CN111393302A - Method for preparing high-purity p-phenylenediamine by using magnetic solid base as catalyst - Google Patents
Method for preparing high-purity p-phenylenediamine by using magnetic solid base as catalyst Download PDFInfo
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- CN111393302A CN111393302A CN202010269461.4A CN202010269461A CN111393302A CN 111393302 A CN111393302 A CN 111393302A CN 202010269461 A CN202010269461 A CN 202010269461A CN 111393302 A CN111393302 A CN 111393302A
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- magnetic solid
- phenylenediamine
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- 239000007787 solid Substances 0.000 title claims abstract description 51
- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 239000003513 alkali Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000002585 base Substances 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006722 reduction reaction Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000004927 fusion Effects 0.000 claims description 15
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000987 azo dye Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 150000004984 aromatic diamines Chemical class 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000988 sulfur dye Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of p-phenylenediamine processing, in particular to a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst, which comprises the following operation steps: uniformly mixing magnetic FesO4 powder and MgO powder in a certain proportion, adding a KF solution, uniformly stirring, adding into a reaction kettle, heating, sintering, and cooling to room temperature to obtain the required magnetic solid alkali; adding deionized water and p-nitroaniline into a high-pressure reaction kettle, increasing the pressure to 2.5-4MPa, then adding absolute ethyl alcohol and magnetic solid alkali, and continuously introducing hydrogen under a continuous stirring state to carry out hydrogenation reduction reaction; adding a proper amount of sodium hydroxide solution into the solution after reaction, then adding deionized water, filtering, placing the solution into a centrifuge for secondary separation to obtain a magnetic solid base catalyst, and drying the magnetic solid base catalyst in vacuum at low temperature to obtain the high-purity p-phenylenediamine; the invention has high reaction efficiency and high product purity, reduces the pressure of environmental pollution, can recycle the catalyst and reduces the production cost.
Description
Technical Field
The invention relates to the technical field of p-phenylenediamine processing, in particular to a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst.
Background
Para-phenylenediamine is one of the simplest aromatic diamines, is also an intermediate with wide application, can be used for preparing azo dyes and high molecular polymers, can also be used for producing fur coloring agents, rubber anti-aging agents and photo developers, and is also a commonly used sensitive reagent for detecting iron and copper. P-phenylenediamine is an extremely important dye intermediate, and is mainly used for aramid, azo dyes, sulfur dyes, acid dyes and the like.
The traditional production method of p-phenylenediamine is characterized in that p-nitrochlorobenzene is used as a raw material and reacts with ammonia water (or ammonia gas) under the conditions of high temperature and high pressure to prepare p-nitroaniline, the p-nitroaniline is reduced by sodium sulfide or iron powder to generate a p-phenylenediamine crude product, and the p-phenylenediamine with high purity is prepared by recrystallization and purification. The process has the biggest defects that more industrial wastewater is generated, a large amount of iron mud is generated by reducing iron powder, the environment is seriously polluted, the purity of the p-phenylenediamine produced by the process is low, generally about 95 percent, recrystallization purification is needed to obtain a product with the purity of more than 99 percent, and the cost is high.
Disclosure of Invention
The invention aims to provide a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst comprises the following operation steps:
s1: preparation of magnetic solid base: uniformly mixing magnetic FesO4 powder and MgO powder in a certain proportion, fully grinding, adding equal-volume KF solution, uniformly stirring and soaking for a certain time, then adding into a reaction kettle, heating to 200 ℃ for fusion for 1h, heating to 400 ℃ for fusion for 2h, heating to 600 ℃ for fusion for 3h, taking out and cooling to room temperature to obtain the required magnetic solid alkali;
s2: adding a certain weight part of deionized water and p-nitroaniline into a high-pressure reaction kettle, increasing the pressure to 2.5-4MPa, adding a certain amount of absolute ethyl alcohol and 0.15-0.21% of magnetic solid alkali by mass, continuously introducing hydrogen under a stirring state, controlling the temperature in the reaction kettle to be 65-85 ℃, and carrying out hydrogenation reduction reaction;
s3: adding a proper amount of sodium hydroxide solution into the solution after reaction, adjusting the pH value of the solution to 6-7, then adding deionized water, cooling and filtering the reaction solution, placing the filtered reaction solution into a centrifuge for secondary separation to obtain a magnetic solid base catalyst, and drying the magnetic solid base catalyst in vacuum at low temperature to obtain the high-purity p-phenylenediamine.
Preferably, the mass ratios of KF/MgO in S1) are 25%, 30%, 35%, 40%, and 45%, respectively.
Preferably, the ratio of the magnetic FesO4 powder to the MgO powder is 2: 1.1-1.6.
