CN102993772A

CN102993772A - Preparation method of orange reactive dye

Info

Publication number: CN102993772A
Application number: CN2012104203913A
Authority: CN
Inventors: 褚平忠; 孟云龙
Original assignee: Individual
Current assignee: Individual
Priority date: 2011-12-14
Filing date: 2012-10-29
Publication date: 2013-03-27

Abstract

The invention discloses a preparation method of an orange reactive dye. The preparation method comprises the following steps of: 1. primary condensation reaction; 2. secondary condensation; 3. diazo reaction; 4. coupling reaction: adding diazo salt to secondary condensation solution, controlling the temperature to be 0-15 DEG C, then adjusting the PH value to be 5.5-6.5 with 15% of pure alkali solution and diazo salt disappearing after reaction for 3 hours; and 5. third-time condensation: adding 2-aminoethyl-2' sulfonyl hydroxyethyl sulfone sulfate to coupling solution, adjusting the PH value to be 6.5-8.5 with 15% of pure alkali solution, then raising the temperature to 60-80 DEG C, controlling the temperature and the PH value, reacting for 4-5 hours until the finishing point and drying the dye solution, thus obtaining the orange reactive dye.

Description

A kind of preparation method of orange active dye

Technical field

The invention provides a kind of preparation method of orange active dye.

Background technology

The reactive dyestuffs of producing at present are the halo Triazine normally, and phenylethyl sulfone sulfate type or halo triazine and phenylethyl sulfone sulfate mixed type cause more greatly Determinating Chromaticity of Dyeing Effluent large with the salt amount in dyeing course, and environmental pollution is heavy.Secondly dye at present reactive black KN-B(reactive black 5 commonly used when pitch black) with reactive orange KN-GR(REACTIVE ORANGE 12 9) blending forms.Yet the dyestuff pitch black degree that this blending forms is often not ideal enough, again because reactive orange KN-GR is the active group of dichlorotriazine and the avidity height of cellulosic fibre, be adsorbed on first on the fiber, and reactive black KNB colouring is slow, so cause aberration, easily cause the look flower, particularly orange component is easily heavy when adding the alkali fixation carefully separates out, and causes color spot.

Summary of the invention

The invention provides a kind of preparation method of orange active dye, it not only can improve the dye fixing rate, and the performance raising that mixes, and is difficult for causing the look flower, improves pitch black pitch black degree.

The present invention has adopted following technical scheme: a kind of preparation method of orange active dye, it may further comprise the steps: step 1, one contracting reaction: in a contracting bucket, put 150 parts of mixture of ice and water, 18.5 parts of the cyanuric chlorides of adding 100%, 0 ℃ of lower making beating 45-60 minute, then drip 4.2 parts of cyanamide solution of 100%, add 0-5 ℃ of rear control temperature, it is 7-9 that NaOH solution with 10% is regulated PH, conditioned reaction 10-40 minute; Step 2, two contractings: in the dissolving bucket, put into 200 parts, drop into 23.9 parts of 100% J acid, pull an oar after one hour with 10% NaOH liquid adjusting PH5.8-6.5, molten clearly, and adjust volume and control J acid concentration 4-5%, then join in the contracting thing, intensification 35-40 ℃, and to regulate PH with 15% soda ash liquid be 3-6, react 3-4 hour to terminal, it is for subsequent use to be down to normal temperature; Step 3, carry out doazo reaction: in the diazonium bucket, put 100 parts of mixture of ice and water, drop into p-(beta-sulfuric ester ethyl sulfonyl) aniline 100% 28.1 parts, pulled an oar 10 minutes, add 12 parts of industrial goods hydrochloric acid, then add 6.9 parts of sodium nitrite solutions of 100%, control simultaneously temperature 0-5 ℃, finish, control temperature≤10 ℃, the little blue colour response of starch potassium iodide paper was eliminated excessive nitrous acid with thionamic acid after 2 hours; Step 4, coupled reaction: diazonium salt is joined in the two contracting liquid 0-15 ℃ of control temperature; then regulating PH with 15% soda ash liquid is 5.5-6.5; react 3 hours diazonium salts and disappear, step 5, three contractings: 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfone sulfates are joined in the above-mentioned coupling solution; and to regulate PH with 15% soda ash liquid be 6.5-8.5; then be warming up to 60-80 ℃, control temperature and pH value react 4-5 hour to terminal; and with the dye liquor drying, get orange active dye.

Orange active dye in the step 4 of the present invention contains anionic group-SO3H.Orange active dye in the step 4 of the present invention adopts alkali-metal aqueous solution form.

