CN101705017A - Orange reactive dye for wool and preparation method thereof - Google Patents
Orange reactive dye for wool and preparation method thereof Download PDFInfo
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- CN101705017A CN101705017A CN200910228206A CN200910228206A CN101705017A CN 101705017 A CN101705017 A CN 101705017A CN 200910228206 A CN200910228206 A CN 200910228206A CN 200910228206 A CN200910228206 A CN 200910228206A CN 101705017 A CN101705017 A CN 101705017A
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Abstract
The invention discloses an orange reactive dye for wool and a preparation method thereof. The orange reactive dye for the wool is a compound having a general formula (I) structure as follows. The usage and the preparation for the dye can reduce environmental pollution; and the orange reactive dye for wool is characterized by low cost of raw materials, high product solubility, bright color, excellent application performance, convenient use and strong applicability.
Description
Technical field
The present invention relates to a kind of reactive dye for wool and preparation method thereof, particularly relate to a kind of orange reactive dye for wool and preparation method thereof.
Background technology
Now general dyeing wool, cashmere, used dyestuff are matching stain, acid mordant dye and metallized dye.Because with the material that these kinds of dyes are dyed, fastness is all not good enough, coloured light is not really gorgeous, but also can cause trouble to environmental protection.Enter 21 century, because the restriction of environmental ecology is more and more higher for the requirement of dye uptake, degree of fixation and dyeing waste-water.Matching stain can not satisfy development of times again.
Technical problem to be solved by this invention is, provides one can reduce environmental pollution, and the desired raw material cost is low, the product solubility height, and also bright in colour, the application performance excellence, easy to use, orange reactive dye for wool that suitability is strong and preparation method thereof.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of orange reactive dye for wool, this orange reactive dye for wool is the compound with following general formula (I) structure:
The preparation method of the dye composition of said structure formula (I) comprises the steps:
The dissolving of a, J acid
Transferring the pH of J acid solution with sodium hydroxide solution is 6.5-7.0, and the mass/volume concentration of adjusting solution is 7.5%, gets the J acid solution;
B, condensation reaction
Adjusting J acid solution mass/volume concentration is 6%, keeps pH=6~6.5 with sodium bicarbonate, 5~10 ℃ of temperature, and 40~60 minutes times spent, add 2,3-two bromo propionyl chloros and acetone mixed solution reacted 1-3 hour, got condensated liquid.
C, diazotization reaction
Sulfonation para-ester is dissolved in the water, and the regulator solution temperature is less than 0 ℃, and the pH that keeps solution with hydrochloric acid adds Sodium Nitrite fast less than 2, keeps 0~5 ℃ of reaction of temperature 1-3 hour, eliminates excessive nitrous acid with thionamic acid, diazonium liquid,
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, holding temperature 10-30 ℃, keep pH=5-8, reacted 3-5 hour coupling solution.
E, neutralization reaction
Coupling solution is adjusted to pH=6-6.5 with hydrochloric acid soln, stirred 10-20 minute.
F, drying
With dry formula (I) compound that gets of the solution spray of e step.
Preferably, the preparation method of the dye composition of said structure formula (I) comprises the steps:
The dissolving of a, J acid
With water dissolution J acid, transfer pH=6.5-7 with sodium hydroxide solution then, make material dissolution, clarification, the mass/volume concentration of adjusting solution is 7.5%, gets the J acid solution;
B, condensation reaction
Under 5~7 ℃ of temperature, adjusting J acid solution mass/volume concentration is 6%, keep pH=6~6.5 with sodium bicarbonate, 5~10 ℃ of temperature, 40~60 minutes times spent, add 2,3-two bromo propionyl chloros and acetone mixed solution, 5~10 ℃ of holding temperatures and pH value 6~6.5 were reacted 1-3 hour, got condensated liquid.
C, diazotization reaction
Sulfonation para-ester is dissolved in the water, adding hydrochloric acid, the regulator solution temperature is less than 0 ℃, and the pH that keeps solution adds Sodium Nitrite fast less than 2, keeps 0~5 ℃ of reaction of temperature 1-3 hour, eliminates excessive nitrous acid with thionamic acid, gets diazonium liquid,
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, and transfers pH=7 with yellow soda ash, is warmed up to 10 ℃, holding temperature 10-30 ℃, keep pH=5-8, reacted 3-5 hour coupling solution.
E, neutralization reaction
Coupling solution is adjusted to pH=6-6.5 with hydrochloric acid soln, stirred 10-20 minute.
F, drying
With dry formula (I) compound that gets of the solution spray of e step.
More preferably, the preparation method of the dye composition of said structure formula (I) comprises the steps:
The dissolving of a, J acid
In beaker, add water, add 100%J acid then, stir down and transfer pH=6.5-7, make material dissolution with 30% sodium hydroxide solution, clarification, the volume of adjustment solution, the mass/volume concentration that makes solution is 7.5% J acid solution.
