CN106565591A - 3/4-nitrophthalimide coproduction process - Google Patents
3/4-nitrophthalimide coproduction process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/44—Iso-indoles; Hydrogenated iso-indoles
- C07D209/48—Iso-indoles; Hydrogenated iso-indoles with oxygen atoms in positions 1 and 3, e.g. phthalimide
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Abstract
The invention provides a 3/4-nitrophthalimide coproduction process and belongs to the technical field of fine chemical industry. According to the technical scheme of the invention, a mixed mono-nitrophthalic acid, which is cheap and is the by-product of the 3-nitrophthalic acid production, is adopted as a raw material. With the presence of a high-boiling-point solvent, the raw material directly reacts with urea to generate a 3/4-nitrophthalimide mixture. In this way, the coproduction of 3-nitrophthalimide and 4-nitrophthalimide is realized.
Description
Technical field
The invention belongs to technical field of fine, and in particular to single nitrophthalimide isomer mixture
Industrialized producing technology.
Background technology
3- nitrophthalimides and 4- nitrophthalimides are important organic synthesiss, medicine centre
Body and Pigment Intermediates, using value is high, wide market.Wherein synthesized the 4- for obtaining by 4- nitrophthalimides
Aminophthalimide and 5-Cyano-phthalide can be used to prepare the dyestuff of azo series and antidepressant class drug citalopram,
Be with a wide range of applications, market demand is also improved year by year, synthesize and separate single nitrophthalimide have compared with
Good market prospect.
Zhejiang Polytechnical University's journal is in disclosed in 2003《The production method of 4- nitrophthalimides》It is with neighbour
Phthalimide is initiation material, and Jing nitration mixture or concentrated nitric acid are nitrified and be obtained.The method is mixed with sulphuric acid with nitric acid or nitric acid
Compound is nitrating agent, and nitrification efficiency is low, and having in production process have in a large number spent acid to produce, and processing cost is very high, considerably increases life
Produce cost.This is also the wide variety of bottleneck problem of restriction 4- nitrophthalimides.Therefore single nitro neighbour benzene two is developed
The new technology of carboximide production, reduces production cost, reduces or eliminates the discharge of spent acid, has important practical significance.
3- nitrophthalimides disclosed in CN1369480 or 4- nitrophthalimides another kind producer
Method is that 3- nitrophthalic acids or 4- nitrophthalic acids react with carbamide in high boiling solvent.The method is with pure
3- nitrophthalic acids or 4- nitrophthalic acids are raw material, therefore cost of material is higher, and the cost of product remains high,
Constrain the popularization and application of the technique.
When 3- nitrophthalic acids are prepared, 4- nitrophthalic acids are generated simultaneously.Due to 4- nitro O-phthalics
Acid dissolubility in aqueous is larger, while 3- nitrophthalic acids and 4- nitrophthalic acids can form complex,
3- nitrophthalic acids are in aqueous after Crystallization Separation, still containing 30% 3- nitrophthalic acids and 70% in mother solution
4- nitrophthalic acids, this mixture value is relatively low, and price is partially suitable.To 3- nitros neighbour's benzene two in published document
Substantial amounts of work has been done in the separation of formic acid and 4- nitro phthalandione isomers, such as post separation, be converted into and be easily isolated
Salt or esters etc..But these technological processes are longer, cost is very high, causes the market price of 4- nitrophthalic acids
It is more much higher than 3- nitrophthalic acid.
The content of the invention
The purpose of the present invention is exactly to overcome existing 3- nitrophthalimides and 4- nitrophthalimides
The deficiency of production technology, there is provided a kind of production process environmental protection, the joint production process of the 3/4- nitrophthalimides of low cost.
The present invention is comprised the following steps：
1）Will the single nitrophthalic acid of mixing, carbamide and high boiling solvent mixing, the temperature of reaction system be 130 DEG C～
Reacted under conditions of 160 DEG C；
2）Filter after the material cooling that reaction end is obtained, obtain filter cake；
3）It is dried after filter cake is washed with the aqueous solution of alcohol, obtains 3- nitrophthalimides and 4- nitro O-phthalics
Imido mixture.
