CN106008220A - Method for preparing p-nitrobenzoic acid through polystyrene foam - Google Patents
Method for preparing p-nitrobenzoic acid through polystyrene foam Download PDFInfo
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- CN106008220A CN106008220A CN201610449944.6A CN201610449944A CN106008220A CN 106008220 A CN106008220 A CN 106008220A CN 201610449944 A CN201610449944 A CN 201610449944A CN 106008220 A CN106008220 A CN 106008220A
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- polystyrene foam
- acid
- prepare
- nitrodracylic
- method utilizing
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing p-nitrobenzoic acid through polystyrene foam. The method includes the following steps of firstly, foam processing; secondly, microwave digestion; thirdly, catalytic oxidization; fourthly, product separating and purifying. The method is easy and convenient to operate and easy to implement; with waste polystyrene foam as the raw material, by means of a nitric acid digestion and oxygen oxidization method, on one hand, waste is turned into wealth and raw material cost is reduced, and on the other hand, the problem that corrosion is severe when nitric acid is directly used for oxidization is effectively solved; the product is high in purity, high in yield and easy to separate.
Description
Technical field
The present invention relates to chemical products field, particularly relate to a kind of method utilizing polystyrene foam to prepare Nitrodracylic acid.
Background technology
Nitrodracylic acid is a kind of important medicine intermediate and organic synthesis raw material, can be used for producing the important source material of the medicine such as procaine hydrochloride, procaine amide hydrochloride, folic acid, benzocaine, tranamic acid, also being the important intermediate producing the chemical products such as pesticide, dyestuff, industrial demand is the biggest.Traditional Nitrodracylic acid uses high-valency metal salt oxidizing p-nitrotoluene, because cost is the highest, serious to equipment corrosion and produce a large amount of industrial wastes and be prohibited.Existing method uses nitric acid oxidation and liquid-phase catalysis air oxidation process, the former low cost, and postharvest treatment is simple, but the seriously corroded to equipment；The latter, with glacial acetic acid as solvent, produces industrial wastewater, waste gas, pollutes environment；Preparing further, since current Nitrodracylic acid all carries out oxidation with para-nitrotoluene for raw material, cost of material is higher.
Summary of the invention
The technical problem that present invention mainly solves is to provide a kind of method utilizing polystyrene foam to prepare Nitrodracylic acid, it is possible to solve the difficult problem that the etching apparatus of preparation existence, pollution environment and the cost of material of existing Nitrodracylic acid are high.
For solving above-mentioned technical problem, the technical scheme that the present invention uses is: provides a kind of method utilizing polystyrene foam to prepare Nitrodracylic acid, comprises the steps:
(1) defoaming treatment: polystyrene foam is added in hot froth breaker, defoaming treatment 1～3h at 60～80 DEG C, make foam volume narrow down to original 1/30, then take out pulverizing；
(2) micro-wave digestion: the polystyrene foam after defoaming treatment in step (1) is added in microwave dissolver, is simultaneously introduced a certain amount of salpeter solution, carries out micro-wave digestion process under uniform temperature and pressure；
(3) catalysis oxidation: the mixture after micro-wave digestion in step (2) is carried out filter pressing, take filtrate and insert in reactor, then a certain amount of catalyst dissolution liquid is added, after mix homogeneously, pour oxysome to reacting kettle inner pressure and reach 1～2MPa, finally carrying out isothermal reaction 8～10h in the water bath of uniform temperature, reaction is cooled to room temperature after terminating；
(4) separation and purification of products: add deionized water stirring layering in step (3) in reacted mixed liquor, takes the supernatant and is added thereto to dilute acid soln extremely acidity, then sucking filtration, vacuum drying, obtaining described Nitrodracylic acid.
In a preferred embodiment of the present invention, in described step (2), the mass concentration of described salpeter solution is 60～65%, and its addition is 1～2 times of described polystyrene foam quality.
In a preferred embodiment of the present invention, in described step (2), the temperature of described micro-wave digestion is 220～250 DEG C, and pressure is 20～25MPa, and the time is 3～5min.
In a preferred embodiment of the present invention, in described step (3), addition is filtrate volume 2～5 times of described catalyst dissolution liquid；Described reaction temperature is 120 DEG C.
In a preferred embodiment of the present invention, described catalyst dissolution liquid is that cobalt phthalocyanine is dissolved in the mixed liquor of hydrophobic ionic liquid with the mass ratio of 1:80～120.
In a preferred embodiment of the present invention, in described step (4), described diluted acid is dilute hydrochloric acid or dilute sulfuric acid.
The invention has the beneficial effects as follows: a kind of method utilizing polystyrene foam to prepare Nitrodracylic acid of the present invention, easy and simple to handle, easily realizing, it is with waste polystyrene foam as raw material, utilizes nitric acid to clear up the method with dioxygen oxidation, on the one hand turn waste into wealth, reduce cost of material, on the other hand efficiently solve the problem directly utilizing the seriously corroded that nitric acid oxidation causes, and the purity of product is high, productivity is big, and product is easily isolated process.
Detailed description of the invention
Below presently preferred embodiments of the present invention is described in detail, so that advantages and features of the invention can be easier to be readily appreciated by one skilled in the art, thus protection scope of the present invention is made apparent clear and definite defining.
The embodiment of the present invention includes:
Present invention is disclosed a kind of method utilizing polystyrene foam to prepare Nitrodracylic acid, it is with waste polystyrene foam as raw material, utilizes nitric acid to carry out micro-wave digestion process, and recycling oxygen carries out catalysis oxidation, prepares Nitrodracylic acid.