B, condensation reaction
Adjust J acid solution temperature to 5~7 ℃ with direct ice and water, adjusting liquor capacity concentration is 6%, keep pH=6~6.5 with sodium bicarbonate then, with 5~10 ℃ of direct ice holding temperatures, 40~60 minutes times spent are with 2 of suitable moles mass, 3-two bromo propionyl chloros and acetone mixed solution add, 5~10 ℃ of holding temperatures and pH value 6~6.5 were reacted 1-3 hour, got condensated liquid.
C, diazotization reaction
In beaker, add water, add sulfonation para-ester then, stirred 10-20 minute.30% hydrochloric acid soln is added, adjust solution temperature less than 0 ℃ with direct ice, adjusting mass/volume concentration is 5.5%, under reaction soln guarantees that the pH value is less than 2 condition, 30% sodium nitrite solution of suitable moles mass is added 0~5 ℃ of holding temperature fast, reacted 1-3 hour, eliminate excessive nitrous acid with thionamic acid, get diazonium liquid
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, and transfers pH=7 with yellow soda ash, is warmed up to 10 ℃, and holding temperature 10-30 ℃, keep pH=5-8, reacted 3-5 hour.
E, neutralization reaction
Coupled reaction liquid is adjusted to pH=6-6.5 with 30% hydrochloric acid soln, stirred 10-20 minute.
F, drying
The look liquid of e step is joined in the feed liquid preheater, adjust the spray tower inlet temperature and carry out spraying drying, obtain product.
In the aforesaid method, J acid is the abbreviation of 2-amino-5-naphthols-7-sulfonic acid or 6-amino-1-naphthols-3-sulfonic acid.
Its structural formula is as follows:
The chemistry of sulfonation para-ester is called 4-β-ethyl sulfuryl sulfate ester aniline-2-sulfonic acid, and its structural formula is as follows:
Aforesaid method and hereinafter in the method for embodiment, the unit of mass/volume concentration is grams per milliliter (g/ml) or thousand/liter (kg/L).
Used various raw materials all can be bought from the market and obtain in the aforesaid method.
Using and preparing of the compound of the present invention's preparation can reduce environmental pollution, and the desired raw material cost is low, the product solubility height, and lovely luster, the application performance excellence, easy to use, be the strong orange reactive dye for wool of a kind of suitability.
Embodiment
The following examples just to the explanation of technical scheme of the present invention, do not form any restriction to technical scheme of the present invention and protection domain.
Embodiment 1
The dissolving of a, J acid
In 500 ml beakers, add 200 milliliters in water, add 100%J acid 23.9 grams then, stir down and transfer pH=6.5-7, make material dissolution, clarification with 30% sodium hydroxide solution.The volume of adjusting solution is 319 milliliters.The mass/volume concentration that makes solution is 7.5%
B, condensation reaction
Adjust J acid solution temperature to 5~7 ℃ with direct ice and water, adjusting solution quality/volumetric concentration is 6%, follow 96% sodium bicarbonate to keep pH=6~6.5 then, with 5~10 ℃ of direct ice holding temperatures, 50 minutes times spent, with 100% 2,3-two bromo propionyl chloros 32.6 gram and the adding of acetone mixed solution, 5~10 ℃ of holding temperatures and pH value 6~6.5, react 2 hours must condensated liquid.
C, diazotization reaction
In 800 ml beakers, add 200 milliliters in water, then 100% sulfonation para-ester, 36.1 grams are added, stirred 15 minutes.Again 15.8 grams, 30% hydrochloric acid soln is added.Adjust solution temperature less than 0 ℃ with direct ice, adjusting mass/volume concentration is 5.5%, under reaction soln guarantees that the pH value is less than 2 condition, with 100% Sodium Nitrite, 7.04 grams, is made into 30% sodium nitrite solution and adds fast.0~5 ℃ of holding temperature was reacted 2 hours, eliminated excessive nitrous acid with thionamic acid, got diazonium liquid
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, and transfers pH=7 with 96% yellow soda ash, is warmed up to 20 ℃, and holding temperature 20-30 ℃, keep pH=7-7.5, reacted 4 hours.
E, neutralization reaction
Coupled reaction liquid is adjusted to pH=6-6.5 with 30% hydrochloric acid soln, stirred 15 minutes.
F, drying
The look liquid of e step is joined in the feed liquid preheater, adjust the spray tower inlet temperature and carry out spraying drying.Get the orange dye of following formula structure:
The orange reactive dye for wool application performance of the embodiment of the invention 1 preparation is as shown in the table:
Compound of the present invention and preparation method thereof is described by specific embodiment.Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, processing condition and realize corresponding other purpose, its relevant change does not all break away from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and all be regarded as comprising within the scope of the present invention.
