CN108892620A - 4,4 ' of one kind, the 4 " preparation methods of-triaminotriphenyl-methane - Google Patents
4,4 ' of one kind, the 4 " preparation methods of-triaminotriphenyl-methane Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C209/78—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton from carbonyl compounds, e.g. from formaldehyde, and amines having amino groups bound to carbon atoms of six-membered aromatic rings, with formation of methylene-diarylamines
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/34—Polysulfides of sodium or potassium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C221/00—Preparation of compounds containing amino groups and doubly-bound oxygen atoms bound to the same carbon skeleton
Abstract
The present invention provides one kind 4,4 ', 4 "-triaminotriphenyl-methane preparation method; the preparation of preparation, para aminotenzaldehyde including sodium polysulfide solution, the preparation of crude product, once saltout, primary purification, it is secondary saltout, seven steps of secondary refining; obtaining purity and being greater than 99%, iron ion content can control in 20ppm below 4; 4 ', 4 "-triaminotriphenyl-methanes.The present invention is compared with existing route, with the advantage that process route is simple and quantity of three wastes greatly reduces.
Description
Technical field
The present invention relates to adhesive preparation technical fields, and in particular to a kind of 4,4 ', 4 "-triaminotriphenyl-methane of high-purity
Preparation method.
Background technique
4,4 ', 4 "-triaminotriphenyl-methane also known as p-Leuconiline are one kind of triaminotriphenyl-methane dyestuff, main
It is used as adhesive-column Kona rubber primary raw material of manufacture rubber and metal.
Mainly there are two lines to prepare 4,4 ', 4 "-triaminotriphenyl-methanes at present：
One of method is reported under hydrochloric acid or acetic acid existence condition by former Soviet Union patent RU2258724, zinc powder reduction
Paramagenta obtains 4,4 ', 4 "-triaminotriphenyl-methane.The route first has to obtain dyestuff paramagenta, then paramagenta reduction is obtained
Target product is obtained, operating procedure is tired more, and reaction is not easily controlled, and dyestuff paramagenta yield itself is not high, reducing agent price
High (zinc and hydrochloric acid or sodium hydrosulfite carry out in alcoholic solution).From the point of view of Technological Economy viewpoint, this method does not have industrial value.
"-triaminotriphenyl-methane work that another method is disclosed by Chinese patent CN106977408, provides 4,4 ', 4
Industry preparation route prepares para aminotenzaldehyde through sodium polysulfide redox, in hydrochloric acid using para-nitrotoluene as starting material
Under catalysis, crude product is obtained with aniline condensation, crude product content after refining is 93% or so, and fusing point is 192 DEG C.The industrialization of this route
Easy to operate, but quantity of three wastes is big, it is relatively low to be prepared product content, can not meet customer requirement.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of 4,4 ', 4 " preparation sides of-triaminotriphenyl-methane
Method.The technical scheme is that：
" preparation method of-triaminotriphenyl-methane, includes the following steps one kind 4,4 ', 4：
1) preparation of sodium polysulfide solution：Sodium hydroxide solution is heated to 90~100 DEG C, sulphur is added portionwise,
Insulated and stirred 3~5 hours later；Shown in reaction equation such as formula [1]：
6NaOH+5S→Na2S+Na2S2+Na2S2O3+3H2O [1]；
2) preparation of para aminotenzaldehyde：The mixed solution of para-nitrotoluene and ethyl alcohol is heated to flowing back, is added dropwise in batches
Sodium polysulfide solution, control time for adding are 3~4 hours, after being added dropwise, and flow back lower heat preservation 3~5 hours, are concentrated to dryness, point
It Shou Ji not para aminotenzaldehyde concentrate and ethyl alcohol；Shown in reaction equation such as formula [2]：
3) preparation of crude product：Aniline is added into para aminotenzaldehyde concentrate, it is whole to para aminotenzaldehyde concentrate
It is dissolved in aniline, hydrochloric acid and phase transfer catalyst is added, be warming up at 100~105 DEG C and react 8~12 hours, after reaction, in
With to alkalinity, vacuum concentration, collect 4,4 ', 4 respectively "-triaminotriphenyl-methane crude product and aniline；Reaction equation such as formula [3]
