CN101735652B - Red reactive dye and preparation method thereof - Google Patents

Red reactive dye and preparation method thereof Download PDF

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CN101735652B
CN101735652B CN 200910228594 CN200910228594A CN101735652B CN 101735652 B CN101735652 B CN 101735652B CN 200910228594 CN200910228594 CN 200910228594 CN 200910228594 A CN200910228594 A CN 200910228594A CN 101735652 B CN101735652 B CN 101735652B
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张兴华
苏长湘
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天津德凯化工股份有限公司
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Abstract

The invention relates to a red reactive dye for wool and a preparation method thereof. The red reactive dye for the wool is a compound having a structure as the general formula (I) shown in the specification. The use and preparation of the dye can reduce environmental pollution, required raw materials have low cost, the solubility of the product is high, the color is bright, the application performance is excellent, the use is convenient and the red reactive dye for the wool has high adaptivity.

Description

一种红色活性染料及其制备方法 As a red reactive dye and preparation method

技术领域 FIELD

[0001] 本发明涉及一种毛用活性染料及其制备方法,特别是涉及一种毛用红色活性染料及其制备方法。 [0001] The present invention relates to a reactive dye for wool and its preparation method, particularly to a red reactive dye for wool and its preparation method.

背景技术 Background technique

[0002] 现在一般染羊毛、羊绒、所用染料均为酸性染料、酸性媒介染料和金属络合染料。 [0002] Now general dyeing wool, cashmere, the dyes are acid dyes, acid mordant dyes and metal complex dyes. 由于用这些种类染料所染的物料,牢度均欠佳,色光不很艳丽,而且还会给环保造成麻烦。 Because these types of dye-dyed material, fastness are poor, not very bright shade, but can also cause problems for the environment. 进入21世纪,由于环境生态的制约,对于上色率、固色率以及染色废水的更求越来越高。 In the 21st century, due to the environmental and ecological constraints, for color yield, fixation and dyeing wastewater more demand higher and higher. 酸性染料已不能再满足时代的发展。 Acid dyes can no longer meet the times.

[0003] 本发明所要解决的技术问题是,提供一个能减少环境污染,所需原料成本低,产品溶解度高,而且色泽鲜艳,应用性能优异,使用方便,适用性强的毛用红色活性染料及其制备方法。 [0003] The present invention solves the technical problem, to reduce environmental pollution and to provide a desired low cost of raw materials, high solubility, and bright color, superior application performance, ease of use, and applicability of the red reactive dyes wool and methods for their preparation.

发明内容 SUMMARY

[0004] 为了解决上述技术问题,本发明提供了一种毛用红色活性染料,该毛用红色活性染料是具有如下通式(I)结构的化合物: [0004] To solve the above problems, the present invention provides a reactive red dye wool, wool with the red reactive dye compound having structure (I) of the general formula:

[0005] [0005]

Figure CN101735652BD00041

[0006] 上述结构式(I)的染料化合物的制备方法包括如下步骤: [0006] Preparation of a compound of the above formula (I) dyes comprising the steps of:

[0007] a、H酸的溶解 [0007] a, H acid was dissolved

[0008] 用氢氧化钠溶液调H酸溶液的pH为6. 5-7. 0,调整溶液的质量/体积浓度为15%,得H酸溶液; [0008] The pH of the solution adjusted with sodium hydroxide to a solution of the acid H 6 5-70, the solution is adjusted mass / volume concentration of 15%, an acid solution to obtain H.;

[0009] b、缩合反应 [0009] b, a condensation reaction

[0010] 调整H酸溶液质量/体积浓度为10%,用碳酸氢钠维持pH = 6〜6. 5,在温度5〜10°c,用时40〜60分钟,加入2,3-二溴丙酰氯和丙酮混合液,反应1-3小时,得缩合液。 [0010] adjusting the H acid solution mass / volume concentration of 10%, maintaining pH = 6~6. 5 with sodium bicarbonate, at a temperature of 5~10 ° c, when used 40~60 minutes, was added 2,3-dibromopropyl chloride and acetone mixture, the reaction for 1-3 hours to obtain the condensation liquid.

