation a with anhydrous methanol, R-epichlorohydrin, disodium ethylene diamine tetraacetate, sodium cellulose, sodium molybdate and staurous chloride powder according to the weight ratio of 6-8: 65-70: 5-7: 0.15-0.25: 0.2-0.5: 2-4: 7-9, heating to keep the temperature in the reaction kettle at 44-50 ℃, stirring for reaction for 2-3 hours, and taking out to obtain a mixture B for later use; the mixture A and the component R-epichlorohydrin are subjected to quaternization reaction to generate quaternary ammonium salt, and then are compositely grafted on the surface of the yellow tin ore powder with sodium cellulose and sodium molybdate under the action of disodium ethylene diamine tetraacetate, so that the surface group type and content of the yellow tin ore powder are improved, and the Li is enhanced+The embedding fixing effect of (1);
c. performing rotary evaporation, elution treatment and vacuum drying on the mixture B prepared in the operation B to obtain a material C for later use;
d. mixing the material C obtained in the operation C with a dispersing agent and deionized water according to a weight ratio of 10-14: 3-6: 90-100, then soaking the crop straw powder treated in the step (4) into the solution, and filtering out the crop straw powder for later use after carrying out ultrasonic treatment for 2-3 h;
e. putting the crop straw powder obtained in the operation d into a drying oven for drying treatment for later use;
(6) carbonizing treatment:
and (3) putting the crop straw powder treated in the step (5) into carbonization equipment for carbonization, taking nitrogen as a protective environment, controlling the carbonization temperature to be 520-580 ℃, preserving heat, carbonizing for 2-2.5 h, and taking out. The modified components can be stably fixed in the biochar to optimize the interlayer structure of the biochar by carbonizing after the modification treatment, and the electrical property and quality of the surface of the biochar can be influenced and the overall stability is damaged if the modification treatment is carried out after the carbonization treatment.
Further, the mass fraction of sodium hydroxide in the sodium hydroxide solution in the step (1) is 8-12%.
Further, the steam explosion treatment operation in the step (3) is specifically to introduce water vapor with the temperature of 103-108 ℃ into the steam explosion tank, increase the pressure in the steam explosion tank to 0.5-0.6 MPa, perform heat preservation and pressure maintaining treatment for 20-24 min, unload the steam explosion tank to normal temperature and normal pressure within 2min, and finally take out the crop straws.
Further, the tartaric acid solution in the step (4) contains 3-5% by mass of tartaric acid.
Further, the particle size of the yellow tin ore powder in the operation b of the step (5) is 0.1-1 μm.
Further, the elution treatment in the operation c of the step (5) is an elution treatment using anhydrous ethyl ether.
Further, the dispersant in the operation d of the step (5) is a low molecular wax dispersant, and the frequency of ultrasonic wave during ultrasonic treatment is 300-350 kHz.
Further, in the drying treatment in the operation e in the step (5), the temperature in the drying oven is controlled to be 75-80 ℃.
The invention improves the preparation method of the biological carbon, well utilizes the crop straw waste, and the prepared biological carbon has good electrical property and can be used as a negative electrode material of a lithium battery. In the preparation process, alkali liquor cooking and oxidation soaking treatment are firstly carried out, so that components which are not beneficial to carbonization in the straws are removed, the carbonization rate and the material utilization rate are favorably improved, then steam explosion treatment is carried out, the tissue structure of the crop straws is effectively loosened, the fiber gaps and the specific surface area are improved, a foundation is laid for subsequent treatment, then tartaric acid solution soaking treatment is carried out, the tissue gaps are further enlarged by using acid liquor, the further refinement of fine fibers is promoted, the specific surface area is improved, and the surface characteristics are activated; then, modification treatment is carried out, and a specially treated composite component material C which takes the cassiterite powder particles as the main body is infiltrated and fixed into the crop straw powder fibers, so that the specific surface area of the whole biological carbon can be increased, the exchange adsorption capacity of the subsequent biological carbon is enhanced, and the interlaminar biological carbon can be enlargedSpacing for more Li+While the large number of active groups contained in the intercalation compound can also promote Li+The embedding, fixing and releasing of the organic carbon composite material improve the discharge capacity and the cycling stability together, and enhance the electrical property of the biological carbon; finally, carbonization treatment is carried out, so that the components are effectively stabilized in the biochar, and the overall use stability and quality are improved.