It is shown：
4) it once saltouts：To 4,4 ', 4 " hydrochloric acid and water are added in-triaminotriphenyl-methane crude product, is warming up to 60~70 DEG C,
After all dissolutions, sodium chloride is added in batches, after addition, insulated and stirred 2 hours at 60~70 DEG C make its abundant salt
Analysis, is then cooled to 30~35 DEG C, " the hydrochloride, crude of-triaminotriphenyl-methane that is obtained by filtration 4,4 ', 4；
5) primary purification：By 4,4 ', 4, " hydrochloride, crude, water and the active carbon of-triaminotriphenyl-methane are uniformly mixed, and are risen
Temperature was to insulated and stirred 1~3 hour at 60~80 DEG C, and heat filtering removes active carbon and insoluble matter, filtrate are neutralized to alkalinity with ammonium hydroxide,
Then it is warming up at 80~100 DEG C and stirs 1~3 hour, so that it is sufficiently turned brilliant, be cooled to 20~30 DEG C later, be obtained by filtration one
Secondary highly finished product；
6) secondary to saltout：A refined product and mixed in hydrochloric acid are uniform, 60~80 DEG C are warming up to, is all dissolved to crude product,
Sodium chloride is added in batches, after addition, insulated and stirred 2 hours, make it sufficiently saltout at 60~80 DEG C, are then cooled to 15
" the hydrochloride sterling of-triaminotriphenyl-methane that~25 DEG C, is obtained by filtration 4,4 ', 4；
7) secondary refining：" hydrochloride sterling, deionized water, active carbon and the metal of-triaminotriphenyl-methane by 4,4 ', 4
Complexing agent is uniformly mixed, and is warming up to insulated and stirred 1~3 hour at 60~80 DEG C, and after filtering, filtrate is neutralized to alkalinity with ammonium hydroxide,
Then it is warming up at 80~100 DEG C and stirs 1~3 hour, so that it is sufficiently turned brilliant, be cooled to room temperature, secondary fine product is obtained by filtration.
Further, concentration of sodium hydroxide solution is 30~35% in the step 1), and sulfur consumption is with itself and hydroxide
The molar ratio of sodium is (0.5~1): 1 meter.
Further, in the step 2) para-nitrotoluene dosage by its molar ratio with sulphur for 1: in terms of (1~2), second
Alcohol dosage is 2~5 times of para-nitrotoluene weight inventory.
Further, in the step 3) aniline dosage by its molar ratio with para-nitrotoluene for (6~12): in terms of 1, salt
Sour dosage is by its molar ratio with para-nitrotoluene for (3~4): 1 in terms of, phase transfer catalyst dosage is the throwing of para-nitrotoluene weight
The 1~10% of doses.
Further, the phase transfer catalyst includes quaternary ammonium salt or polyethers.
Further, in the step 4) hydrochloric acid dosage by its molar ratio with para-nitrotoluene for (2~3): in terms of 1, water
Dosage is 3~5 times of para-nitrotoluene weight inventory, and sodium chloride dosage is the 1~1.5 of para-nitrotoluene weight inventory
Times.
Further, water consumption is 8~12 times of para-nitrotoluene weight inventory in the step 5), activated carbon dosage
It is the 5~20% of para-nitrotoluene weight inventory.
Further, concentration of hydrochloric acid is 11% in the step 6), and hydrochloric acid dosage is with the molar ratio of itself and a refined product
For (4~6): 1 meter, sodium chloride dosage is 1~1.5 times of a refined product weight inventory.
Further, deionized water dosage is 8~12 times of a refined product weight inventory in the step 7), activity
Charcoal dosage is the 5~20% of a refined product weight inventory, and metal chelating agent dosage is a refined product weight inventory
0.5~5%.
Further, the deionized water is distilled water or reverse osmosis water.
Further, the metal chelating agent includes ethylenediamine tetra-acetic acid or disodium EDTA.
Secondary fine product of the invention is greater than 99% through liquid spectrum detection level, and metal ion content is in 20ppm hereinafter, especially
It is that iron ion content can control well in 20ppm or less.
Advantage for present invention：Provided by the invention 4,4 ', 4 "-triaminotriphenyl-methane preparation route and existing road
Line is compared, simply and the advantage that greatly reduces of quantity of three wastes with process route, and prepared by the present invention 4,4 ', 4 "-three ammonia of use
Base triphenylmenthane fluorenes coloration is good, and purity is greater than 99%, and iron ion content can control in 20ppm hereinafter, can satisfy client needs
It asks, is mainly used for exporting to foreign countries.