[0011] C、重氮化反应 [0011] C, the diazotization

[0012] 将对位酯溶解于水中,调节溶液温度小于0°C,用盐酸保持溶液的pH小于2,快速加入亚硝酸钠,保持温度0〜5°C反应1-3小时,用氨基磺酸消除过量的亚硝酸,得重氮液, [0012] para-ester was dissolved in water, adjusting the solution temperature is less than 0 ° C, maintaining the solution pH less than 2 with hydrochloric acid, adding sodium nitrite quickly, maintaining the temperature at 0~5 ° C for 1 to 3 hours, with sulfamic to eliminate excess nitrous acid to give a diazo solution,

[0013] d、偶合反应 [0013] d, the coupling reaction

[0014] 将c步骤得到的重氮液加入到b步骤得到的缩合液中,维持温度10_30°C,维持pH=5-8,反应3-5小时得偶合液。 [0014] The diazo solution obtained in step c was added to the condensation solution obtained in step b maintaining the temperature 10_30 ° C, maintaining pH = 5-8, for 3-5 hours to obtain a reaction liquid coupling.

[0015] e、中和反应[0016] 将偶合液用盐酸溶液调整至pH = 6-6. 5,搅拌10-20分钟。 [0015] e, and the reaction [0016] The coupling was washed with hydrochloric acid solution was adjusted to pH = 6-6. 5, stirred for 10-20 minutes.

[0017] f、干燥 [0017] f, dried

[0018] 将e步骤的溶液喷雾干燥得式(I)化合物。 [0018] spraying a solution of the compound of formula e drying step (I). [0019] 优选地,上述结构式(I)的染料化合物的制备方法包括如下步骤: [0019] Preferably, the preparation of a compound of formula (I) dyes comprising the steps of:

[0020] a、H酸的溶解 [0020] a, H acid was dissolved

[0021] 用水溶解H酸,然后用氢氧化钠溶液调pH = 6. 5-7,使物料溶解、澄清,调整溶液的质量/体积浓度为15 %,得H酸溶液; [0021] H acid dissolved in water, and then with a sodium hydroxide solution pH = 6. 5-7, the material was dissolved, a clear, the solution is adjusted mass / volume concentration of 15%, an acid solution to obtain H;

[0022] b、缩合反应 [0022] b, a condensation reaction

[0023] 在温度5〜7°C下,调整H酸溶液质量/体积浓度为10%,用碳酸氢钠维持pH =6〜6. 5,在温度5〜10°C,用时40〜60分钟,加入2, 3-二溴丙酰氯和丙酮混合液,维持温度5〜10°C和pH值6〜6. 5,反应1-3小时,得缩合液。 [0023] at 5~7 ° C, H acid solution to adjust the mass / volume concentration of 10%, with sodium bicarbonate to maintain pH = 6~6. 5, at a temperature of 5~10 ° C, when used 40~60 minutes , was added 2,3-dibromo-propionyl chloride and acetone mixture, maintaining a temperature of 5~10 ° C and pH 6~6. 5, the reaction for 1-3 hours to obtain the condensation liquid.

[0024] C、重氮化反应 [0024] C, the diazotization

[0025] 将对位酯溶解于水中,加入盐酸,调节溶液温度小于0°C ,保持溶液的pH小于2,快速加入亚硝酸钠,保持温度0〜5°C反应1-3小时,用氨基磺酸消除过量的亚硝酸,得重氮液, [0025] para-ester was dissolved in water, hydrochloric acid was added to adjust the solution temperature is less than 0 ° C, maintaining pH of the solution is less than 2, by adding sodium nitrite quickly, maintaining the temperature at 0~5 ° C for 1 to 3 hours, with amino to eliminate excess nitrous acid to give a diazo solution,

[0026] d、偶合反应 [0026] d, the coupling reaction

[0027] 将c步骤得到的重氮液加入到b步骤得到的缩合液中,用碳酸钠调pH = 7,升温到IO0C,维持温度10-30°C,维持pH = 5-8,反应3-5小时得偶合液。 [0027] The diazo solution obtained in step c was added to the condensation solution obtained in step b with sodium carbonate adjusted pH = 7, heated to IO0C, maintaining a temperature of 10-30 ° C, maintaining pH = 5-8, the reaction 3 5 hours to obtain coupling liquid.

[0028] e、中和反应 [0028] e, and the reaction

[0029] 将偶合液用盐酸溶液调整至pH = 6-6. 5,搅拌10_20分钟。 [0029] The coupling was washed with hydrochloric acid solution was adjusted to pH = 6-6. 5, 10_20 minutes stirring.