The present invention has following beneficial effect: the present invention introduces new active group 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfone sulfates and the halo triazine is combined into halo triazine and aliphatics ethyl sulfonyl sulfate mixed type reactive dyestuffs; can improve the dye fixing rate; every fastness such as photostabilization, wash resistant, anti-daylight-sweat fastness are good; can carry out colorant match with reactive black KNB on the one hand; the performance that mixes improves; be difficult for causing the look flower, improve pitch black pitch black degree.

Embodiment

The invention provides a kind of preparation method of orange active dye, it may further comprise the steps: step 1, one contracting reaction: in a contracting bucket, put 150 parts of mixture of ice and water, 18.5 parts of the cyanuric chlorides of adding 100%, 0 ℃ of lower making beating 45-60 minute, then drip 4.2 parts of cyanamide solution of 100%, add 0-5 ℃ of rear control temperature, it is 7-9 that NaOH solution with 10% is regulated PH, conditioned reaction 10-40 minute; Step 2, two contractings: in the dissolving bucket, put into 200 parts, drop into 23.9 parts of 100% J acid, pull an oar after one hour with 10% NaOH liquid adjusting PH5.8-6.5, molten clearly, and adjust volume and control J acid concentration 4-5%, then join in the contracting thing, intensification 35-40 ℃, and to regulate PH with 15% soda ash liquid be 3-6, react 3-4 hour to terminal, it is for subsequent use to be down to normal temperature; Step 3, carry out doazo reaction: in the diazonium bucket, put 100 parts of mixture of ice and water, drop into p-(beta-sulfuric ester ethyl sulfonyl) aniline 100% 28.1 parts, pulled an oar 10 minutes, add 12 parts of industrial goods hydrochloric acid, then add 6.9 parts of sodium nitrite solutions of 100%, control simultaneously temperature 0-5 ℃, finish, control temperature≤10 ℃, the little blue colour response of starch potassium iodide paper was eliminated excessive nitrous acid with thionamic acid after 2 hours; Step 4, coupled reaction: diazonium salt is joined in the two contracting liquid, 0-15 ℃ of control temperature, then regulating PH with 15% soda ash liquid is 5.5-6.5, reacts 3 hours diazonium salts and disappears; Step 5; three contractings: 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfone sulfates are joined in the above-mentioned coupling solution; and to regulate PH with 15% soda ash liquid be 6.5-8.5; then be warming up to 60-80 ℃, control temperature and pH value react 4-5 hour to terminal; and with the dye liquor drying; get orange active dye, orange active dye contains anionic group-SO3H, and orange active dye adopts alkali-metal aqueous solution form.

Claims

1. the preparation method of an orange active dye, it may further comprise the steps:

Step 1, one contracting reaction: in a contracting bucket, put 150 parts of mixture of ice and water, 18.5 parts of the cyanuric chlorides of adding 100%, 0 ℃ of lower making beating 45-60 minute, then drip 4.2 parts of cyanamide solution of 100%, add 0-5 ℃ of rear control temperature, it is 7-9 that the NaOH solution with 10% is regulated PH, conditioned reaction 10-40 minute;

Step 2, two contractings: in the dissolving bucket, put into 200 parts, drop into 23.9 parts of 100% J acid, pull an oar after one hour with 10% NaOH liquid adjusting PH5.8-6.5, molten clearly, and adjust volume and control J acid concentration 4-5%, then join in the contracting thing, intensification 35-40 ℃, and to regulate PH with 15% soda ash liquid be 3-6, react 3-4 hour to terminal, it is for subsequent use to be down to normal temperature;

Step 3, carry out doazo reaction: in the diazonium bucket, put 100 parts of mixture of ice and water, drop into p-(beta-sulfuric ester ethyl sulfonyl) aniline 100% 28.1 parts, pulled an oar 10 minutes, add 12 parts of industrial goods hydrochloric acid, then add 6.9 parts of sodium nitrite solutions of 100%, control simultaneously temperature 0-5 ℃, finish, control temperature≤10 ℃, the little blue colour response of starch potassium iodide paper was eliminated excessive nitrous acid with thionamic acid after 2 hours;

Step 4, coupled reaction: diazonium salt is joined in the two contracting liquid, 0-15 ℃ of control temperature, then regulating PH with 15% soda ash liquid is 5.5-6.5, reacts 3 hours diazonium salts and disappears;

Step 5; three contractings: 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfone sulfates are joined in the above-mentioned coupling solution; and to regulate PH with 15% soda ash liquid be 6.5-8.5; then be warming up to 60-80 ℃; control temperature and pH value; react 4-5 hour to terminal, and with the dye liquor drying, orange active dye got.

2. orange active dye according to claim 1 and preparation method thereof is characterized in that the orange active dye in the step 4 contains anionic group-SO3H.

3. orange active dye according to claim 1 and preparation method thereof is characterized in that the orange active dye in the step 4 adopts alkali-metal aqueous solution form.