Specific embodiment
In the description of the present invention, it should be noted that the person that is not specified actual conditions in embodiment, according to normal conditions or
The condition that manufacturer suggests carries out.Reagents or instruments used without specified manufacturer is that can be obtained by commercially available purchase
Conventional products.
The present invention is described in further details below with reference to specific embodiment, it is described be explanation of the invention without
It is to limit.
Embodiment 1
44g sodium hydroxide is added into 250ml flask and 90g water, heated solution stir at this temperature to 90~100 DEG C
After mixing 10min, sulphur powder 26g, feed time 30min in batches.After finishing, after being stirred 3 hours at 90~100 DEG C, obtain
Dark yellow transparency liquid, it is spare.
70g para-nitrotoluene and 246g ethyl alcohol are added into the flask of 1000ml, and is heated to strong inverse flow state.It is returning by force
Under stream mode (temperature is about at 84 DEG C or so), configured sodium polysulfide solution is slowly added dropwise, feed time is 3 hours.More sulphur
After changing sodium solution addition, stirred 3 hours under strong inverse flow state.After insulation reaction, start that ethyl alcohol is distilled off, when
Stop heating when vapo(u)rizing temperature is up to 105~110 DEG C, material at this time is very sticky paste.
558g aniline is added into above-mentioned 1000ml flask, continues the aniline stirred to para aminotenzaldehyde is all dissolved into
Solution is subsequently added into 189g33% hydrochloric acid and 7g tetrabutylammonium bromide, heats feed liquid up to 100~105 DEG C, at 100~105 DEG C
Stirring 12 hours, is added solid 76g sodium hydroxide, and the aobvious alkalinity of feed liquid then removes excessive benzene using oil pump high vacuum distillation
Amine.
After distillation, 161g33% hydrochloric acid and 244g water are then added into flask, and be heated to 60 DEG C to make its whole
Dissolution, is added portionwise 86g refined salt at 60 DEG C, and adding the salt time is 5~10 minutes, and insulated and stirred 2 hours at 60 DEG C terminate
Afterwards, 30~35 DEG C are cooled to, filters to obtain yellow filter cake, and with saturated common salt water washing filter cake.
Previous step yellow filter cake and 590g water are added into 1000ml flask, is heated to material to 60 DEG C, at 60 DEG C, adds
Enter 7g active carbon, stirred 2 hours at 60 DEG C, heat filtering removes activated carbon and insoluble matter, obtains kermesinus transparence liquid, is added
In ammonium hydroxide and material liquid PH value is 9~11, and is warming up to 85 DEG C, is stirred 1 hour at 85 DEG C.20~30 DEG C are water-cooled to, mistake
Neutrality is filtered and be washed with water to, obtains 70.1g product, yield 48.5%, content 96.0% after dry.
The dilute hydrochloric acid of 70.1g crude product and 402g11% is added into 1000ml four-hole boiling flask, when being heated to 60 DEG C, crude product is complete
Portion's dissolution, 71g refined salt is added at this time, is sufficiently stirred 2 hours, is water-cooled to 20~25 DEG C, filter to obtain pale solid, be used in combination
Saturated common salt water washing filter cake.
Obtained pale solid is added in four-hole boiling flask, 720g deionized water and 0.7g ethylenediamine tetrem is added
Acid is heated to material to 60 DEG C, at 60 DEG C, 7g active carbon is added, stirs 2 hours at 60 DEG C, is filtered to remove activated carbon, obtains
Kermesinus transparence liquid, is added in ammonium hydroxide and feed liquid is aobvious alkaline, and is warming up to 85 DEG C, stirs 1 hour at 85 DEG C.Use cold water
It is cooled to room temperature, filters and be washed with water to neutrality, obtain 65g product after dry.Content is 99.3%, total recovery 45%,
It is 6.3ppm that iron ion, which contains,.
Embodiment 2
44g sodium hydroxide is added into 250ml flask and 82g water, heated solution stir at this temperature to 90~100 DEG C
After mixing 10min, sulphur powder 20g, feed time 30min in batches.After finishing, after being stirred 4 hours at 90~100 DEG C, obtain
Dark yellow transparency liquid, it is spare.