Reaction equation is as follows：
The present invention is using the cheap by-product to produce 3- nitrophthalic acids --- and mixing single nitrophthalic acid is
Raw material, directly carries out reaction generation 3/4- nitrophthalimides and mixes under conditions of high boiling solvent is present with carbamide
The method of thing, realizes the coproduction of 3- nitrophthalimides and 4- nitrophthalimides.
The present invention is mixing single nitrophthalic acid（Main component is 3- nitrophthalic acids and 4- nitros neighbour's benzene two
Formic acid）For raw material, with carbamide the mixture of single nitrophthalimide is reduced into, price inexpensively, and can abundant profit
With raw material, production process route is short, and product cost is low.Compared with the prior art, this technique shortens technological process, production process
It is the production technology of a cleaning without spent acid discharge, meets the demand for development of current clean manufacturing and the industrial policy of correlation.For
The production and its popularization and application of single nitrophthalimide has important practical significance, while producing for phthalic anhydride nitrification
The comprehensive utilization of the by-product of 3- nitrophthalic acids provides new thinking.
Raw material list nitrophthalic acid mixture is obtained through mixed acid nitrification by phthalic anhydride, although to nitrifying thick product
Thing has carried out washing and pickling post processing, but sulphuric acid still can not be washed off completely, and its content is 8%.When sulfuric acid content surpasses in raw material
Timestamp, then nitrifying the wet single nitrophthalic acid for obtaining can not be dried to powdery dry product, but thick wet product, i.e.,
Drying to nitrifying product has an impact.If the prior impact of sulphuric acid is reacted with the exceeded raw material of sulfuric acid content, meeting
Generate more by-products.So, before being reacted, it should which single nitrophthalic acid mixture is processed into qualified original
Material.
The present invention removes part of sulfuric acid firstly the need of by single nitrophthalic acid mixture, the control of sulphuric acid mass content
In 5 (wt) below %, impact can not be produced on reaction result in 190 DEG C and its following reaction.
In addition, high boiling solvent of the present invention is o-dichlorohenzene or at least one in Nitrobenzol.In this two kinds of solvents
In, the dissolubility of 3- nitrophthalimides and 4- nitrophthalimides is less, and solution viscosity is low, and solid is easy
Separate out.
The mass ratio that feeds intake of the mixing list nitrophthalic acid, carbamide and high boiling solvent is 100: 23～35:
120～150.Within the range, the conversion ratio of raw material list nitrophthalic acid reaches 94～99.5%.Carbamide addition is more than
This ratio, carbamide is much excessive, causes the waste of carbamide；And this ratio is less than, single nitrophthalic acid conversion is incomplete, makes
It is complicated into post processing.
The aqueous solution of the alcohol is at least any one mixture with water in methanol, ethanol, normal propyl alcohol or isopropanol.
This aqueous solution can simultaneously wash away the organic solvent and inorganic salt in reaction system, shorten reaction process；Simultaneously in alcohol water
The dissolubility of 3- nitrophthalimides and 4- nitrophthalimides is less in solution, does not result in the damage of product
Lose, improve the yield of product.
Alcohol and the volume ratio of water are 10～95: 100 in the aqueous solution of the alcohol.Within this range, alcohol-water solution can be simultaneously
Wash away the organic solvent and inorganic salt in reaction system.When the ratio of alcohol is less than 10%, it is impossible to by the high boiling point in reaction system
Solvent is washed off completely；And when the ratio of alcohol is higher than 95%, the inorganic salt in reaction system can not be removed.
Specific embodiment
Will be helpful to understand the present invention by example below, but be not intended to limit present disclosure.
Mixture with 3- nitrophthalic acids and 4- nitrophthalic acids as raw material, coproduction 3- nitro O-phthalics
The processing step of acid imide and 4- nitrophthalimides：
First, material prepares：
1st, raw material takes from the by-product of production 3- nitrophthalic acids --- the single nitrophthalic acid of mixing.
Jing tests wherein mainly contain 3- nitrophthalic acids, 4- nitrophthalic acids, sulphuric acid, water and micro benzene
Acid anhydride, the wherein mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids are 3:7.The content of sulphuric acid is 8%（Quality point
Number）.
Sulphur removal low-kappa number：Wash in sour kettle in stirring, add the single nitrophthalic acid 150g and 150mL water of mixing, plus
Enter a small amount of NaOH.After stirring 30min, filter, filter cake is directly used in reaction, and filtrate returns to stirring and washes sour kettle, for next group
Wash acid to be used.