Preferably, deionized water is added into the S3), a part of the magnetic solid alkali is filtered, then the residual magnetic solid alkali is separated by centrifugation through a centrifuge, and the catalyst is recycled.
Preferably, a proper amount of magnesium nitrate is added into the reaction kettle in the S1) as a reaction auxiliary.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts magnetic FesO4 powder and MgO powder as raw materials to prepare magnetic solid alkali as a catalyst, promotes the reduction reaction in the process of generating p-phenylenediamine, so that the process of preparing p-phenylenediamine is simpler and easier to operate, and has the advantages of high reaction efficiency, high utilization rate of raw materials, high product purity, reduction of production waste, reduction of environmental pollution pressure, reutilization of the catalyst and reduction of production cost.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst comprises the following operation steps:
s1: preparation of magnetic solid base: uniformly mixing magnetic FesO4 powder and MgO powder in a certain proportion, fully grinding, adding equal-volume KF solution, uniformly stirring and soaking for a certain time, then adding into a reaction kettle, heating to 200 ℃ for fusion for 1h, heating to 400 ℃ for fusion for 2h, heating to 600 ℃ for fusion for 3h, taking out and cooling to room temperature to obtain the required magnetic solid alkali;
s2: adding a certain weight part of deionized water and p-nitroaniline into a high-pressure reaction kettle, increasing the pressure to 2.5-4MPa, adding a certain amount of absolute ethyl alcohol and 0.15-0.21% of magnetic solid alkali by mass, continuously introducing hydrogen under a stirring state, controlling the temperature in the reaction kettle to be 65-85 ℃, and carrying out hydrogenation reduction reaction;
s3: adding a proper amount of sodium hydroxide solution into the solution after reaction, adjusting the pH value of the solution to 6-7, then adding deionized water, cooling and filtering the reaction solution, placing the filtered reaction solution into a centrifuge for secondary separation to obtain a magnetic solid base catalyst, and drying the magnetic solid base catalyst in vacuum at low temperature to obtain the high-purity p-phenylenediamine.
Further, mass ratios of KF/MgO in S1) were 25%, 30%, 35%, 40%, and 45%, respectively.
Further, the ratio of the magnetic FesO4 powder to the MgO powder is 2: 1.1-1.6.
Further, deionized water is added into the S3), a part of magnetic solid alkali is filtered out, then the residual magnetic solid alkali is separated out through centrifugal separation by a centrifugal machine, and the catalyst is recycled.
Further, adding a proper amount of magnesium nitrate as a reaction auxiliary agent into the reaction kettle in the S1).
Example 2: a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst comprises the following operation steps:
s1: preparation of magnetic solid base: uniformly mixing magnetic FesO4 powder and MgO powder in a certain proportion, fully grinding, adding equal-volume KF solution, uniformly stirring and soaking for a certain time, then adding into a reaction kettle, heating to 200 ℃ for fusion for 1h, heating to 400 ℃ for fusion for 2h, heating to 600 ℃ for fusion for 3h, taking out and cooling to room temperature to obtain the required magnetic solid alkali;
s2: adding a certain weight part of deionized water and p-nitroaniline into a high-pressure reaction kettle, increasing the pressure to 2.5-4MPa, then adding a certain amount of absolute ethyl alcohol, magnesium nitrate and 0.15% by weight of magnetic solid alkali, continuously introducing hydrogen under a stirring state, controlling the temperature in the reaction kettle to be 65-85 ℃, and carrying out hydrogenation reduction reaction;
s3: adding a proper amount of sodium hydroxide solution into the solution after reaction, adjusting the pH value of the solution to 6-7, then adding deionized water, cooling and filtering the reaction solution, placing the filtered reaction solution into a centrifuge for secondary separation to obtain a magnetic solid base catalyst, and drying the magnetic solid base catalyst in vacuum at low temperature to obtain the high-purity p-phenylenediamine.
Further, the mass ratio of KF/MgO in S1) was 35%, respectively.
Further, the ratio of the magnetic FesO4 powder to the MgO powder is 2: 1.3.
example 2 is the same as the above examples in material, but different in the ratio and processing steps.
