CN1100403A

CN1100403A - Iron powder-adding preparation process of 1.5,1.8-diamido naphthalene mixture

Info

Publication number: CN1100403A
Application number: CN 94110239
Authority: CN
Inventors: 黄元海; 洪国胜
Original assignee: JIANGHUI CHEMICAL PLANT YINGKOU
Current assignee: JIANGHUI CHEMICAL PLANT YINGKOU
Priority date: 1994-05-07
Filing date: 1994-05-07
Publication date: 1995-03-22

Abstract

In the said prepn. process, dinitronaphthalene, iron powder, alcohol, water, glacial acetic acid, caustic soda and sodium bisulfite compounded in a certain proportion are passed through mixing, stirring,t emp. raising,t emp. keeping, dilution, separation, filtering and stoving to produce 1.5- and 1.8- diamino naphthalene mixture. Compared with hydrogenating reduction process, the said process has the merits of low cost and high quality.

Description

Iron powder-adding preparation process of 1.5,1.8-diamido naphthalene mixture

The invention belongs to the production method of the intermediate of organic synthesis thing in the chemical field, exactly is the production method of intermediate-1.5, the 1.8 diaminonaphthalene mixture of producing pigment dyestuff, superpolymer in the field of fine chemical.

At present, in Naphtocyclinon dyestuff, superpolymer and the azoic dyestuff of the various coloring plastics of preparation, all need 1.8-diamino naphthalene and 1.5-diaminonaphthalene both at home and abroad.And 1.8-diaminonaphthalene and 1.5-diaminonaphthalene extract in the 1.8-diaminonaphthalene mixture often from 1.5.The production way of this mixture have only Japan, the U.S. two families to produce at present in the world, but its production cost is higher, and its method is the hydrogenating reduction method.

The objective of the invention is new to produce 1.5 for people provide a kind of, the production method of 1.8-diaminonaphthalene is the iron powder reducing preparation method.

The object of the present invention is achieved like this:

At first get material: (part is a weight unit) dinitronaphthalene (130-180) part, iron powder: (260-400) part, alcohol (150-200) part by following prescription, water (150-200), Glacial acetic acid (8-12), caustic soda (7-10) part, sodium bisulfite (1.3-2) part; Then by following requirement preparation: water and alcohol are put into reactor, add Glacial acetic acid again, machine, make it stir revolution and be (75-85) rev/min, add iron powder after the start immediately, feeding steam afterwards heats up, when its heat-up rate waited to rise to 80 ℃ for (20 ℃-80 ℃)/(40-60) divide, insulation (14-16) minute added dinitronaphthalene afterwards in batches, each add (10-15) minute, every (10-15) minute adds once; Feed steam after all adding again and keep 80 ℃-85 ℃, 3-4 hour, stir simultaneously, when treating that its temperature is reduced to 75 ℃ of left and right sides, add caustic soda solution and make its pH value between 8-9; Add sodium bisulfite afterwards, stir after 5 minutes and filter immediately; Be put into afterwards to separate out and add entry (1500-2000) part dilution in the still, afterwards, placed 8-10 hour, filter once more afterwards, send into oven dry in the dryer afterwards, packing is put in storage at last.

After the present invention realizes, be iron powder reducing preparation 1.5, the 1.8-diaminonaphthalene provides a kind of novel method, and present method compares with the hydrogenation preparation method of Japan, the U.S., has that cost is low, the quality advantages of higher.

Embodiment:

Get material by following prescription:

Dinitronaphthalene: 15Kg, iron powder 30Kg, alcohol 20Kg, water 20Kg, Glacial acetic acid 1Kg, caustic soda 1Kg, sodium bisulfite 0.13Kg; Then by following requirement preparation: with water, alcohol is put into reactor, add Glacial acetic acid, afterwards, machine, make it stir revolution and be (75-85) rev/min, add iron powder after the start immediately, feed steam afterwards and heat up, its heat-up rate (20 ℃-80)/(40-60) divides, when waiting to rise to 80 ℃, insulation (14-16) minute, add dinitronaphthalene afterwards in batches, add 1.2Kg at every turn, added once in per 12 minutes, after treating all to add, feed steam again and be warming up to 82 ℃, be incubated 3.5 hours, stir simultaneously, when treating that its temperature is reduced to 75 ℃ of left and right sides, it is 9 that the adding caustic soda solution makes its pH value; Add sodium bisulfite afterwards, stir after 5 minutes, filter immediately, afterwards, put into and separate out the dilution of still adding 180Kg water, placed afterwards 9 hours; Filter afterwards, and send into oven dry in the dryer, at last the packing warehouse-in.

Claims

A kind of iron powder reducing produces 15, the processing method of 18--diaminonaphthalene mixture, its thing is levied and is dinitronaphthalene (130-180) part, iron powder (260-400) part, alcohol (150-200) part, water (150-200) part, Glacial acetic acid (8-12) part, caustic soda (7-10) part, sodium bisulfite (1.3-2) part; Prepare by following requirement: water and alcohol are put into reactor, add Glacial acetic acid again, machine, make it stir revolution and be (75-85) rev/min, add iron powder after the start immediately, feed steam afterwards and heat up, its heat-up rate is that (20 ℃-80 ℃)/(40-60) divide, when waiting to rise to 80 ℃, insulation (14-16) minute, add dinitronaphthalene afterwards in batches, each adding (10-15) part, and every (10-15) minute adding is once; Feed steam again after adding and be warming up to 80 ℃-85 ℃, be incubated 3-4 hour afterwards, stir simultaneously, when treating that its temperature is reduced to 75 ℃ of left and right sides, add caustic soda, solution makes its pH value between 8-9; Add sodium bisulfite afterwards, stir after 5 minutes and filter immediately; Be put into afterwards and separate out adding (1500-2000) part water dilution in the still, placed afterwards 8-10 hour, filter once more afterwards, send into afterwards in the dryer and dry, at last the packing warehouse-in.