The quality of Jing analysis wet cakes is 115 grams, and wherein the content of sulphuric acid is 3.8%.
2nd, solvent 1：O-dichlorohenzene, Nitrobenzol, or the mixture of o-dichlorohenzene and Nitrobenzol.
Solvent 1a：O-dichlorohenzene；
Solvent 1b：Nitrobenzol；
Solvent 1c：The mixture of o-dichlorohenzene or Nitrobenzol, its volume ratio is 8:2；
Solvent 1d：The mixture of o-dichlorohenzene or Nitrobenzol, its volume ratio is 2:8；
Solvent 1e：The mixture of o-dichlorohenzene or Nitrobenzol, its volume ratio is 5:5.
3rd, solvent 2：The aqueous solution of alcohol, including methanol, ethanol, normal propyl alcohol, isopropanol etc., also including their mixture.
Solvent 2a：The mixture of first alcohol and water, its volume ratio is 7:3；
Solvent 2b：The mixture of first alcohol and water, its volume ratio is 3:7；
Solvent 2c：The mixture of second alcohol and water, its volume ratio is 5:5；
Solvent 2d：The mixture of second alcohol and water, its volume ratio is 8:2；
Solvent 2e：The mixture of normal propyl alcohol and water, its volume ratio is 5:5.
2nd, example is produced：
1st, embodiment one：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 3.8%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1a and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1a and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2a in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A1) returns to extraction kettle.Jing
The quality of analysis dry cake is 82.3 grams, and wherein the content of 3- nitrophthalimides is 28.6%, 4- nitros neighbour's benzene two
The content of carboximide is 69.3%.
Filtrate (A1) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1a for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
2nd, embodiment two：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 3.8%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1b and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1b and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2b in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A2) returns to extraction kettle.Jing
The quality of analysis dry cake is 79.1 grams, and wherein the content of 3- nitrophthalimides is 28.8%, 4- nitros neighbour's benzene two
The content of carboximide is 69.1%.
Filtrate (A2) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1b for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
3rd, embodiment three：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 3.8%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1c and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1c takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1c returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1c and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2c in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A3) returns to extraction kettle.Jing
The quality of analysis dry cake is 78.6 grams, and wherein the content of 3- nitrophthalimides is 26.8%, 4- nitros neighbour's benzene two
The content of carboximide is 68.2%.
Filtrate (A3) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1c for isolating is returned
To reactor, solvent 2c enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
4th, example IV：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 3.8%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1d and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1d takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1d returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1d and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2d in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A4) returns to extraction kettle.Jing
The quality of analysis dry cake is 75.9 grams, and wherein the content of 3- nitrophthalimides is 28.1%, 4- nitros neighbour's benzene two
The content of carboximide is 67.3%.
Filtrate (A4) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1d for isolating is returned
To reactor, solvent d2 enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
5th, embodiment five：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 3.8%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1e and carbamide, are warming up to 135 DEG C and start reaction.The water that solvent 1d takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1e returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1e and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2e in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A5) returns to extraction kettle.Jing
The quality of analysis dry cake is 75.6 grams, and wherein the content of 3- nitrophthalimides is 28.2%, 4- nitros neighbour's benzene two
The content of carboximide is 67.5%.
Filtrate (A4) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1d for isolating is returned
To reactor, solvent d2 enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
6th, embodiment six：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 5:5, the content of sulphuric acid is 3.8%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1a and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1a and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2a in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A6) returns to extraction kettle.Jing
The quality of analysis dry cake is 82.7 grams, and wherein the content of 3- nitrophthalimides is 29.1%, 4- nitros neighbour's benzene two
The content of carboximide is 69.0%.
Filtrate (A6) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1a for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
7th, embodiment seven：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 5:5, the content of sulphuric acid is 2.1%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 120 grams of agent 1a and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1a and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2a in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A7) returns to extraction kettle.Jing
The quality of analysis dry cake is 82.5 grams, and wherein the content of 3- nitrophthalimides is 28.7%, 4- nitros neighbour's benzene two
The content of carboximide is 69.4%.