[0030] f、干燥 [0030] f, dried

[0031] 将e步骤的溶液喷雾干燥得式(I)化合物。 [0031] spraying a solution of the compound of formula e drying step (I).

[0032] 更优选地,上述结构式(I)的染料化合物的制备方法包括如下步骤: [0032] More preferably, the preparation of a compound of the above formula (I) dyes comprising the steps of:

[0033] a、H酸的溶解 [0033] a, H acid was dissolved

[0034] 向烧杯中加水,然后加入100% H酸,搅拌下用30%氢氧化钠溶液调pH = 6. 5-7,使物料溶解,澄清,调整溶液的体积,使溶液的质量/体积浓度为15%的H酸溶液。 [0034] Water was added to the beaker, and then 100% H acid was added, with stirring with 30% sodium hydroxide solution to adjust pH = 6. 5-7, the material was dissolved, a clear, adjust the volume of the solution, the quality of the solution / volume concentration of 15% solution of H acid.

[0035] b、缩合反应 [0035] b, a condensation reaction

[0036] 用直接冰和水调整H酸溶液温度至5〜7°C,调整溶液体积浓度为10 %,然后用碳酸氢钠维持pH = 6〜6. 5,用直接冰维持温度5〜10°C,用时40〜60分钟,将相当摩尔数质量的2,3- 二溴丙酰氯和丙酮混合液加入,维持温度5〜10°C和PH值6〜6. 5,反应1_3小时,得缩合液。 [0036] H-acid solution to adjust the temperature of the ice and water direct to 5~7 ° C, adjusting the solution concentration of 10% by volume, and then with sodium bicarbonate to maintain pH = 6~6. 5, maintaining the temperature 5 to 10 direct ice ° C, 40~60 minutes during use, a considerable number of moles of the mass of 2,3-dibromo-propionyl chloride and acetone mixture was added, maintaining a temperature of 5~10 ° C, and the PH value 6~6. 5, the reaction 1_3 hours to give condensed liquid.

[0037] C、重氮化反应 [0037] C, the diazotization

[0038] 在烧杯中加水,然后加入对位酯,搅拌10-20分钟。 [0038] Water was added to the beaker, followed by addition of para-ester, stirred for 10-20 minutes. 将30%盐酸溶液加入,用直接冰凋整溶液温度小于(TC,调整质量/体积浓度为5. 5 %,在反应溶液确保pH值小于2的条件下,将相当摩尔数质量的30%亚硝酸钠溶液快速加入,维持温度0〜5V '反应1-3小时,用氨基磺酸消除过量的亚硝酸,得重氮液, 30% hydrochloric acid solution was added, with ice adjustment is a direct solution temperature is less than (the TC, adjusting the mass / volume concentration of 5.5%, to ensure that at a pH of less than 2, a considerable number of moles of ethylene 30% by mass of the reaction solution in sodium nitrate solution is rapidly added, maintaining the temperature 0~5V 'the reaction for 1-3 hours to eliminate excess nitrous acid with sulphamic acid to give a diazo solution,

[0039] d、偶合反应 [0039] d, the coupling reaction

[0040] 将c步骤得到的重氮液加入到b步骤得到的缩合液中,用碳酸钠调pH = 7,升温到IO0C,维持温度10-300C,维持pH = 5-8,反应3-5小时。 [0040] The diazo solution obtained in step c was added to the condensation solution obtained in step b with sodium carbonate adjusted pH = 7, heated to IO0C, maintaining the temperature 10-300C, maintaining pH = 5-8, the reaction 3-5 hour. [0041] e、中和反应 [0041] e, and the reaction

[0042] 将偶合反应液用30%盐酸溶液调整至pH = 6-6. 5,搅拌10_20分钟。 [0042] The coupling reaction was adjusted with 30% hydrochloric acid solution to pH = 6-6. 5, 10_20 minutes stirring.

[0043] f、干燥 [0043] f, dried

[0044] 将e步骤的色液加入到料液预热器中,调整好喷雾塔进口温度进行喷雾干燥,得到产品。 [0044] The color solution is added to the step e preheater feed solution, adjusting the inlet temperature of the spray tower good spray-dried to give the product.