Compared with the prior art, the invention has the following advantages:
the invention provides a preparation method of biochar, which has standard integral process and is convenient for batch production, the prepared biochar has excellent electrical property, the discharge capacity and the cycle stability are obviously improved, the quality of the biochar serving as a lithium battery cathode material is enhanced, and the biochar has high market competitiveness and popularization and application values.
Detailed Description
Example 1
A preparation method of biochar with good electrical property comprises the following steps:
(1) and (3) cooking treatment:
putting crop straws into a sodium hydroxide solution, heating to boil, boiling for 20min, and taking out the crop straws for later use;
(2) oxidation soaking treatment:
soaking the crop straws treated in the step (1) in a hydrogen peroxide solution with the volume fraction of 20% for 4h, taking out, washing with deionized water to be neutral for later use;
(3) and (3) steam explosion treatment:
putting the crop straws treated in the step (2) into a steam explosion tank for steam explosion treatment, taking out the crop straws after the steam explosion treatment is finished, drying and crushing the crop straws, and sieving the crop straws with 100 meshes to obtain crop straw powder for later use;
(4) activation treatment:
putting the crop straw powder obtained in the step (3) into a tartaric acid solution, soaking for 5min, taking out, washing to be neutral by deionized water, and drying for later use;
(5) modification treatment:
a. introducing argon into a reaction kettle, mixing methyltriethoxysilane and diisopropanolamine according to the weight ratio of 1:2, heating to keep the temperature in the reaction kettle at 118 ℃, carrying out suction filtration, pressure reduction and distillation after stirring reaction for 5 hours, and obtaining a mixture A for later use;
b. introducing argon into the reaction kettle, and mixing the mixture A prepared in the operation a with anhydrous methanol, R-epichlorohydrin, ethylene diamine tetraacetic acid disodium, sodium cellulose, sodium molybdate and staurous chloride powder according to the weight ratio of 6:65:5: 0.15: 0.2: 2: 7, mixing, heating to keep the temperature in the reaction kettle at 44 ℃, stirring for reaction for 2 hours, and taking out to obtain a mixture B for later use;
c. performing rotary evaporation, elution treatment and vacuum drying on the mixture B prepared in the operation B to obtain a material C for later use;
d. mixing the material C obtained in the operation C with a dispersing agent and deionized water according to a weight ratio of 10:3:90, then soaking the crop straw powder treated in the step (4) into the solution, and filtering out the crop straw powder for later use after 2 hours of ultrasonic treatment;
e. putting the crop straw powder obtained in the operation d into a drying oven for drying treatment for later use;
(6) carbonizing treatment:
and (3) putting the crop straw powder treated in the step (5) into carbonization equipment for carbonization, taking nitrogen as a protective environment, controlling the carbonization temperature to be 520 ℃, preserving heat, carbonizing for 2 hours, and taking out.
Further, the mass fraction of sodium hydroxide in the sodium hydroxide solution in the step (1) is 8%.
Further, the steam explosion treatment operation in the step (3) is specifically to introduce water vapor with the temperature of 103 ℃ into the steam explosion tank, increase the pressure in the steam explosion tank to 0.5MPa, perform heat preservation and pressure maintaining treatment for 20min, unload the steam explosion tank to normal temperature and normal pressure within 2min, and finally take out the crop straws.
Further, the tartaric acid solution in the step (4) has a tartaric acid mass fraction of 3%.
Further, the particle size of the yellow tin ore powder in the operation b of the step (5) is 0.1-1 μm.
Further, the elution treatment in the operation c of the step (5) is an elution treatment using anhydrous ethyl ether.
Further, the dispersant in the operation d of the step (5) is a low molecular wax dispersant, and the frequency of the ultrasonic wave during the ultrasonic treatment is 300 kHz.
Further, the temperature in the drying oven was controlled to 75 ℃ during the drying process described in operation e of step (5).
