CN104371371A

CN104371371A - Manufacturing process of disperse orange composition

Info

Publication number: CN104371371A
Application number: CN201410549918.1A
Authority: CN
Inventors: 邱成顺; 章华生
Original assignee: HANGZHOU YUTIAN TECHNOLOGY Co Ltd
Current assignee: HANGZHOU YUTIAN TECHNOLOGY Co Ltd
Priority date: 2014-10-16
Filing date: 2014-10-16
Publication date: 2015-02-25

Abstract

The invention belongs to the process production technical field, relates to a manufacturing process of a disperse dye, and especially relates to a manufacturing process of a disperse orange composition. The manufacturing process of the disperse orange composition comprises the following steps: a, diazotization; b, coupling; and c, press filtration. The manufacturing process has the advantages that through the three steps of diazotization, coupling and press filtration, the preparation of the disperse orange is completed, the entire manufacturing process steps are simplified, the time required for manufacturing is shortened, the production efficiency is improved, besides, the product optimal rate is high, and emissions are cut short. In addition, all data after the product is finished can meet the product requirements, a full reaction can be achieved in a process of adding sodium nitrite, and incomplete reactions and other phenomena are avoided.

Description

DISPERSE ORANGE 30 200 composition manufacturing process

Technical field

The invention belongs to process production techniques field, relate to a kind of manufacturing process of dispersed dye, especially a kind of DISPERSE ORANGE 30 200 composition manufacturing process.

Background technology

Dispersed dye are the water-soluble lower nonionic dyes of a class.The earliest for the dyeing of cellulose acetate fibre, be called cellulose acetate dye.Along with the development of synthon, polyamide fibre, terylene occur in succession, especially terylene, high owing to having permutation degree, the characteristics such as fiber gap is few, and hydrophobicity is strong, and will make swelling of fiber having under carrier or high temperature, thermosol, dyestuff just can enter fiber and upper dye.Therefore, new requirement is proposed to dyestuff, namely require the dyestuff with better hydrophobicity and certain dispersiveness and resistance to distillation etc.Along with the Change and Development in market, being in great demand of the burnt-out printing process products such as sofa backrest conventional in hotel, restaurant, hotel, meeting room and handrail, quilt cover, sheet, curtain, the tablecloth, tea-cloth, clothes.Although current DISPERSE ORANGE 30 200 manufacturing processed can meet existing market to a certain extent, the manufacturing process product strength of DISPERSE ORANGE 30 200 is low, and yield is low, and the discharge of wastewater of unit commodity is high.

Summary of the invention

The object of the invention is for the problems referred to above, provide one to enhance productivity, the excellent rate of product is high, decreases the DISPERSE ORANGE 30 200 composition manufacturing process of sewage discharge simultaneously.

For achieving the above object, present invention employs following technical proposal: DISPERSE ORANGE 30 200 composition manufacturing process, is characterized in that, comprise the following steps,

A, diazotization:

1) in coupling pot, add water, open and stir, add sulfuric acid, p-Nitroaniline, making beating 2-4 hour;

2) in Sodium Nitrite dissolving pan, add water, open and stir, add Sodium Nitrite, be stirred to Sodium Nitrite entirely molten, stop stirring, stand-by;

3) after p-Nitroaniline beating time arrives, be on the rocksly cooled to-10 DEG C--7 DEG C, start to add sodium nitrite solution, after adding Sodium Nitrite, control temperature is below 5 DEG C, adds sodium nitrite solution with 1-2 hour;

4) after Sodium Nitrite finishes, insulation reaction 2-4 hour, test doazo reaction is to terminal;

B, coupling:

1) in diazonium, add sulfuric acid, urea, OP-10 successively, stir 10-20 minute, add benzyl thing, control temperature is little of reaction end at 33 DEG C of-36 DEG C of insulated and stirred reaction 19-21;

2) be warming up to 68 DEG C-71 DEG C, be incubated 1 hour;

C, press filtration: pressure filter thrown into by the material that coupling is good, washing, dries up, discharging; So that filter cake quality index: HPLC >=89%; Intensity >=500%; PH >=3; Solid content >=40%; Coloured light: microstage (doing monochromatic requirement).