Example 3: a method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst comprises the following operation steps:
s1: preparation of magnetic solid base: uniformly mixing magnetic FesO4 powder and MgO powder in a certain proportion, fully grinding, adding equal-volume KF solution, uniformly stirring and soaking for a certain time, then adding into a reaction kettle, heating to 200 ℃ for fusion for 1h, heating to 400 ℃ for fusion for 2h, heating to 600 ℃ for fusion for 3h, taking out and cooling to room temperature to obtain the required magnetic solid alkali;
s2: adding a certain weight part of deionized water and p-nitroaniline into a high-pressure reaction kettle, increasing the pressure to 2.5-4MPa, then adding a certain amount of absolute ethyl alcohol, magnesium nitrate and 0.20% by weight of magnetic solid alkali, continuously introducing hydrogen under a stirring state, controlling the temperature in the reaction kettle to be 65-85 ℃, and carrying out hydrogenation reduction reaction;
s3: adding a proper amount of sodium hydroxide solution into the solution after reaction, adjusting the pH value of the solution to 6-7, then adding deionized water, cooling and filtering the reaction solution, placing the filtered reaction solution into a centrifuge for secondary separation to obtain a magnetic solid base catalyst, and drying the magnetic solid base catalyst in vacuum at low temperature to obtain the high-purity p-phenylenediamine.
Further, the mass ratios of KF/MgO in S1) were 45%, respectively.
Further, the ratio of the magnetic FesO4 powder to the MgO powder is 2: 1.6.
example 3 is the same as the above examples in material, but different in the ratio and processing steps.
The yield, catalyst recovery, and reaction efficiency of p-phenylenediamine prepared according to the formulation and preparation methods described in examples 1-3 were tested and evaluated at A, B, C, D, as shown in the following table:
| examples | Yield of the product | Catalyst recovery | Efficiency of reaction |
| Example 1 | A | A | B |
| Example 2 | C | A | B |
| Example 3 | B | C | B |
As can be seen from the table, the p-phenylenediamine prepared according to the proportion and the preparation method in the embodiment 1 has good effects on the yield and the catalyst recovery rate; the p-phenylenediamine prepared according to the proportion and the preparation method in the embodiment 2 has a good effect on the recovery rate of the catalyst; the p-phenylenediamine prepared according to the mixture ratio and the preparation method in the embodiment 3 has better effect in the aspects of yield and reaction efficiency, but has less effect than the embodiment 1.
The invention adopts the magnetic FesO4 powder and MgO powder as raw materials to prepare the magnetic solid alkali as the catalyst, promotes the reduction reaction in the process of generating the p-phenylenediamine, so that the process of preparing the p-phenylenediamine is simpler and easier to operate, and has the advantages of high reaction efficiency, high utilization rate of raw materials, high product purity, reduction of production waste, reduction of environmental pollution pressure, reutilization of the catalyst and reduction of production cost.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing high-purity p-phenylenediamine by using magnetic solid alkali as a catalyst is characterized by comprising the following steps: the method comprises the following operation steps:
s1: preparation of magnetic solid base: uniformly mixing magnetic FesO4 powder and MgO powder in a certain proportion, fully grinding, adding equal-volume KF solution, uniformly stirring and soaking for a certain time, then adding into a reaction kettle, heating to 200 ℃ for fusion for 1h, heating to 400 ℃ for fusion for 2h, heating to 600 ℃ for fusion for 3h, taking out and cooling to room temperature to obtain the required magnetic solid alkali;
s2: adding a certain weight part of deionized water and p-nitroaniline into a high-pressure reaction kettle, increasing the pressure to 2.5-4MPa, adding a certain amount of absolute ethyl alcohol and 0.15-0.21% of magnetic solid alkali by mass, continuously introducing hydrogen under a stirring state, controlling the temperature in the reaction kettle to be 65-85 ℃, and carrying out hydrogenation reduction reaction;
s3: adding a proper amount of sodium hydroxide solution into the solution after reaction, adjusting the pH value of the solution to 6-7, then adding deionized water, cooling and filtering the reaction solution, placing the filtered reaction solution into a centrifuge for secondary separation to obtain a magnetic solid base catalyst, and drying the magnetic solid base catalyst in vacuum at low temperature to obtain the high-purity p-phenylenediamine.
2. The method for preparing high-purity p-phenylenediamine with the magnetic solid base as the catalyst according to claim 1, wherein the method comprises the following steps: the mass ratios of KF/MgO in S1) are respectively 25%, 30%, 35%, 40% and 45%.
3. The method for preparing high-purity p-phenylenediamine with the magnetic solid base as the catalyst according to claim 1, wherein the method comprises the following steps: the proportion of the magnetic FesO4 powder to the MgO powder is 2: 1.1-1.6.
4. The method for preparing high-purity p-phenylenediamine with the magnetic solid base as the catalyst according to claim 1, wherein the method comprises the following steps: and S3), adding deionized water, filtering out a part of magnetic solid alkali, centrifuging by using a centrifuge to separate out the residual magnetic solid alkali, and recycling the catalyst.
5. The method for preparing high-purity p-phenylenediamine with the magnetic solid base as the catalyst according to claim 1, wherein the method comprises the following steps: and adding a proper amount of magnesium nitrate into the reaction kettle in the S1) as a reaction auxiliary agent.
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