Claims (4)
2. the preparation method of dyestuff according to claim 1, this method comprises the steps:
The dissolving of a, J acid
Transferring the pH of J acid solution with sodium hydroxide solution is 6.5-7.0, and the mass/volume concentration of adjusting solution is 7.5%, gets the J acid solution;
B, condensation reaction
Adjusting J acid solution mass/volume concentration is 6%, keeps pH=6~6.5 with sodium bicarbonate, 5~10 ℃ of temperature, and 40~60 minutes times spent, add 2,3-two bromo propionyl chloros and acetone mixed solution reacted 1-3 hour, got condensated liquid;
C, diazotization reaction
Sulfonation para-ester is dissolved in the water, and the regulator solution temperature is less than 0 ℃, and the pH that keeps solution with hydrochloric acid adds Sodium Nitrite fast less than 2, keeps 0~5 ℃ of reaction of temperature 1-3 hour, eliminates excessive nitrous acid with thionamic acid, diazonium liquid,
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, holding temperature 10-30 ℃, keep pH=5-8, reacted 3-5 hour coupling solution;
E, neutralization reaction
Coupling solution is adjusted to pH=6-6.5 with hydrochloric acid soln, stirred 10-20 minute;
F, drying
With dry formula (I) compound that gets of the solution spray of e step.
3. method according to claim 2, this method comprises the steps:
The dissolving of a, J acid
With water dissolution J acid, transfer pH=6.5-7 with sodium hydroxide solution then, make material dissolution, clarification, the mass/volume concentration of adjusting solution is 7.5%, gets the J acid solution;
B, condensation reaction
Under 5~7 ℃ of temperature, adjusting J acid solution mass/volume concentration is 6%, keep pH=6~6.5 with sodium bicarbonate, 5~10 ℃ of temperature, 40~60 minutes times spent, add 2,3-two bromo propionyl chloros and acetone mixed solution, 5~10 ℃ of holding temperatures and pH value 6~6.5 were reacted 1-3 hour, got condensated liquid;
C, diazotization reaction
Sulfonation para-ester is dissolved in the water, adding hydrochloric acid, the regulator solution temperature is less than 0 ℃, and the pH that keeps solution adds Sodium Nitrite fast less than 2, keeps 0~5 ℃ of reaction of temperature 1-3 hour, eliminates excessive nitrous acid with thionamic acid, gets diazonium liquid,
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, and transfers pH=7 with yellow soda ash, is warmed up to 10 ℃, holding temperature 10-30 ℃, keep pH=5-8, reacted 3-5 hour coupling solution;
E, neutralization reaction
Coupling solution is adjusted to pH=6-6.5 with hydrochloric acid soln, stirred 10-20 minute;
F, drying
With dry formula (I) compound that gets of the solution spray of e step.
4. according to claim 2 or 3 described methods, this method comprises the steps:
The dissolving of a, J acid
In beaker, add water, add 100%J acid then, stir down and transfer pH=6.5-7, make material dissolution with 30% sodium hydroxide solution, clarification, the volume of adjustment solution, the mass/volume concentration that makes solution is 7.5% J acid solution;
B, condensation reaction
Adjust J acid solution temperature to 5~7 ℃ with direct ice and water, adjusting liquor capacity concentration is 6%, keep pH=6~6.5 with sodium bicarbonate then, with 5~10 ℃ of direct ice holding temperatures, 40~60 minutes times spent are with 2 of suitable moles mass, 3-two bromo propionyl chloros and acetone mixed solution add, 5~10 ℃ of holding temperatures and pH value 6~6.5 were reacted 1-3 hour, got condensated liquid;
C, diazotization reaction
In beaker, add water, add sulfonation para-ester then, stirred 10-20 minute; 30% hydrochloric acid soln is added, adjust solution temperature less than 0 ℃ with direct ice, adjusting mass/volume concentration is 5.5%, under reaction soln guarantees that the pH value is less than 2 condition, 30% sodium nitrite solution of suitable moles mass is added 0~5 ℃ of holding temperature fast, reacted 1-3 hour, eliminate excessive nitrous acid with thionamic acid, get diazonium liquid
D, coupled reaction
The diazonium liquid that the c step is obtained joins in the condensated liquid that the b step obtains, and transfers pH=7 with yellow soda ash, is warmed up to 10 ℃, and holding temperature 10-30 ℃, keep pH=5-8, reacted 3-5 hour;
E, neutralization reaction
Coupled reaction liquid is adjusted to pH=6-6.5 with 30% hydrochloric acid soln, stirred 10-20 minute;
F, drying
The look liquid of e step is joined in the feed liquid preheater, adjust the spray tower inlet temperature and carry out spraying drying, obtain product.
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CN 200910228206 CN101705017B (en) | 2009-11-16 | 2009-11-16 | Orange reactive dye for wool and preparation method thereof |
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CN 200910228206 CN101705017B (en) | 2009-11-16 | 2009-11-16 | Orange reactive dye for wool and preparation method thereof |
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CN101705017A true CN101705017A (en) | 2010-05-12 |
CN101705017B CN101705017B (en) | 2012-03-14 |
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Address after: 300270 No. 1558 Kaixuan street, Dagang Petrochemical Industrial Park, Binhai New Area, Tianjin Patentee after: Tianjin Dek Chemical Co.,Ltd. Address before: 300163 Tianjin city Dongli District ZhangGuiZhuang road Ji'an Road Patentee before: Tianjin Dek Chemical Co.,Ltd. |
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Effective date of registration: 20230131 Granted publication date: 20120314 |