CN108927148B - Preparation method of high-activity palladium hydroxide carbon - Google Patents
Preparation method of high-activity palladium hydroxide carbon Download PDFInfo
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- NXJCBFBQEVOTOW-UHFFFAOYSA-L palladium(2+);dihydroxide Chemical compound O[Pd]O NXJCBFBQEVOTOW-UHFFFAOYSA-L 0.000 title claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 31
- 230000000694 effects Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006264 debenzylation reaction Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 239000012696 Pd precursors Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 21
- 239000012498 ultrapure water Substances 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 19
- 239000006229 carbon black Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000007598 dipping method Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 238000012805 post-processing Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000009461 vacuum packaging Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- 150000002940 palladium Chemical class 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 3
- 238000011085 pressure filtration Methods 0.000 claims description 3
- 239000003273 ketjen black Substances 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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Abstract
The invention provides a preparation method of high-activity palladium hydroxide carbon for debenzylation, which belongs to the technical field of preparation methods of supported noble metal catalysts and comprises the following steps: conductive carbon black pretreatment, palladium precursor impregnation, palladium hydroxide precipitation and aftertreatment. The preparation method provided by the invention has the advantages of simple process and low cost, and the obtained palladium hydroxide carbon is suitable for a general hydrogenation reaction system, especially a hydrodebenzyl reaction, and has uniform particle size and high activity.
Description
Technical Field
The invention belongs to the technical field of preparation methods of supported noble metal catalysts, and particularly relates to a preparation method of high-activity palladium hydroxide carbon.
Background
The palladium carbon hydroxide has wide application in the fields of medicine organic synthesis and chemical industry, and mainly plays a role in catalytic hydrogenation, including debenzylation, olefin hydrogenation, benzoic acid reduction, aldehyde oxidation and the like. Since the preparation of palladium carbon hydroxide by William m.pearlman in 1967 using an ion exchange method, it has attracted much attention due to its excellent catalytic activity, but the activity of the existing palladium carbon hydroxide is still low.
The invention discloses a palladium-carbon catalyst and a preparation method and application thereof (application number is CN201611205052.8) in the prior patent application, which comprises the following steps: carrying out acid oxidation treatment on the activated carbon raw material; treating the acid-oxidized activated carbon with an alkali metal hydroxide; and taking the treated active carbon as a carrier to prepare the palladium-carbon catalyst. However, the active carbon is treated by using acid solution such as nitric acid in the preparation process, so that the danger is high, and the obtained palladium carbon catalyst has uneven particle size and low activity.
Disclosure of Invention
The invention aims to provide a preparation method of high-activity palladium hydroxide carbon, which has simple process and low cost, and the obtained palladium hydroxide carbon is suitable for a general hydrogenation reaction system, particularly a hydrogenation debenzylation reaction, and has uniform particle size and high activity.
The invention provides the following technical scheme:
a preparation method of high-activity palladium hydroxide carbon comprises the following steps:
s1, conductive carbon black pretreatment: weighing 1-100 parts of conductive carbon black, putting the conductive carbon black into a container, adding 1-100 parts of organic solvent and 1-500 parts of ultrapure water, treating for 10-90 min, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 1-1000 parts of ultrapure water into the carbon black treated in the step S1, then pouring a palladium salt solution, and stirring at the speed of 100-500 rmp for 0.5-5 h;
s3, precipitation of palladium hydroxide: adding an alkali metal hydroxide solution or a carbonate solution into the mixed solution obtained in the step S2, adjusting the pH to 8-13, stirring at the speed of 100-500 rmp, carrying out microwave heating reaction, and aging for 12 hours;
s4, post-processing: and (3) filtering the aged solution in S3, washing with ultrapure water for 3-10 times until the pH value of the filtrate is neutral, then vacuum-drying until the water content is 10% -80%, obtaining a high-activity palladium hydroxide carbon finished product, and vacuum-packaging.
Preferably, the organic solvent in S1 is one or more of methanol, ethanol or ethylene glycol, which is beneficial to improving the dispersion uniformity of the conductive carbon black.
Preferably, the conductive carbon black in S1 is one of Ketjen black series conductive carbon black, Cabot XC-72 series conductive carbon black or BP series conductive carbon black, has a good mesoporous structure, is large in specific surface area and moderate in pore size, and is beneficial to loading of active particles.
Preferably, the filtering method in S1 is positive pressure filtering or vacuum filtration, the drying method is vacuum drying, the drying temperature is 40-100 ℃, and the drying time is 10-24 hours.
Preferably, the palladium salt solution in S2 is one of palladium acetate, palladium chloride or palladium nitrate solution.
Preferably, the alkali metal hydroxide solution in S3 is a sodium hydroxide solution, and the carbonate solution is a sodium carbonate solution.
Preferably, the microwave heating power in S3 is 400-900W, and the reaction time is 5-20 min.
Preferably, the filtration method in S4 is positive pressure filtration, and the temperature for vacuum drying is 40 to 100 ℃.
