CN1250768A - Process for preparing anthracene, phenanthrene and karbazole - Google Patents

Abstract

The raw material crude anthracene is loaded into the reaction still of xylene solvent to obtain a mixture of anthracene and carbazole; the mixture is added to the cauldron of potassium solution to further obtain anthracene (A), phenanthrene (P) and carbazole (C); (A) and (P) are further added to the normal-pressure evaporation cauldron to obtain white mixture of (A) and (P); the white mixture is loaded into the reaction still of xylene solvent to obtain the products of (A) and (P); (C) is added to the reaction still with water to obtain (C) filter cake; the filter cake is added to the evaporation cauldron to obtain crude (C); the crude (C) is added to the reaction still of xylene solvent, and can be obtd. after reaction. By use of one set of process, three products are simultaneosly obtd. with low cost and high purity.

Description

The preparation method of anthracene, phenanthrene, carbazole

The present invention relates to the preparation method of a kind of anthracene, non-, carbazole, the present invention especially relates to a kind of method of utilizing a cover typical process flow to produce anthracene, phenanthrene, carbazole simultaneously.

Anthracene, phenanthrene, carbazole belong to the Coal Chemical Industry fine product, are that the crude anthracene with coal tar is a raw material, through operations such as overheated filter, chemical separation, steaming liter and solvent washs and make.

The traditional technology of producing anthracene, phenanthrene, carbazole is to utilize solvent method, distillation method, chemical method and subliming method to produce.More than four kinds of production methods have following defective, mainly show:

The first, every cover technology can only be produced a kind of product;

The second, complex process, operation easier is big:

As adopt solvent method: need with 4 kinds of solvents, as producing anthracene, phenanthrene, three kinds of products of carbazole, washing times will reach 20 times;

As adopt distillation method: pipeline stops up easily, thereby produces pressure, causes to fire;

As adopt chemical method: be that high-temperature material directly is drained in the solvent, easily cause sharply and be heated, boil that solvent volatilizees in a large number, pollutes;

As adopt subliming method: the reaction times is oversize, and the easy charing of material yields poorly, the cost height.

The 3rd, product purity is low, and yield is low, unstable product quality;

The 4th, product appearance is poor;

The 5th, investment is big, and loss is big, the cost height;

The 6th, blowdown is many, and toxicity is big, causes serious environmental to pollute.

Purpose of the present invention is exactly at above-mentioned the deficiencies in the prior art, and the preparation method of a kind of anthracene, phenanthrene, carbazole is provided.

1, the preparation method of a kind of anthracene, phenanthrene, carbazole, it comprises the following steps:

(1) the raw material crude anthracene is joined in the reactor that xylene solvent is housed, the ratio of crude anthracene and solvent is 1: 1.2, when being heated to 90-100 ℃, all dissolvings, mixture after the dissolving enters in the crystallizing pan that has filter cylinder, and filtrate is through crystallisation by cooling, to 28-32 ℃, centrifugation then obtains anthracene, carbazole mixture;

(2) anthracene, carbazole mixture are joined in the molten still of the potassium that potassium hydroxide is housed, ratio is 3: 1, reacting by heating is to 200-220 ℃, be incubated 2 hours, reaction finishes, this reaction mass entered be cooled to 30 ℃ in the airtight container, open closed cell, take out the carbazole of anthracene, phenanthrene and the lower floor on upper strata respectively;

(3) upper strata anthracene, luxuriant and rich with fragrance mixture are joined the normal pressure steaming and rise in the still, maintain the temperature at 250-270 ℃, anthracene, phenanthrene begin to waft in receiving vat, obtain white anthracene, luxuriant and rich with fragrance mixture;

(4) white anthracene, luxuriant and rich with fragrance mixture are joined in the reactor that xylene solvent is housed, ratio is 1: 2, remains on 90-100 ℃, is incubated 1 hour, is cooled to 30 ℃ again, is drained in the whizzer and separates, and obtains the finished product anthracene; Separate rear filtrate and pack into and distill in the still kettle, temperature is 150-170 ℃, and solvent all steams, and is the finished product phenanthrene at the bottom of the still;

(5) will join in the reactor of band water after lower floor's carbazole pulverizing, the ratio of water and carbazole is 3: 1, directly steams with steam and blows 3 hours, and temperature remains on 80-100 ℃, separates then, obtains the filter cake carbazole;

(6) the filter cake carbazole is joined steam and rises in the still, 250-270 ℃ of maintenance temperature, carbazole begins to waft in the receiving vat, obtains thick carbazole;

(7) thick carbazole is joined in the reactor that xylene solvent is housed, its ratio is 1: 2, remains on 90-100 ℃, is incubated 1 hour, is cooled to 40 ℃ again, is drained in the whizzer and separates, and obtains the finished product carbazole.

The preparation method of anthracene, phenanthrene, carbazole is essentially different than solvent method, distillation method, chemical method and subliming method, and its superiority mainly shows:

The first, utilize a cover technology can produce anthracene, phenanthrene, three kinds of products of carbazole simultaneously;

The second, reduced the solvent usage quantity, reduced production cost;

The 3rd, simplified production technique, schedule of operation is simple;

The 4th, quality product obviously improves, and outward appearance is good, steady quality;

The 5th, shortened the production cycle, the yield height has enlarged throughput;

The 6th, take the fully-closed mode of production, thoroughly eliminated pollution.