In above-mentioned DISPERSE ORANGE 30 200 composition manufacturing process, described benzyl thing is N-cyanoethyl-Phenhenzamine, and HPLC purity >=93%.

In above-mentioned DISPERSE ORANGE 30 200 composition manufacturing process, described OP-10 and alkylphenol polyoxyethylene, its quality control index is: outward appearance is light yellow or yellow paste; PH is 6-7; Cloud point 50-55 DEG C; Moisture content≤1.0%;

In above-mentioned DISPERSE ORANGE 30 200 composition manufacturing process, in described step diazo process, added sodium nitrite solution with 1-2 hour, usually added by slug flow.

In above-mentioned DISPERSE ORANGE 30 200 composition manufacturing process, total nitrogen content >=46.5% of described urea.

Compared with prior art, the invention has the advantages that: by diazotization, coupling, press filtration, three steps complete the preparation of DISPERSE ORANGE 30 200, achieve the simplification of whole process steps, shorten the time needed for manufacture, improve production efficiency, the excellent rate of product is high simultaneously, reduces discharge.In addition, the every data after finished product all can reach product requirement, and the process adding Sodium Nitrite can realize it and react fully, avoid some reactions phenomenon such as insufficient.

Embodiment

Below in conjunction with the chart in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.

Embodiment one

DISPERSE ORANGE 30 200 composition manufacturing process, comprises the following steps a, diazotization:

1) in coupling pot, add water, open and stir, add sulfuric acid, p-Nitroaniline, pull an oar 2 hours;

3) after p-Nitroaniline beating time arrives, be on the rocksly cooled to-10 DEG C, start to add sodium nitrite solution,

After adding Sodium Nitrite, control temperature is below 5 DEG C, adds sodium nitrite solution with 1 hour;

4) after Sodium Nitrite finishes, insulation reaction 2 hours, test doazo reaction is to terminal;

Diazotization allocation sheet:

B, coupling:

1) in diazonium, add total nitrogen content >=46.5% of sulfuric acid, urea, urea successively, OP-10, OP ?10 i.e. alkylphenol polyoxyethylene, its quality control index is: outward appearance is light yellow or yellow paste; PH is 6; Cloud point (1% aqueous solution) 50 DEG C; Moisture content≤1.0%; Add rear stirring 10 minutes, add benzyl thing, described benzyl thing is N ?cyanogen second base ?N ?benzylaniline, and HPLC purity >=93%, and temperature processed reacts 19 little of reaction end 33 DEG C of insulated and stirred;

2) be warming up to 68 DEG C, be incubated 1 hour;

The allocation sheet of coupling:

Embodiment two

1) in coupling pot, add water, open and stir, add sulfuric acid, p-Nitroaniline, making beating 4 is little

Time;

3) after p-Nitroaniline beating time arrives, be on the rocksly cooled to-7 DEG C, start to add sodium nitrite solution, after adding Sodium Nitrite, control temperature is below 5 DEG C, adds sodium nitrite solution with 2 hours;

4) after Sodium Nitrite finishes, insulation reaction 4 hours, test doazo reaction is to terminal;

Diazotization allocation sheet:

B, coupling:

1) in diazonium, add total nitrogen content >=46.5% of sulfuric acid, urea, urea successively, OP-10, OP ?10 i.e. alkylphenol polyoxyethylene, its quality control index is: outward appearance is light yellow or yellow paste; PH is 7; Cloud point (1% aqueous solution) 55 DEG C; Moisture content≤1.0%; Add rear stirring 20 minutes, add benzyl thing, described benzyl thing is N ?cyanogen second base ?N ?benzylaniline, and HPLC purity >=93%, and temperature processed reacts 21 little of reaction end 36 DEG C of insulated and stirred;