[0045] 上述方法中,H酸是I-氨基-8-萘酚-3,6-二磺酸单钠盐的简称,其结构式如下: [0045] The above process, H is the acid I- amino-8-naphthol-3,6-disulfonic acid monosodium salt short, having the formula as follows:

[0046] [0046]

Figure CN101735652BD00061

[0047] 对位酯又称对(¢-硫酸酯乙基砜)苯胺,乙烯砜硫酸酯,4-硫酸乙酯砜基苯胺,对-P -羟基乙砜苯胺硫酸酯或对-P -羟基乙砜苯胺硫酸酯,其结构式如下: [0047] ester, also known as para-on (¢ - ethyl sulfone sulfate) aniline sulfate vinyl sulfone, ethyl sulfone aniline-4-sulfate, on -P - hydroxy ethyl sulfone sulfate aniline or p -P - hydroxy ethyl sulfone aniline sulfate, which structural formula is as follows:

[0048] [0048]

Figure CN101735652BD00062

[0049] 上述方法和下文实施例的方法中,质量/体积浓度的单位为克/毫升(g/ml)或千克/ 升(kg/L)。 [0049] The above-described embodiments and a method embodiment hereinafter, mass / volume concentration units of grams / milliliter (g / ml) or kilograms / liter (kg / L).

[0050] 上述方法中所用到的各种原料物质都是能够从市场上购买得到的。 [0050] The various starting materials used in the above methods are purchased from the market can be obtained.

[0051] 本发明制备的化合物的使用和制备能够减少环境污染,所需原料成本低,产品溶解度高,色泽鲜艳,应用性能优异,使用方便,是一种适用性强的毛用红色活性染料。 Preparation and Use [0051] The compounds of the present invention can be prepared to reduce environmental pollution, low cost of raw materials required, high solubility, bright color, superior application performance, ease of use, a strong applicability reactive dye hair red.

具体实施方式 Detailed ways

[0052] 下面的实施例只是对本发明的技术方案的解释,并不对本发明的技术方案和保护范围形成任何的限制。 [0052] The following examples are to explain the technical solution of the present invention, it does not form any limit to the technical solutions of the present invention and scope.

[0053] 实施例I [0053] Example I

[0054] a、H酸的溶解 [0054] a, H acid was dissolved

[0055] 向500毫升烧杯中加水200毫升,然后加入100% H酸34. I克,搅拌下用30%氢氧化钠溶液调PH = 6. 5-7. 0,使物料溶解,澄清,调整溶液的体积为227毫升,使溶液的质量/体积浓度为15%,得H酸溶液。 [0055] To a 500-ml beaker was added 200 ml of water, followed by addition of 100% H 34. I g of acid, with stirring with 30% sodium hydroxide solution PH = 6. 5-7. 0, the material was dissolved, clarified adjustment the volume of solution is 227 ml, the quality of the solution / volume concentration of 15%, an H acid solution.

[0056] b、缩合反应 [0056] b, a condensation reaction

[0057] 用直接冰和水调整H酸溶液温度至5〜7°C,调整溶液质量/体积浓度为10%,然后伴随96%碳酸氢钠维持pH = 6〜6. 5,用直接冰维持温度5〜10°C,用时50分钟,将100%的2,3-二溴丙酰氯32. 6克和丙酮混合液加入,维持温度5〜10°C和pH值6〜6. 5,反应2小时得缩合液。 [0057] H-acid solution temperature adjusted to 5~7 ° C with ice and water directly, adjusting the solution mass / volume concentration of 10%, along with 96% sodium bicarbonate and then maintain pH = 6~6. 5, to maintain direct ice a temperature of 5~10 ° C, during 50 minutes, 100% of the 2,3-dibromo-propionyl chloride 32.6 g of acetone and the mixture was added, maintaining a temperature of 5~10 ° C and pH 6~6. 5, the reaction 2 hours to obtain the condensation liquid.