Example 2
A preparation method of biochar with good electrical property comprises the following steps:
(1) and (3) cooking treatment:
putting crop straws into a sodium hydroxide solution, heating to boil, boiling for 25min, and taking out the crop straws for later use;
(2) oxidation soaking treatment:
soaking the crop straws treated in the step (1) in a hydrogen peroxide solution with the volume fraction of 23% for 5 hours, taking out, washing with deionized water to be neutral for later use;
(3) and (3) steam explosion treatment:
putting the crop straws treated in the step (2) into a steam explosion tank for steam explosion treatment, taking out the crop straws after the steam explosion treatment is finished, drying and crushing the crop straws, and sieving the crop straws with 100 meshes to obtain crop straw powder for later use;
(4) activation treatment:
putting the crop straw powder obtained in the step (3) into a tartaric acid solution, soaking for 6min, taking out, washing with deionized water to be neutral, and drying for later use;
(5) modification treatment:
a. introducing argon into a reaction kettle, mixing methyltriethoxysilane and diisopropanolamine according to the weight ratio of 1:2.2, heating to keep the temperature in the reaction kettle at 120 ℃, stirring for reaction for 6 hours, and then performing suction filtration, reduced pressure and distillation treatment to obtain a mixture A for later use;
b. introducing argon into the reaction kettle, and mixing the mixture A prepared in the operation a with anhydrous methanol, R-epichlorohydrin, ethylene diamine tetraacetic acid disodium, sodium cellulose, sodium molybdate and staurous chloride powder according to a weight ratio of 7:68:6: 0.2: 0.4: 3: 8, mixing, heating to keep the temperature in the reaction kettle at 46 ℃, stirring for reaction for 2.5 hours, and taking out to obtain a mixture B for later use;
c. performing rotary evaporation, elution treatment and vacuum drying on the mixture B prepared in the operation B to obtain a material C for later use;
d. mixing the material C obtained in the operation C with a dispersing agent and deionized water according to the weight ratio of 12:5:96, then soaking the crop straw powder treated in the step (4) into the solution, and filtering out the crop straw powder for later use after ultrasonic treatment for 2.5 hours;
e. putting the crop straw powder obtained in the operation d into a drying oven for drying treatment for later use;
(6) carbonizing treatment:
and (3) putting the crop straw powder treated in the step (5) into carbonization equipment for carbonization, taking nitrogen as a protective environment, controlling the carbonization temperature to be 560 ℃, preserving heat, carbonizing for 2.3h, and taking out.
Further, the mass fraction of sodium hydroxide in the sodium hydroxide solution in the step (1) is 10%.
Further, the steam explosion treatment operation in the step (3) is specifically to introduce water vapor with the temperature of 105 ℃ into the steam explosion tank, increase the pressure in the steam explosion tank to 0.55MPa, perform heat preservation and pressure maintaining treatment for 22min, unload the steam explosion tank to normal temperature and normal pressure within 2min, and finally take out the crop straws.
Further, the tartaric acid solution in the step (4) has a tartaric acid content of 4% by mass.
Further, the particle size of the yellow tin ore powder in the operation b of the step (5) is 0.1-1 μm.
Further, the elution treatment in the operation c of the step (5) is an elution treatment using anhydrous ethyl ether.
Further, the dispersant in the operation d of the step (5) is a low molecular wax dispersant, and the frequency of the ultrasonic wave during the ultrasonic treatment is 330 kHz.
Further, the temperature in the drying oven was controlled to 78 ℃ during the drying process described in operation e of step (5).