2) be warming up to 71 DEG C, be incubated 1 hour;

The allocation sheet of coupling:

Embodiment three

5) in coupling pot, add water, open and stir, add sulfuric acid, p-Nitroaniline, pull an oar 3 hours;

6) in Sodium Nitrite dissolving pan, add water, open and stir, add Sodium Nitrite, be stirred to Sodium Nitrite entirely molten, stop stirring, stand-by;

7) after p-Nitroaniline beating time arrives, be on the rocksly cooled to-9 DEG C, start to add sodium nitrite solution, after adding Sodium Nitrite, control temperature is at 4 DEG C, adds sodium nitrite solution with 1.5 hours;

8) after Sodium Nitrite finishes, insulation reaction 3 hours, test doazo reaction is to terminal;

Diazotization allocation sheet:

B, coupling:

3) in diazonium, add total nitrogen content >=46.5% of sulfuric acid, urea, urea successively, OP-10, OP ?10 i.e. alkylphenol polyoxyethylene, its quality control index is: outward appearance is light yellow or yellow paste; PH is 6.5; Cloud point (1% aqueous solution) 50-55 DEG C; Moisture content≤1.0%; Add rear stirring 15 minutes, add benzyl thing, described benzyl thing is N ?cyanogen second base ?N ?benzylaniline, and HPLC purity >=93%, and temperature processed reacts 20 little of reaction end 35 DEG C of insulated and stirred;

4) be warming up to 69 DEG C, be incubated 1 hour;

The allocation sheet of coupling:

The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims

1. DISPERSE ORANGE 30 200 composition manufacturing process, is characterized in that, comprises the following steps,

A, diazotization:

In coupling pot, add water, open and stir, add sulfuric acid, p-Nitroaniline, making beating 2-4 hour;

In Sodium Nitrite dissolving pan, add water, open and stir, add Sodium Nitrite, be stirred to Sodium Nitrite entirely molten, stop stirring, stand-by;

After p-Nitroaniline beating time arrives, be on the rocksly cooled to-10 DEG C--7 DEG C, start to add sodium nitrite solution, after adding Sodium Nitrite, control temperature is below 5 DEG C;

After Sodium Nitrite finishes, insulation reaction 2-4 hour, test doazo reaction is to terminal;

B, coupling:

In diazonium, add sulfuric acid, urea, OP-10 successively, stir 10-20 minute, add benzyl thing, control temperature is little of reaction end at 33 DEG C of-36 DEG C of insulated and stirred reaction 19-21;

Be warming up to 68 DEG C-71 DEG C, be incubated 1 hour;

C, press filtration: pressure filter thrown into by the material that coupling is good, washing, dries up, discharging; So that filter cake quality index: HPLC >=89%; Intensity >=500%; PH >=3; Solid content >=40%.

2. according to the DISPERSE ORANGE 30 200 composition manufacturing process described in claim 1, it is characterized in that, described benzyl thing is N-cyanoethyl-Phenhenzamine, and HPLC purity >=93%.

3. according to the DISPERSE ORANGE 30 200 composition manufacturing process described in claim 1, it is characterized in that, described OP-10 and alkylphenol polyoxyethylene, its quality control index is: outward appearance is light yellow or yellow paste; PH is 6-7; Cloud point 50-55 DEG C.

4., according to the DISPERSE ORANGE 30 200 composition manufacturing process described in claim 1, it is characterized in that, total nitrogen content >=46.5% of described urea.

5. according to the DISPERSE ORANGE 30 200 composition manufacturing process described in claim 3, it is characterized in that, described OP-10 and the moisture controlled of alkylphenol polyoxyethylene are ≤1.0%.

6. according to the DISPERSE ORANGE 30 200 composition manufacturing process described in claim 1, it is characterized in that, in described step diazo process, added sodium nitrite solution with 1-2 hour, usually added by slug flow.