The invention has the beneficial effects that:
(1) the invention adopts the conductive carbon black, has good mesoporous structure, large specific surface area and moderate aperture, is beneficial to the loading of active particles, has easily obtained raw materials, and is easier to uniformly disperse in methanol, ethanol or ethylene glycol organic solvent compared with other carbon black.
(2) The invention adopts the organic solvent and the pure water with proper proportion to treat the conductive carbon black, has no danger, and has easy acquisition of raw materials and low cost.
(3) In the step S3, in the precipitation of palladium hydroxide, an alkali metal hydroxide solution or a carbonate solution is used for adjusting the pH value to 8-13, so that palladium salt reacts at a certain speed in an alkaline environment to generate palladium hydroxide precipitate; microwave heating is adopted, and heating is rapid and uniform; and finally, aging, so that palladium hydroxide is precipitated on the conductive carbon black carrier to grow active particles, and the particle size distribution of the active particles is uniform.
(4) The preparation method provided by the invention is simple in process and suitable for large-scale production and application.
(5) The palladium hydroxide carbon prepared by the method has uniform granularity, is suitable for a general hydrogenation reaction system, and particularly improves the catalytic activity and the utilization rate of active components in the debenzylation hydrogenation process.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a TEM image of highly active palladium hydroxide on carbon prepared in example 1.
Detailed Description
Example 1
A preparation method of high-activity palladium hydroxide carbon comprises the following steps:
s1, conductive carbon black pretreatment: weighing 4.5g of XC-72 conductive carbon black, putting the XC-72 conductive carbon black into a 250ml container, adding 10ml of methanol and 100ml of ultrapure water, treating for 1h, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 100ml of ultrapure water into the carbon black treated in the step S1, then pouring a palladium acetate solution (the content of palladium is 0.5g) into the mixture, and stirring the mixture at the speed of 100rmp for 2 hours;
s3, precipitation of palladium hydroxide: adding a sodium hydroxide solution into the mixed solution obtained in the step S2, adjusting the pH value to 9-11, stirring at the speed of 100rmp, carrying out microwave heating reaction with the microwave power of 600W and the reaction time of 10min, and aging for 12 h;
s4, post-processing: and (3) filtering the aged solution in S3, cleaning for 3-10 times by using ultrapure water until the pH value of the filtrate is neutral, then performing vacuum drying at 100 ℃ until the water content is 50% to obtain a high-activity palladium hydroxide carbon finished product, and performing vacuum packaging.
Fig. 1 is a TEM image of the high-activity palladium hydroxide carbon prepared in this example, and it can be seen that the palladium hydroxide carbon particles prepared in this example have a small particle size and a uniform distribution.
Example 2
A preparation method of high-activity palladium hydroxide carbon comprises the following steps:
s1, conductive carbon black pretreatment: weighing 4.5g of BP2000 conductive carbon black, putting the BP2000 conductive carbon black into a 250ml container, adding 10ml of methanol and 100ml of ultrapure water, treating for 1h, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 100ml of ultrapure water into the carbon black treated in the step S1, then pouring a palladium acetate solution (the content of palladium is 0.5g) into the mixture, and stirring the mixture at the speed of 100rmp for 2 hours;
s3, precipitation of palladium hydroxide: adding a sodium hydroxide solution into the mixed solution obtained in the step S2, adjusting the pH value to 9-11, stirring at the speed of 100rmp, carrying out microwave heating reaction with the microwave power of 600W and the reaction time of 10min, and aging for 12 h;
s4, post-processing: and (3) filtering the aged solution in S3, cleaning for 3-10 times by using ultrapure water until the pH value of the filtrate is neutral, then performing vacuum drying at 100 ℃ until the water content is 50% to obtain a high-activity palladium hydroxide carbon finished product, and performing vacuum packaging.
Example 3
A preparation method of high-activity palladium hydroxide carbon comprises the following steps:
s1, conductive carbon black pretreatment: weighing 4.5g of XC-72 conductive carbon black, putting the XC-72 conductive carbon black into a 250ml container, adding 10ml of methanol and 100ml of ultrapure water, treating for 1h, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 100ml of ultrapure water into the carbon black treated in the step S1, then pouring a palladium chloride solution (the content of palladium is 0.5g) into the carbon black, and stirring the mixture at the speed of 100rmp for 2 hours;
s3, precipitation of palladium hydroxide: adding a sodium hydroxide solution into the mixed solution obtained in the step S2, adjusting the pH value to 9-11, stirring at the speed of 100rmp, carrying out microwave heating reaction with the microwave power of 600W and the reaction time of 10min, and aging for 12 h;
s4, post-processing: and (3) filtering the aged solution in S3, cleaning for 3-10 times by using ultrapure water until the pH value of the filtrate is neutral, then performing vacuum drying at 100 ℃ until the water content is 50% to obtain a high-activity palladium hydroxide carbon finished product, and performing vacuum packaging.