70g para-nitrotoluene and 175g ethyl alcohol are added into the flask of 1000ml, and is heated to strong inverse flow state.It is returning by force
Under stream mode (temperature is about at 84 DEG C or so), configured sodium polysulfide solution is slowly added dropwise, feed time is 4 hours.More sulphur
After changing sodium solution addition, stirred 4 hours under strong inverse flow state.After insulation reaction, start that ethyl alcohol is distilled off, when
Stop heating when vapo(u)rizing temperature is up to 105~110 DEG C, material at this time is very sticky paste.
Then 418g aniline is added into above-mentioned 1000ml flask, continues to stir to being all dissolved into para aminotenzaldehyde
Aniline solution is subsequently added into 166g33% hydrochloric acid and 3.5g methyl bromide ammonium, heats feed liquid up to 100~105 DEG C, 100~105
It is stirred 10 hours at DEG C, solid 66g sodium hydroxide is added, the aobvious alkalinity of feed liquid is then removed using oil pump high vacuum distillation excessive
Aniline.
After distillation, 110g33% hydrochloric acid and 280g water are then added into flask, and be heated to 65 DEG C to make its whole
Dissolution, is added portionwise 70g refined salt at 65 DEG C, and adding the salt time is 5~10 minutes, and insulated and stirred 2 hours at 65 DEG C terminate
Afterwards, 30~35 DEG C are cooled to, filters to obtain yellow filter cake, and with saturated common salt water washing filter cake.
Previous step yellow filter cake and 700g water are added into 1000ml flask, is heated to material to 70 DEG C, at 70 DEG C, adds
Entering 10.5g active carbon, is stirred 1 hour at 70 DEG C, heat filtering removes activated carbon and insoluble matter, kermesinus transparence liquid is obtained,
It is added in ammonium hydroxide and material liquid PH value is 9~11, and be warming up to 90 DEG C, stirred 2 hours at 90 DEG C.It is cooled to room temperature with cold water,
Neutrality is filtered and be washed with water to, obtains 58g product, yield 40.1%, content 97.5% after dry.
The dilute hydrochloric acid of 58g crude product and 270g11% is added into 1000ml four-hole boiling flask, when being heated to 70 DEG C, crude product is whole
70g refined salt is added at this time, 2 lab scales are sufficiently stirred, are water-cooled to 15~20 DEG C, filters to obtain pale solid for dissolution, and with satisfying
With brine It filter cake.
Obtained pale solid is added in four-hole boiling flask, 470g deionized water and 1.7g ethylenediamine tetrem is added
Acid is heated to material to 70 DEG C, at 70 DEG C, 9g active carbon is added, stirs 2 hours at 70 DEG C, is filtered to remove activated carbon, obtains
Kermesinus transparence liquid, is added in ammonium hydroxide and feed liquid is aobvious alkaline, and is warming up to 90 DEG C, stirs 2 hours at 90 DEG C.Use cold water
It is cooled to room temperature, filters and be washed with water to neutrality, obtain 50g product after dry.Content is 99.4%, total recovery is
34.6%, it is 10.2ppm that iron ion, which contains,.
Embodiment 3
44g sodium hydroxide is added into 250ml flask and 102g water, heated solution stir at this temperature to 90~100 DEG C
After mixing 10min, sulphur 32g, feed time 30min in batches.After finishing, after being stirred 5 hours at 90~100 DEG C, obtain dark
Yellow transparent liquid, it is spare.
70g para-nitrotoluene and 350g ethyl alcohol are added into the flask of 1000ml, and is heated to strong inverse flow state.It is returning by force
Under stream mode (temperature is about at 84 DEG C or so), configured sodium polysulfide solution is slowly added dropwise, feed time is 3 hours.More sulphur
After changing sodium solution addition, stirred 5 hours under strong inverse flow state.After insulation reaction, start that ethyl alcohol is distilled off, when
Stop heating when vapo(u)rizing temperature is up to 105~110 DEG C, material at this time is very sticky paste.
Then 279g aniline is added into above-mentioned 1000ml flask, continues to stir to being all dissolved into para aminotenzaldehyde
Aniline solution is subsequently added into 221g33% hydrochloric acid and 7g polyethylene glycol-8 00, heats feed liquid up to 100~105 DEG C, 100~105
It is stirred 8 hours at DEG C, solid 88g sodium hydroxide is added, the aobvious alkalinity of feed liquid is then removed using oil pump high vacuum distillation excessive
Aniline.