Example 3
A preparation method of biochar with good electrical property comprises the following steps:
(1) and (3) cooking treatment:
putting crop straws into a sodium hydroxide solution, heating to boil, boiling for 30min, and taking out the crop straws for later use;
(2) oxidation soaking treatment:
soaking the crop straws treated in the step (1) in a hydrogen peroxide solution with the volume fraction of 25% for 6 hours, taking out, washing with deionized water to be neutral for later use;
(3) and (3) steam explosion treatment:
putting the crop straws treated in the step (2) into a steam explosion tank for steam explosion treatment, taking out the crop straws after the steam explosion treatment is finished, drying and crushing the crop straws, and sieving the crop straws with 100 meshes to obtain crop straw powder for later use;
(4) activation treatment:
putting the crop straw powder obtained in the step (3) into a tartaric acid solution, soaking for 7min, taking out, washing with deionized water to be neutral, and drying for later use;
(5) modification treatment:
a. introducing argon into a reaction kettle, mixing methyltriethoxysilane and diisopropanolamine according to the weight ratio of 1:2.4, heating to keep the temperature in the reaction kettle at 124 ℃, carrying out suction filtration, pressure reduction and distillation treatment after stirring reaction treatment for 7 hours, and obtaining a mixture A for later use;
b. introducing argon into the reaction kettle, and mixing the mixture A prepared in the operation a with anhydrous methanol, R-epichlorohydrin, ethylene diamine tetraacetic acid disodium, sodium cellulose, sodium molybdate and staurous chloride powder according to a weight ratio of 8: 70: 7: 0.25: 0.5: 4: 9, mixing, heating to keep the temperature in the reaction kettle at 50 ℃, stirring for reaction for 3 hours, and taking out to obtain a mixture B for later use;
c. performing rotary evaporation, elution treatment and vacuum drying on the mixture B prepared in the operation B to obtain a material C for later use;
d. mixing the material C obtained in the operation C with a dispersing agent and deionized water according to a weight ratio of 14:6:100, then soaking the crop straw powder treated in the step (4) into the solution, and filtering out the crop straw powder for later use after ultrasonic treatment for 3 hours;
e. putting the crop straw powder obtained in the operation d into a drying oven for drying treatment for later use;
(6) carbonizing treatment:
and (3) putting the crop straw powder treated in the step (5) into carbonization equipment for carbonization, taking nitrogen as a protective environment, controlling the carbonization temperature to be 580 ℃, preserving heat, carbonizing for 2.5h, and taking out.
Further, the mass fraction of sodium hydroxide in the sodium hydroxide solution in the step (1) is 12%.
Further, the steam explosion treatment operation in the step (3) is specifically to introduce water vapor with the temperature of 108 ℃ into the steam explosion tank, increase the pressure in the steam explosion tank to 0.6MPa, perform heat preservation and pressure maintaining treatment for 24min, unload the steam explosion tank to normal temperature and normal pressure within 2min, and finally take out the crop straws.
Further, the tartaric acid solution in the step (4) has a tartaric acid content of 5% by mass.
Further, the particle size of the yellow tin ore powder in the operation b of the step (5) is 0.1-1 μm.
Further, the elution treatment in the operation c of the step (5) is an elution treatment using anhydrous ethyl ether.
Further, the dispersant in the operation d of the step (5) is a low molecular wax dispersant, and the frequency of ultrasonic wave in the ultrasonic treatment is 350 kHz.
Further, in the drying treatment in operation e of step (5), the temperature in the drying oven was controlled to 80 ℃.
Comparative example 1
In this comparative example 1, compared with example 2, operation a, operation b and operation C in the modification treatment in step (5) were omitted, and the material C component in operation d was replaced with an equal mass part of kesterite powder, except that the other steps of the method were the same.
Comparative example 2
In comparative example 2, the steps of the modification treatment in step (5) and the carbonization treatment in step (6) were changed over to each other, that is, the biocarbon was directly modified by the modification treatment in step (5) in comparison with example 2, except that the other steps were the same.
Control group
The existing crop straw carbonization treatment process.
In order to compare the effects of the invention, the biochar prepared in the embodiment 2, the comparative embodiment 1, the comparative embodiment 2 and the comparative example are processed into the negative electrode material according to the same process, and then the charge and discharge tests are carried out according to the same method, so that the current density of the negative electrode material of the lithium ion battery is controlled to be 100mAhg-1And the voltage range is 0.01-3V, then the electrical property of the cathode material is tested, and the specific comparison data is shown in the following table 1:
TABLE 1
As can be seen from the above table 1, the electrical property and quality of the biochar prepared by the method are obviously improved, the quality and value of the biochar as the lithium ion battery cathode material are enhanced, a treatment scheme with better prospect is provided for the reutilization of crop straws, and the method has good economic benefits.