[0058] C、重氮化反应[0059] 在800毫升烧杯中加水200毫升,然后将100%对位酯28. I克加入,搅拌15分钟。 [0058] C, the diazotization [0059] 200 ml of water in 800 ml beaker, and 100% para 28. I g of the ester was added, stirred for 15 minutes. 再将15. 8克30%盐酸溶液加入,用直接冰调整溶液温度小于0°C,调整质量/体积浓度为 Then 15.8 g of 30% hydrochloric acid solution was added, with ice directly adjusting a solution temperature of less than 0 ° C, adjusted mass / volume concentration

5. 5 %,在反应溶液确保pH值小于2的条件下,将100%亚硝酸钠7. 04克,配成30%亚硝酸钠溶液快速加入,维持温度0〜5°C,反应2小时,用氨基磺酸消除过量的亚硝酸,得重氮液 5.5%, to ensure that the reaction solution at a pH of less than 2, 100% sodium nitrite 7.04 g, formulated as a 30% sodium nitrite solution was added quickly, maintaining the temperature at 0~5 ° C, 2 hours , with sulfamic acid to eliminate excess nitrous acid to give a diazo solution

[0060] d、偶合反应 [0060] d, the coupling reaction

[0061] 将c步骤得到的重氮液加入到b步骤得到的缩合液中,用96%碳酸钠调pH = 7,升温到200C,维持温度20-300C,维持pH = 7-7. 5,反应4小时。 [0061] The diazo solution obtained in step c was added to the condensation solution obtained in step b, adjusted with 96% sodium carbonate, pH = 7, heated to 200C of, maintaining a temperature of 20-300C, to maintain pH = 7-7. 5, for 4 hours.

[0062] e、中和反应 [0062] e, and the reaction

[0063] 将偶合反应液用30%盐酸溶液调整至pH = 6-6. 5,搅拌15分钟。 [0063] The coupling reaction was adjusted with 30% hydrochloric acid solution to pH = 6-6. 5, stirred for 15 minutes. [0064] f、干燥 [0064] f, dried

[0065] 将e步骤的色液加入到料液预热器中,调整好喷雾塔进口温度进行喷雾干燥。 [0065] The color solution is added to the step e preheater feed solution, adjusting the spray tower inlet temperature of the spray drying is good. 得下式结构的红色染料。 To obtain a red dye of the formula.

[0066] [0066]

0 0

Figure CN101735652BD00071

[0067] 本发明实施例I制备的毛用红色活性染料应用性能如下表所示: [0067] The embodiments of the present invention prepared in Example I with red hair application performance reactive dye shown in the following table:

[0068] [0068]

Figure CN101735652BD00072

[0069] 本发明的化合物及其制备方法已经通过具体的实施例进行了描述。 [0069] The compounds and methods of the present invention have been described by way of specific examples. 本领域技术人员可以借鉴本发明的内容适当改变原料、工艺条件等环节来实现相应的其它目的,其相关改变都没有脱离本发明的内容,所有类似的替换和改动对于本领域技术人员来说是显而易见的,都被视为包括在本发明的范围之内。 Those skilled in the art can learn the present invention is suitably part of the raw material changes, the respective process conditions to achieve the other objects, the relevant changes without departing from the present invention, all similar substitutes and modifications of ordinary skill in the art are apparent, are regarded as included within the scope of the present invention.

Claims (3)