Example 4
A preparation method of high-activity palladium hydroxide carbon comprises the following steps:
s1, conductive carbon black pretreatment: weighing 4.5g of XC-72 conductive carbon black, putting the XC-72 conductive carbon black into a 250ml container, adding 10ml of methanol and 100ml of ultrapure water, treating for 1h, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 100ml of ultrapure water into the carbon black treated in the step S1, then pouring a palladium acetate solution (the content of palladium is 0.5g) into the mixture, and stirring the mixture at the speed of 100rmp for 2 hours;
s3, precipitation of palladium hydroxide: adding a sodium hydroxide solution into the mixed solution obtained in the step S2, adjusting the pH value to 9-11, stirring at the speed of 20rmp, carrying out microwave heating reaction with the microwave power of 600W and the reaction time of 10min, and aging for 12 h;
s4, post-processing: and (3) filtering the aged solution in S3, cleaning for 3-10 times by using ultrapure water until the pH value of the filtrate is neutral, then performing vacuum drying at 100 ℃ until the water content is 50% to obtain a high-activity palladium hydroxide carbon finished product, and performing vacuum packaging.
Example 5
A preparation method of high-activity palladium hydroxide carbon comprises the following steps:
s1, conductive carbon black pretreatment: weighing 4.5g of XC-72 conductive carbon black, putting the XC-72 conductive carbon black into a 250ml container, adding 10ml of methanol and 100ml of ultrapure water, treating for 1h, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 100ml of ultrapure water into the carbon black treated in the step S1, then pouring a palladium acetate solution (the content of palladium is 0.5g) into the mixture, and stirring the mixture at the speed of 100rmp for 2 hours;
s3, precipitation of palladium hydroxide: adding a sodium hydroxide solution into the mixed solution obtained in the step S2, adjusting the pH value to 9-11, stirring at the speed of 100rmp, carrying out microwave heating reaction with the microwave power of 900W and the reaction time of 10min, and aging for 12 h;
s4, post-processing: and (3) filtering the aged solution in S3, cleaning for 3-10 times by using ultrapure water until the pH value of the filtrate is neutral, then performing vacuum drying at 100 ℃ until the water content is 50% to obtain a high-activity palladium hydroxide carbon finished product, and performing vacuum packaging.
Table 1 is a table of the catalytic debenzylation performance of palladium hydroxide on carbon prepared in examples 1 to 5
As can be seen from Table 1, the smaller the particle size of the palladium hydroxide carbon particles, the more uniform the distribution, the shorter the time required for completion of the reaction, and the higher the catalyst activity.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of high-activity palladium hydroxide carbon for debenzylation is characterized by comprising the following steps:
s1, conductive carbon black pretreatment: weighing 1-100 parts of conductive carbon black, putting the conductive carbon black into a container, adding 1-100 parts of organic solvent and 1-500 parts of ultrapure water, treating for 10-90 min, and then filtering, washing and drying to obtain treated carbon black;
s2, dipping of palladium precursor: adding 1-1000 parts of ultrapure water into the carbon black treated in the step S1, then pouring a palladium salt solution, and stirring at the speed of 100-500 rmp for 0.5-5 h;
s3, precipitation of palladium hydroxide: adding an alkali metal hydroxide solution or a carbonate solution into the mixed solution obtained in the step S2, adjusting the pH to 8-13, stirring at the speed of 100-500 rmp, carrying out microwave heating reaction, and aging for 12 hours;
s4, post-processing: and (3) filtering the aged solution in S3, washing with ultrapure water for 3-10 times until the pH value of the filtrate is neutral, then vacuum-drying until the water content is 10% -80%, obtaining a high-activity palladium hydroxide carbon finished product, and vacuum-packaging.
2. The method for preparing high-activity palladium hydroxide carbon for debenzylation according to claim 1, wherein the organic solvent in S1 is one or more of methanol, ethanol or ethylene glycol.
3. The method of claim 1, wherein the conductive carbon black of S1 is one of Ketjen black series conductive carbon black, Cabot XC-72 series conductive carbon black or BP series conductive carbon black.
4. The method for preparing palladium hydroxide carbon with high activity for debenzylation according to claim 1, wherein the filtration method in S1 is positive pressure filtration or vacuum filtration, the drying method is vacuum drying, the drying temperature is 40-100 ℃, and the drying time is 10-24 h.
5. The method as claimed in claim 1, wherein the palladium salt solution in S2 is one of palladium acetate, palladium chloride and palladium nitrate.
6. The method of claim 1, wherein the alkali metal hydroxide solution in S3 is sodium hydroxide solution, and the carbonate solution is sodium carbonate solution.
7. The method for preparing palladium hydroxide carbon with high activity for debenzylation according to claim 1, wherein the microwave heating power in S3 is 400-900W, and the reaction time is 5-20 min.
8. The method for preparing palladium hydroxide carbon with high activity for debenzylation according to claim 1, wherein the filtration method in S4 is positive pressure filtration, and the temperature for vacuum drying is 40-100 ℃.
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