Claims (8)
1. A preparation method of biochar with good electrical property is characterized by comprising the following steps:
(1) and (3) cooking treatment:
putting crop straws into a sodium hydroxide solution, heating to boil, boiling for 20-30 min, and taking out the crop straws for later use;
(2) oxidation soaking treatment:
soaking the crop straws treated in the step (1) in a hydrogen peroxide solution with the volume fraction of 20-25% for 4-6 h, taking out, washing with deionized water to be neutral for later use;
(3) and (3) steam explosion treatment:
putting the crop straws treated in the step (2) into a steam explosion tank for steam explosion treatment, taking out the crop straws after the steam explosion treatment is finished, drying and crushing the crop straws, and sieving the crop straws with 100 meshes to obtain crop straw powder for later use;
(4) activation treatment:
putting the crop straw powder obtained in the step (3) into a tartaric acid solution, soaking for 5-7 min, taking out, washing with deionized water to be neutral, and drying for later use;
(5) modification treatment:
a. introducing argon into a reaction kettle, mixing methyltriethoxysilane and diisopropanolamine according to the weight ratio of 1: 2-2.4, heating to keep the temperature in the reaction kettle at 118-124 ℃, stirring for reaction for 5-7 hours, and then performing suction filtration, reduced pressure and distillation treatment to obtain a mixture A for later use;
b. introducing argon into the reaction kettle, and then mixing the mixture A prepared in the operation a with anhydrous methanol, R-epichlorohydrin, disodium ethylene diamine tetraacetate, sodium cellulose, sodium molybdate and staurous chloride powder according to the weight ratio of 6-8: 65-70: 5-7: 0.15-0.25: 0.2-0.5: 2-4: 7-9, heating to keep the temperature in the reaction kettle at 44-50 ℃, stirring for reaction for 2-3 hours, and taking out to obtain a mixture B for later use;
c. performing rotary evaporation, elution treatment and vacuum drying on the mixture B prepared in the operation B to obtain a material C for later use;
d. mixing the material C obtained in the operation C with a dispersing agent and deionized water according to a weight ratio of 10-14: 3-6: 90-100, then soaking the crop straw powder treated in the step (4) into the solution, and filtering out the crop straw powder for later use after carrying out ultrasonic treatment for 2-3 h; the dispersant is low molecular wax dispersant;
e. putting the crop straw powder obtained in the operation d into a drying oven for drying treatment for later use;
(6) carbonizing treatment:
and (3) putting the crop straw powder treated in the step (5) into carbonization equipment for carbonization, taking nitrogen as a protective environment, controlling the carbonization temperature to be 520-580 ℃, preserving heat, carbonizing for 2-2.5 h, and taking out.
2. The method for preparing biochar with good electrical properties according to claim 1, wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution in the step (1) is 8-12%.
3. The method for preparing biochar with good electrical properties according to claim 1, wherein the steam explosion treatment in the step (3) is specifically carried out by introducing water vapor with the temperature of 103-108 ℃ into a steam explosion tank, increasing the pressure in the steam explosion tank to 0.5-0.6 MPa, carrying out heat preservation and pressure maintaining treatment for 20-24 min, then unloading the steam explosion tank to normal temperature and normal pressure within 2min, and finally taking out the crop straws.
4. The method for preparing biochar with good electrical properties according to claim 1, wherein the tartaric acid solution in the step (4) contains 3-5% by weight of tartaric acid.
5. The method for preparing biochar with good electrical properties as claimed in claim 1, wherein the particle size of the yellow tin ore powder in the operation b of step (5) is 0.1-1 μm.
6. The method for preparing biochar with good electrical properties as claimed in claim 1, wherein the elution treatment in the step (5), operation c, is performed by using anhydrous ether.
7. The method for preparing biochar with good electrical properties according to claim 1, wherein the ultrasonic frequency during the ultrasonic treatment in the operation d of the step (5) is 300-350 kHz.
8. The method for preparing biochar with good electrical properties according to claim 1, wherein the temperature in the drying oven is controlled to be 75-80 ℃ during the drying treatment in the operation e of the step (5).
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