  1. 1. ー种毛用红色活性染料的制备方法,该毛用红色活性染料是具有如下通式(I)结构的化合物: 1. Method for preparing hair types ー red reactive dye, the reactive dye is a red wool with a compound having structure (I) of the general formula:
    Figure CN101735652BC00021
    该方法包括如下步骤: a、H酸的溶解用氢氧化钠溶液调H酸溶液的pH为6. 5-7. 0,调整溶液的质量/体积浓度为0. 15g/ml,得H酸溶液; b、缩合反应调整H酸溶液质量/体积浓度为0. 10g/ml,用碳酸氢钠维持pH = 6〜6. 5,在温度5〜10°C,用时40〜60分钟,加入2,3- ニ溴丙酰氯和丙酮混合液,反应1-3小时,得缩合液; C、重氮化反应将对位酯溶解于水中,调节溶液温度小于0°C,用盐酸保持溶液的pH小于2,快速加入亚硝酸钠,保持温度0〜5°C反应1-3小时,用氨基磺酸消除过量的亚硝酸,得重氮液, d、偶合反应将c步骤得到的重氮液加入到b步骤得到的缩合液中,維持温度10-30°C,維持pH =5-8,反应3-5小时得偶合液; e、中和反应将偶合液用盐酸溶液调整至PH = 6-6. 5,搅拌15分钟; f、干燥将e步骤的溶液喷雾干燥得式(I)化合物。 The method comprises the steps of: a, dissolving sodium hydroxide solution pH with an acid solution H H 6. acid is 5-70, the solution is adjusted mass / volume concentration of 0. 15g / ml, to give H-acid solution. ;. b, H acid solution to adjust the condensation reaction mass / volume concentration of 0. 10g / ml, with sodium bicarbonate to maintain pH = 6~6 5, at a temperature of 5~10 ° C, when used 40~60 minutes, and 2, ni 3- bromopropionyl chloride and acetone mixture, the reaction for 1-3 hours to obtain the condensation liquid; C, the reaction will diazotization-ester was dissolved in water, adjusting the solution temperature is less than 0 ° C, maintaining the pH with hydrochloric acid solution is less than 2, rapid solution of sodium nitrite, maintaining the temperature at 0~5 ° C for 1 to 3 hours to eliminate excess nitrous acid with sulphamic acid to give a diazo solution, d, the coupling reaction in step c was added to the obtained diazo solution condensation liquid obtained in step b maintaining the temperature 10-30 ° C, maintaining pH = 5-8, for 3-5 hours to obtain a reaction fluid coupling; E, and the coupling reaction was treated with hydrochloric acid solution was adjusted to PH = 6-6 5, stirred for 15 minutes; F, spray drying the solution of the compound of formula e drying step (I).
  2. 2.根据权利要求I所述的方法,该方法包括如下步骤: a、H酸的溶解用水溶解H酸,然后用氢氧化钠溶液调pH = 6. 5-7. 0,使物料溶解、澄清,调整溶液的质量/体积浓度为0. 15g/ml,得H酸溶液; b、缩合反应在温度5〜7°C下,调整H酸溶液质量/体积浓度为0. 10g/ml,用碳酸氢钠维持pH =6〜6. 5,在温度5〜10°C,用时40〜60分钟,加入2, 3-ニ溴丙酰氯和丙酮混合液,维持温度5〜10°C和pH值6〜6. 5,反应1-3小时,得缩合液; C、重氮化反应将对位酯溶解于水中,加入盐酸,调节溶液温度小于(TC,保持溶液的pH小于2,快速加入亚硝酸钠,保持温度0〜5°C反应1-3小时,用氨基磺酸消除过量的亚硝酸,得重氮液, d、偶合反应将c步骤得到的重氮液加入到b步骤得到的缩合液中,用碳酸钠调pH = 7,升温到IO0C,维持温度10-30°C,维持pH = 5-8,反应3-5小时得偶合液;e、中和反应将偶合液用盐 2. The method according to claim I, the method comprising the steps of: a, dissolving an acid dissolved in water H H acid and then with sodium hydroxide solution pH = 6. 5-7 0, so that the material to dissolve, clarify. , the solution is adjusted mass / volume concentration of 0. 15g / ml, to give an acid solution H; B, the condensation reaction at 5~7 ° C, adjusting the H acid solution mass / volume concentration of 0. 10g / ml, with a carbonate sodium hydrogen to maintain pH = 6~6. 5, at a temperature of 5~10 ° C, when used 40~60 minutes, was added 2, 3-bromopropionyl chloride ni and acetone mixture, maintaining a temperature of 5~10 ° C and pH 6 . 5 ~ 6, the reaction for 1-3 hours to obtain the condensation liquid; C, the reaction will diazotization-ester was dissolved in water, hydrochloric acid was added to adjust the solution temperature is less than (the TC, maintaining pH of the solution is less than 2, rapid nitrite sodium, maintaining the temperature at 0~5 ° C for 1 to 3 hours to eliminate excess nitrous acid with sulphamic acid to give a diazo solution, d, diazo coupling reaction solution obtained in step c was added to the condensation solution obtained in step b , washed with sodium carbonate, adjusted pH = 7, heated to IO0C, maintaining a temperature of 10-30 ° C, maintaining pH = 5-8, for 3-5 hours to obtain a reaction fluid coupling; E, the coupling reaction solution and brine 溶液调整至PH = 6-6. 5,搅拌15分钟; f、干燥将e步骤的溶液喷雾干燥得式(I)化合物。 Solution was adjusted to PH = 6-6 5, stirred for 15 minutes;. F, spray drying the solution of the compound of formula e drying step (I).