The 7th, the various index correlation datas of the present invention:

1, quality standard contrast

2, production cost contrast

3, technical matters contrast

4, gross investment situation contrast

Unit	Gross investment (Renminbi/unit)	Production kind and throughput: ton/year
					Shanghai Baosteel (solvent method)	100,000,000	Anthracene: 400	Carbazole: 200
Dying of Shanghai seven factories (solvent method)	3,000 ten thousand		Carbazole: 100
					The present invention	7,200,000	Anthracene: 1000	Carbazole: 600	Luxuriant and rich with fragrance: 600

Be described in further detail below by embodiment:

1,1000 kilograms of raw material crude anthracenes are joined in the reactor that xylene solvent is housed, the ratio of crude anthracene and solvent is 1: 1.2, and when being heated to 90-100 ℃, all dissolving enters in the crystallizing pan that has filter cylinder; Filtrate process crystallisation by cooling, to 30 ℃, centrifugation then, filter cake is anthracene, carbazole mixture;

2, filter cake is joined in the molten still of potassium, the ratio of filter cake and potassium hydroxide is 3: 1 in the molten still of potassium, reacting by heating to 200 ℃, be incubated 2 hours, reaction finishes, and this reaction mass is entered be cooled to 30 ℃ in the airtight container, open closed cell, take out the carbazole of anthracene, phenanthrene and the lower floor on upper strata respectively;

3, upper strata anthracene, luxuriant and rich with fragrance mixture are joined the normal pressure steaming and rise in the still, maintain the temperature at 260 ℃, anthracene, phenanthrene begin to waft in receiving vat, obtain white anthracene, luxuriant and rich with fragrance mixture;

4, white anthracene, luxuriant and rich with fragrance mixture are joined (ratio is 1: 2) in the reactor that xylene solvent is housed, remain on 90-100 ℃, be incubated 1 hour, be cooled to 30 ℃ again, be drained in the whizzer and separate, obtain 300 kilograms of finished product anthracenes; Filtrate is packed into and is distilled in the still kettle, and temperature is 160 ℃, and solvent all steams, and residue is 150 kilograms of finished product phenanthrene at the bottom of the still;

5, will join in the reactor of band water after lower floor's carbazole pulverizing, the ratio of water and carbazole is 3: 1, directly steams with steam and blows 3 hours, and temperature remains on 90 ℃, separates then, obtains the filter cake carbazole;

6, the filter cake carbazole is joined steaming and rise in the still, keep 260 ℃ of temperature, carbazole begins to waft in the receiving vat; Obtain thick carbazole;

7, thick carbazole is joined in the reactor that xylene solvent is housed, its ratio is 1: 2, remains on 90-100 ℃, is incubated 1 hour, is cooled to 40 ℃ again, is drained in the whizzer and separates, and obtains 150 kilograms of finished product carbazoles.

Claims (1)

1, the preparation method of a kind of anthracene, phenanthrene, carbazole, it comprises the following steps:

(1) the raw material crude anthracene is joined in the reactor that xylene solvent is housed, the ratio of crude anthracene and solvent is 1: 1.2, when being heated to 90-100 ℃, all dissolvings, mixture after the dissolving enters in the crystallizing pan that has filter cylinder, and filtrate is through crystallisation by cooling, to 28-32 ℃, centrifugation then obtains anthracene, carbazole mixture;

(2) anthracene, carbazole mixture are joined in the molten still of the potassium that potassium hydroxide is housed, ratio is 3: 1, reacting by heating is to 200-220 ℃, be incubated 2 hours, reaction finishes, this reaction mass entered be cooled to 30 ℃ in the airtight container, open closed cell, take out the carbazole of anthracene, phenanthrene and the lower floor on upper strata respectively;

(3) upper strata anthracene, luxuriant and rich with fragrance mixture are joined the normal pressure steaming and rise in the still, maintain the temperature at 250-270 ℃, anthracene, phenanthrene begin to waft in receiving vat, obtain white anthracene, luxuriant and rich with fragrance mixture;

(4) white anthracene, luxuriant and rich with fragrance mixture are joined in the reactor that xylene solvent is housed, ratio is 1: 2, remains on 90-100 ℃, is incubated 1 hour, is cooled to 30 ℃ again, is drained in the whizzer and separates, and obtains the finished product anthracene; Separate rear filtrate and pack into and distill in the still kettle, temperature is 150-170 ℃, and solvent all steams, and is the finished product phenanthrene at the bottom of the still;

(5) will join in the reactor of band water after lower floor's carbazole pulverizing, the ratio of water and carbazole is 3: 1, directly steams with steam and blows 3 hours, and temperature remains on 80-100 ℃, separates then, obtains the filter cake carbazole;

(6) the filter cake carbazole is joined steam and rises in the still, 250-270 ℃ of maintenance temperature, carbazole begins to waft in the receiving vat, obtains thick carbazole;

(7) thick carbazole is joined in the reactor that xylene solvent is housed, its ratio is 1: 2, remains on 90-100 ℃, is incubated 1 hour, is cooled to 40 ℃ again, is drained in the whizzer and separates, and obtains the finished product carbazole.