After distillation, 166g hydrochloric acid and 350g water are then added into flask, and being heated to 70 DEG C dissolves it all,
105g refined salt is added portionwise at 70 DEG C, adding the salt time is 5~10 minutes, insulated and stirred 2 hours at 70 DEG C, after, drop
Temperature filters to obtain yellow filter cake to 30~35 DEG C, and with saturated common salt water washing filter cake.
Previous step yellow filter cake and 800g water are added into 1000ml flask, is heated to material to 80 DEG C, at 80 DEG C, adds
Enter 14g active carbon, stirred 3 hours at 80 DEG C, heat filtering removes activated carbon and insoluble matter, obtains kermesinus transparence liquid, adds
Enter in ammonium hydroxide and the aobvious pH value of feed liquid is 9~11, and be warming up to 95 DEG C, is stirred 3 hours at 95 DEG C.It is cooled to room temperature with cold water,
Neutrality is filtered and be washed with water to, obtains 65g product, yield 45%, content 97.2% after dry.
The dilute hydrochloric acid hydrochloric acid of 65g crude product and 448g11%, when being heated to 80 DEG C, crude product are added into 1000ml four-hole boiling flask
97g refined salt is added at this time, is sufficiently stirred 2 hours, is water-cooled to 15~20 DEG C, filter to obtain pale solid for all dissolutions, and
With saturated common salt water washing filter cake.
Obtained pale solid is added in four-hole boiling flask, 780g deionized water and 3.2g ethylenediamine tetra-acetic acid is added
Disodium salt is heated to material to 80 DEG C, at 80 DEG C, 13g active carbon is added, stirs 2 hours at 80 DEG C, heat filtering removes deactivation
Carbon obtains kermesinus transparence liquid, is added in ammonium hydroxide and feed liquid is aobvious alkaline, and be warming up to 95 DEG C, it is small that 2 are stirred at 95 DEG C
When.It is cooled to room temperature with cold water, filters and be washed with water to neutrality, 55g product is obtained after dry, content 99.5% is total to receive
Rate is 38.1%, and it is 5.4ppm that iron ion, which contains,.
To sum up, using specific embodiment of the invention preparation 4,4 ', 4 "-triaminotriphenyl-methane fluorenes coloration is good, and purity is big
In 99%, iron ion content be can control in 20ppm or less.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. 4,4 ', the 4 " preparation method of-triaminotriphenyl-methane, which is characterized in that include the following steps of one kind：
1) preparation of sodium polysulfide solution：Sodium hydroxide solution is heated to 90~100 DEG C, sulphur is added portionwise, later
Insulated and stirred 3~5 hours；
2) preparation of para aminotenzaldehyde：The mixed solution of para-nitrotoluene and ethyl alcohol is heated to flowing back, more sulphur are added dropwise in batches
Change sodium solution, control time for adding is 3~4 hours, after being added dropwise, and flows back lower heat preservation 3~5 hours, is concentrated to dryness, receives respectively
Collect para aminotenzaldehyde concentrate and ethyl alcohol；
3) preparation of crude product：Aniline is added into para aminotenzaldehyde concentrate, is all dissolved in para aminotenzaldehyde concentrate
Aniline is added hydrochloric acid and phase transfer catalyst, is warming up at 100~105 DEG C and reacts 8~12 hours, after reaction, be neutralized to
Alkalinity, vacuum concentration, collect 4,4 ', 4 respectively "-triaminotriphenyl-methane crude product and aniline；
4) it once saltouts：To 4,4 ', 4 " hydrochloric acid and water is added in-triaminotriphenyl-methane crude product, 60~70 DEG C are warming up to, to complete
After portion's dissolution, sodium chloride is added in batches, after addition, insulated and stirred 2 hours, make it sufficiently saltout at 60~70 DEG C, connect
Be cooled to 30~35 DEG C, " the hydrochloride, crude of-triaminotriphenyl-methane that is obtained by filtration 4,4 ', 4；
5) primary purification：By 4,4 ', 4, " hydrochloride, crude, water and the active carbon of-triaminotriphenyl-methane are uniformly mixed, and are warming up to
Insulated and stirred 1~3 hour at 60~80 DEG C, heat filtering removes active carbon and insoluble matter, filtrate are neutralized to alkalinity with ammonium hydroxide, then
It is warming up at 80~100 DEG C and stirs 1~3 hour, so that it is sufficiently turned brilliant, be cooled to 20~30 DEG C later, primary essence is obtained by filtration
Product；
6) secondary to saltout：A refined product and mixed in hydrochloric acid are uniform, 60~80 DEG C are warming up to, is all dissolved to crude product, in batches
Secondary addition sodium chloride, after addition, insulated and stirred 2 hours, make it sufficiently saltout at 60~80 DEG C, are then cooled to 15~25
DEG C, " the hydrochloride sterling of-triaminotriphenyl-methane that is obtained by filtration 4,4 ', 4；
7) secondary refining：" hydrochloride sterling, deionized water, active carbon and the metal complex of-triaminotriphenyl-methane by 4,4 ', 4
Agent is uniformly mixed, and is warming up to insulated and stirred 1~3 hour at 60~80 DEG C, after filtering, filtrate is neutralized to alkalinity with ammonium hydroxide, then
It is warming up at 80~100 DEG C and stirs 1~3 hour, so that it is sufficiently turned brilliant, be cooled to room temperature, secondary fine product is obtained by filtration.
2. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Concentration of sodium hydroxide solution is 30~35% in step 1), and sulfur consumption is with its molar ratio with sodium hydroxide for (0.5~1): 1
Meter.
3. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Para-nitrotoluene dosage is by its molar ratio with sulphur for 1 in step 2): in terms of (1~2), ethanol consumption is para-nitrotoluene weight
2~5 times of inventory.
4. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Aniline dosage is by its molar ratio with para-nitrotoluene for (6~12) in step 3): in terms of 1, hydrochloric acid dosage with its with to nitro first
The molar ratio of benzene is (3~4): 1 meter, phase transfer catalyst dosage is the 1~10% of para-nitrotoluene weight inventory.
5. according to claim 1 or 4 a kind of 4,4 ', the 4 " preparation method of-triaminotriphenyl-methane, which is characterized in that
The phase transfer catalyst includes quaternary ammonium salt or polyethers.
6. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Hydrochloric acid dosage is by its molar ratio with para-nitrotoluene for (2~3) in step 4): 1 in terms of, water consumption is the throwing of para-nitrotoluene weight
3~5 times of doses, sodium chloride dosage are 1~1.5 times of para-nitrotoluene weight inventory.
7. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Water consumption is 8~12 times of para-nitrotoluene weight inventory in step 5), and activated carbon dosage is that para-nitrotoluene weight feeds intake
The 5~20% of amount.
8. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Concentration of hydrochloric acid is 11% in step 6), and hydrochloric acid dosage is by its molar ratio with a refined product for (4~6): 1 in terms of, sodium chloride use
Amount is 1~1.5 times of a refined product weight inventory.
9. according to claim 1 a kind of 4,4 ', the 4 " preparation methods of-triaminotriphenyl-methane, which is characterized in that described
Deionized water dosage is 8~12 times of a refined product weight inventory in step 7), and activated carbon dosage is a refined product weight
The 5~20% of inventory are measured, metal chelating agent dosage is the 0.5~5% of a refined product weight inventory.
10. according to claim 1 or one kind 4,4 ', 4 described in 9 " preparation method of-triaminotriphenyl-methane, which is characterized in that
The metal chelating agent includes ethylenediamine tetra-acetic acid or disodium EDTA.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979878A (en) * | 2021-10-29 | 2022-01-28 | 浙江工业大学 | Preparation method of 2-aminobenzaldehyde |
| CN114835595A (en) * | 2022-05-16 | 2022-08-02 | 漯河市新旺化工有限公司 | Preparation method of triphenylmethane ultraviolet absorber |
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| CN113979878A (en) * | 2021-10-29 | 2022-01-28 | 浙江工业大学 | Preparation method of 2-aminobenzaldehyde |
| CN113979878B (en) * | 2021-10-29 | 2024-05-03 | 浙江工业大学 | Preparation method of 2-aminobenzaldehyde |
| CN114835595A (en) * | 2022-05-16 | 2022-08-02 | 漯河市新旺化工有限公司 | Preparation method of triphenylmethane ultraviolet absorber |
| CN114835595B (en) * | 2022-05-16 | 2024-04-05 | 漯河市新旺化工有限公司 | Preparation method of triphenylmethane ultraviolet light absorbent |
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