  3. 3.根据权利要求2所述的方法,该方法包括如下步骤: a、H酸的溶解向烧杯中加水,然后加入100% H酸,搅拌下用30%氢氧化钠溶液调pH = 6. 5-7. 0,使物料溶解,澄清,调整溶液的体积,使溶液的质量/体积浓度为0. 15g/ml的H酸溶液; b、缩合反应用直接冰和水调整H酸溶液温度至5〜7°C,调整溶液质量/体积浓度为0. 10g/ml,然后用碳酸氢钠维持pH = 6〜6. 5,用直接冰维持温度5〜10°C,用时40〜60分钟,将相当摩尔数质量的2,3- ニ溴丙酰氯和丙酮混合液加入,維持温度5〜10°C和pH值6〜6. 5,反应1-3小时,得缩合液; C、重氮化反应在烧杯中加水,然后加入对位酯,搅拌15分钟;将30%盐酸溶液加入,用直接冰调整溶液温度小于(TC,调整质量/体积浓度为0. 055g/ml,在反应溶液确保pH值小于2的条件下,将相当摩尔数质量的30%亚硝酸钠溶液快速加入,維持温度0〜5°C,反应1-3小 3. The method according to claim 2, the method comprising the steps of: a, dissolving water was added to the acid H beaker and then 100% H acid was added, with stirring, 30% sodium hydroxide solution to adjust pH = 6. 5 . -70, the material was dissolved, a clear, adjust the volume of the solution, the quality of the solution / volume concentration of 0. 15g / H ml of acid solution; B, H acid condensation reaction solution temperature adjusted with ice and water directly to 5 ~7 ° C, the solution adjusted mass / volume concentration of 0. 10g / ml, and then maintained pH = 6~6. 5 with sodium bicarbonate, maintaining a temperature of 5~10 ° C by direct ice, when used 40~60 minutes, rather molar mass numbers ni bromopropionyl chloride and 2,3-acetone mixture was added, maintaining a temperature of 5~10 ° C and pH 6~6 5, the reaction for 1-3 hours to obtain the condensation liquid;. C, diazotization the reaction was added in a beaker of water, followed by addition of para-ester, stirred for 15 min; 30% hydrochloric acid solution was added to adjust the solution temperature by direct ice is less than (the TC is adjusted mass / volume concentration of 0. 055g / ml, ensuring that the pH in the reaction solution under conditions of less than 2, 30% sodium nitrite solution relatively quickly added molar mass number, maintaining the temperature 0~5 ° C, the reaction little 1-3 时,用氨基磺酸消除过量的亚硝酸,得重氮液, d、偶合反应将c步骤得到的重氮液加入到b步骤得到的缩合液中,用碳酸钠调pH = 7,升温到IO0C,维持温度10-30°C,维持pH = 5-8,反应3-5小时得偶合液; e、中和反应将偶合反应液用30%盐酸溶液调整至pH = 6-6. 5,搅拌15分钟; f、干燥将e步骤的溶液加入到料液预热器中,调整好喷雾塔进ロ温度进行喷雾干燥,得式(I)化合物。 When, with sulfamic acid to eliminate excess nitrous acid to give a diazo solution, d, diazo coupling reaction solution obtained in step c was added to the condensation solution obtained in step b with sodium carbonate adjusted pH = 7, heated to IO0C , maintaining the temperature 10-30 ° C, maintaining pH = 5-8, for 3-5 hours to obtain a reaction fluid coupling; E, in the coupling reaction and the reaction solution was adjusted to pH = 6-6 5 with 30% hydrochloric acid solution, stirred. 15 minutes; F, drying the solution of step e was added to a feed preheater, adjusting the spray tower inlet temperature ro spray drying, to give a compound of formula (I).
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EP0918074A1 (en) 1997-11-20 1999-05-26 ILFORD Imaging Switzerland GmbH Azo dyes, their preparation and use thereof
US6187912B1 (en) 2000-01-07 2001-02-13 Dystar Textifarben Gmbh & Co. Disazo compound their preparation and their use as dyestuffs
CN101215425A (en) 2008-01-22 2008-07-09 天津市德凯化工有限公司 Red reactive dyestuffs and preparation method thereof

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Publication number Priority date Publication date Assignee Title
EP0918074A1 (en) 1997-11-20 1999-05-26 ILFORD Imaging Switzerland GmbH Azo dyes, their preparation and use thereof
US6187912B1 (en) 2000-01-07 2001-02-13 Dystar Textifarben Gmbh & Co. Disazo compound their preparation and their use as dyestuffs
CN101215425A (en) 2008-01-22 2008-07-09 天津市德凯化工有限公司 Red reactive dyestuffs and preparation method thereof

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