Filtrate (A7) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1a for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
8th, embodiment eight：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 4.7%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
35 grams of 120 grams of agent 1a and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1a and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2a in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A8) returns to extraction kettle.Jing
The quality of analysis dry cake is 84.5 grams, and wherein the content of 3- nitrophthalimides is 28.3%, 4- nitros neighbour's benzene two
The content of carboximide is 69.2%.
Filtrate (A8) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1a for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
9th, embodiment nine：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 4.7%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
25 grams of 140 grams of agent 1a and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1a and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2a in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A9) returns to extraction kettle.Jing
The quality of analysis dry cake is 78.3 grams, and wherein the content of 3- nitrophthalimides is 28.5%, 4- nitros neighbour's benzene two
The content of carboximide is 69.7%.
Filtrate (A9) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1a for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
10th, embodiment ten：
In this example, the mass ratio of 3- nitrophthalic acids and 4- nitrophthalic acids in single nitrophthalic acid mixture
For 3:7, the content of sulphuric acid is 4.7%（Mass fraction）.
100 grams of single nitrophthalic acid mixture after deacidification is added in the stirred autoclave with backflow, is added molten
35 grams of 160 grams of agent 1a and carbamide, are warming up to 130 DEG C and start reaction.The water that solvent 1a takes out of in intensification and course of reaction is by a point water
Device is separated, and solvent 1a returns to response system；The tail gas that carbamide is decomposed to give off is by alkali liquor absorption.When reaction system temperature rises to
When 160 DEG C, reaction terminates, and stops heating.
The material that reaction terminates is cooled to room temperature, filters；Filtrate is solvent 1a and a small amount of single nitro phthalyl is sub-
Amine, returns to reactor；Filter cake is washed with solvent 2a in washing kettle；Filter cake after washing is 3- nitro phthalyls
The mixture of imines and 4- nitrophthalimides, is dried with conventional method；Filtrate (A10) returns to extraction kettle.
The quality of Jing analysis dry cakes is 78.4 grams, and wherein the content of 3- nitrophthalimides is 28.6%, 4- nitros neighbour's benzene
The content of dicarboximide is 69.6%.
Filtrate (A10) is extracted in extractor, and organic faciess enter into rectifying column and separated, and the solvent 1a for isolating is returned
To reactor, solvent 2a enters washing kettle, for the washing of lower batch materials.Water is mutually returned directly to washing kettle.
Claims (6)
1. a kind of joint production process of 3/4- nitrophthalimides, it is characterised in that comprise the following steps：
1）Will the single nitrophthalic acid of mixing, carbamide and high boiling solvent mixing, the temperature of reaction system be 130 DEG C～
Reacted under conditions of 160 DEG C；
2）Filter after the material cooling that reaction end is obtained, obtain filter cake；
3）It is dried after filter cake is washed with the aqueous solution of alcohol, obtains 3- nitrophthalimides and 4- nitro O-phthalics
Imido mixture.
2. joint production process according to claim 1, it is characterised in that sulphuric acid in the mixing list nitrophthalic acid
Mass fraction≤5%.
3. joint production process according to claim 1 and 2, it is characterised in that the high boiling solvent is o-dichlorohenzene or nitro
At least one in benzene.
4. joint production process according to claim 1 and 2, it is characterised in that the mixing list nitrophthalic acid, carbamide
The mass ratio that feeds intake with high boiling solvent is 100: 23～35: 120～150.
5. joint production process according to claim 1 and 2, it is characterised in that the aqueous solution of the alcohol be methanol, ethanol, positive third
At least any one mixture with water in alcohol or isopropanol.
6. joint production process according to claim 5, it is characterised in that alcohol is with the volume ratio of water in the aqueous solution of the alcohol
10～95: 100.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113549001A (en) * | 2021-07-21 | 2021-10-26 | 华阳新材料科技集团有限公司 | Preparation method of N-alkyl-4-nitrophthalimide |
Citations (2)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113549001A (en) * | 2021-07-21 | 2021-10-26 | 华阳新材料科技集团有限公司 | Preparation method of N-alkyl-4-nitrophthalimide |
| CN113549001B (en) * | 2021-07-21 | 2024-03-22 | 华阳新材料科技集团有限公司 | Preparation method of N-alkyl-4-nitrophthalimide |
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