Concrete preparation process is as follows.
Embodiment 1
(1) defoaming treatment: after waste and old polystyrene foam cleaning-drying, is called for short fritter, is subsequently adding in hot froth breaker, defoaming treatment 1～3h at 60～80 DEG C, makes foam volume narrow down to original 1/30, takes out and pulverize；
(2) micro-wave digestion: the polystyrene foam after defoaming treatment in step (1) is added in microwave dissolver, it is simultaneously introduced the salpeter solution that mass concentration is 60～65% accounting for polystyrene foam quality 1～2 times, under conditions of 220～250 DEG C and 20～25MPa, carries out micro-wave digestion process 3～5min；
(3) catalysis oxidation: the mixture after micro-wave digestion in step (2) is carried out filter pressing, take filtrate and insert in reactor, then the catalyst dissolution liquid accounting for filtrate volume 2～5 times is added, after mix homogeneously, pour oxysome to reacting kettle inner pressure and reach 1～2MPa, last reaction 8～10h in the water bath with thermostatic control environment of 120 DEG C, reaction is cooled to room temperature after terminating；Wherein, catalyst dissolution liquid is that cobalt phthalocyanine is dissolved in [OMIM] BF with the mass ratio of 1:80～1206The mixed liquor of ionic liquid；
(4) separation and purification of products: add deionized water stirring layering in step (3) in reacted mixed liquor, take the supernatant and be added thereto to the dilute hydrochloric acid of 2mol/L or the dilution heat of sulfuric acid of 0.5～1mol/L to acid, then sucking filtration, vacuum drying, obtain described Nitrodracylic acid.
After tested, product purity is higher than 98% to the Nitrodracylic acid that said method obtains, and productivity is more than 55%.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalent structure utilizing description of the invention content to be made or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, the most in like manner it is included in the scope of patent protection of the present invention.
Claims (6)
1. one kind utilizes the method that polystyrene foam prepares Nitrodracylic acid, it is characterised in that comprise the steps:
(1) defoaming treatment: polystyrene foam is added in hot froth breaker, defoaming treatment 1～3h at 60～80 DEG C, make foam volume narrow down to original 1/30, then take out pulverizing；
(2) micro-wave digestion: the polystyrene foam after defoaming treatment in step (1) is added in microwave dissolver, is simultaneously introduced a certain amount of salpeter solution, carries out micro-wave digestion process under uniform temperature and pressure；
(3) catalysis oxidation: the mixture after micro-wave digestion in step (2) is carried out filter pressing, take filtrate and insert in reactor, then a certain amount of catalyst dissolution liquid is added, after mix homogeneously, pour oxysome to reacting kettle inner pressure and reach 1～2MPa, finally carrying out isothermal reaction 8～10h in the water bath of uniform temperature, reaction is cooled to room temperature after terminating；
(4) separation and purification of products: add deionized water stirring layering in step (3) in reacted mixed liquor, takes the supernatant and is added thereto to dilute acid soln extremely acidity, then sucking filtration, vacuum drying, obtaining described Nitrodracylic acid.
The method utilizing polystyrene foam to prepare Nitrodracylic acid the most according to claim 1, it is characterised in that in described step (2), the mass concentration of described salpeter solution is 60～65%, its addition is 1～2 times of described polystyrene foam quality.
The method utilizing polystyrene foam to prepare Nitrodracylic acid the most according to claim 1, it is characterised in that in described step (2), the temperature of described micro-wave digestion is 220～250 DEG C, and pressure is 20～25MPa, and the time is 3～5min.
The method utilizing polystyrene foam to prepare Nitrodracylic acid the most according to claim 1, it is characterised in that in described step (3), addition is filtrate volume 2～5 times of described catalyst dissolution liquid；Described reaction temperature is 120 DEG C.
The method utilizing polystyrene foam to prepare Nitrodracylic acid the most according to claim 4, it is characterised in that described catalyst dissolution liquid is that cobalt phthalocyanine is dissolved in the mixed liquor of hydrophobic ionic liquid with the mass ratio of 1:80～120.
The method utilizing polystyrene foam to prepare Nitrodracylic acid the most according to claim 1, it is characterised in that in described step (4), described diluted acid is dilute hydrochloric acid or dilute sulfuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610449944.6A CN106008220A (en) | 2016-06-21 | 2016-06-21 | Method for preparing p-nitrobenzoic acid through polystyrene foam |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610449944.6A CN106008220A (en) | 2016-06-21 | 2016-06-21 | Method for preparing p-nitrobenzoic acid through polystyrene foam |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108658777A (en) * | 2018-06-14 | 2018-10-16 | 四川武胜春瑞医药化工有限公司 | A kind of synthetic method of paranitrobenzoic acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407464A (en) * | 2008-11-27 | 2009-04-15 | 南京工业大学 | Method for preparing p-nitrobenzoic acid from waste polystyrene |
| CN101525292A (en) * | 2009-04-02 | 2009-09-09 | 华东师范大学 | Preparation method of paranitrobenzoic acid |
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- 2016-06-21 CN CN201610449944.6A patent/CN106008220A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407464A (en) * | 2008-11-27 | 2009-04-15 | 南京工业大学 | Method for preparing p-nitrobenzoic acid from waste polystyrene |
| CN101525292A (en) * | 2009-04-02 | 2009-09-09 | 华东师范大学 | Preparation method of paranitrobenzoic acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108658777A (en) * | 2018-06-14 | 2018-10-16 | 四川武胜春瑞医药化工有限公司 | A kind of synthetic method of paranitrobenzoic acid |
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Application publication date: 20161012 |