CN101705019B - Red reactive dye for wool and preparation method thereof - Google Patents

Red reactive dye for wool and preparation method thereof Download PDF

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CN101705019B
CN101705019B CN 200910228596 CN200910228596A CN101705019B CN 101705019 B CN101705019 B CN 101705019B CN 200910228596 CN200910228596 CN 200910228596 CN 200910228596 A CN200910228596 A CN 200910228596A CN 101705019 B CN101705019 B CN 101705019B
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acid
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CN101705019A (en )
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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 discloses a red reactive dye for wool and a preparation method thereof. The red 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 red 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

一种毛用红色活性染料及其制备方法 One kind of reactive dyes wool red 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要求越来越高。 In the 21st century, due to the environmental and ecological constraints, for color yield, it requires fixation and dyeing wastewater is increasing. 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 CN101705019BD00041

[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, to adjust the quality of the solution to obtain an acid solution 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] 将邻甲氧基间位酯溶解于水中,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] The inter-o-methoxyphenyl-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 to eliminate excess nitrous acid with sulphamic 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 [0015] e, and the reaction

[0016] 将偶合液用盐酸溶液调整至pH = 6-6. 5,搅拌10-20分钟。 [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] 将邻甲氧基间位酯溶解于水中,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] The inter-o-methoxyphenyl-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 hour, eliminating excess nitrous acid with sulphamic 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 h to obtain the 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 pH 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,然后加入邻甲氧基间位酯,搅拌10-20分钟。 [0038] Water was added in the beaker and then added o-m-methoxy-ester, stirred for 10-20 minutes. 将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0〜5°C,反应1-3小时,用氨基磺酸消除过量的亚硝酸,得重氮液, 30% hydrochloric acid solution was added, with ice directly adjusting a solution temperature of less than 0 ° c, to adjust the mass / volume concentration of 5.5%, under conditions to ensure the PH value of the reaction solution is less than 2, the number corresponding to 30% of ethylene molar mass sodium nitrate solution is rapidly added, maintaining the temperature at 0~5 ° C, 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[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10-30°c,维持pH = 5-8,反应3-5小时。 [0039] d, the coupling reaction [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 a temperature of 10-30 ° c, to maintain the pH = 5-8, the reaction for 3-5 hours.

[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1-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-described method, H acid is 1-amino-8-naphthol-3,6-disulfonic acid monosodium salt short, having the formula as follows:

[0046] [0046]

Figure CN101705019BD00061

[0047] 邻甲氧基间位酯的化学名为2-甲氧基-5-β -乙基砜基硫酸酯苯胺其结构式如下: [0047] Chemical-ester interproximal methoxy-called 2-methoxy -5-β - ethyl sulfone sulfate aniline structural formula as follows:

[0048] [0048]

Figure CN101705019BD00062

[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 description

[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1 [0053] Example 1

[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. 1克,搅拌下用30%氢氧化钠溶液调PH = 6. 5-7,使物料溶解,澄清。 [0055] To a 500-ml beaker was added 200 ml of water, followed by addition of 100% H acid 34.1 g, stirring with 30% sodium hydroxide solution PH = 6. 5-7, the material was dissolved, clarified. 调整溶液的体积为227毫升。 Volume was adjusted to 227 ml solution. 使溶液的质量/体积浓度为15% The solution was mass / volume concentration of 15%

[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 [0058] C, the diazotization

[0059] 在800毫升烧杯中加水200毫升,然后将100% 2_甲氧基_5_ β -乙基砜基硫酸酯苯胺31. 1克加入,搅拌15分钟。 [0059] Water was added 800 ml beaker 200 ml, then 100% 2_ methoxy _5_ β - ethyl sulfone aniline sulfate 31.1 g was added, stirred for 15 minutes. 再将15. 8克30%盐酸溶液加入。 Then 15.8 g of 30% hydrochloric acid solution was added. 用直接冰调整溶液温度小于0°C,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100%亚硝酸钠7. 04克,配成30%亚硝酸钠溶液快速加入。 Direct ice solution was adjusted to a temperature of less than 0 ° C, adjusted mass / volume concentration of 5.5%, to ensure that at a pH of less than 2 in the reaction solution, 100% sodium nitrite 7.04 g, 30% ethylene dubbed sodium nitrate solution was added quickly. 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 Maintaining the temperature at 0~5 ° C, reacted for 2 hours to eliminate excess nitrous acid with sulphamic 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]

Figure CN101705019BD00071
Figure CN101705019BD00072

[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 (4)

  1. 1. 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: A red reactive dye for wool, wool with a red reactive dye which is a compound of structure (I) have the general formula:
    Figure CN101705019BC00021
  2. 2.根据权利要求1所述的染料的制备方法,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- 二溴丙酰氯和丙酮混合液,反应1-3小时,得缩合液;C、重氮化反应将邻甲氧基间位酯溶解于水中,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,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酸溶液调整至PH = 6-6. 5,搅拌10-20分钟;f、干燥将e步骤的溶液喷雾干燥得式(I)化合物 The production method according to claim 1 dye, the method comprising the steps of: a, dissolving sodium hydroxide solution pH with an acid solution H H acid is 5-7.0 6. The adjusted solution mass / volume concentration of 0. 15g / ml, to give an acid solution H; B, the condensation reaction of the acid solution to adjust the mass H / volume concentration of 0. 10g / ml, maintaining the pH = 6~6 5 with sodium bicarbonate, at a temperature of -5 to 10. ° C, when used 40~60 minutes, was added 2,3-dibromo-propionyl chloride and acetone mixture, the reaction for 1-3 hours to obtain the condensation liquid; C, the diazotization reaction between o-methoxy-ester is dissolved in water adjusting the temperature of the solution 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 to eliminate excess nitrous acid with sulphamic acid to give a diazo liquid, d, diazo coupling reaction 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 fluid coupling; E, the coupling reaction was neutralized with hydrochloric acid solution was adjusted to PH = 6-6 5, stirred for 10-20 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- 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;C、重氮化反应将邻甲氧基间位酯溶解于水中,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,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 3. The method according to claim 2, 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, the material was dissolved, clarified adjustment mass of the solution / volume concentration of 0. 15g / ml, to give an acid solution H; b, a condensation reaction at 5~7 ° C, the acid solution to adjust the volume of mass concentration of H 0. 10g / ml, 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, for 1 to 3 hours to obtain the condensation liquid; C, the diazotization reaction between o-methoxy-ester is dissolved in water, hydrochloric acid was added to adjust the solution temperature is less than 0 ° C, maintaining the pH of the solution is less than 2, was added quickly 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, diazo coupling reaction solution obtained in step c was added to the obtained step b condensation solution, adjusted with sodium carbonate pH = 7, heated to IO0C, maintaining a temperature of 10-30 ° c, to maintain pH = 5-8, 3_5 hours to obtain a reaction fluid coupling; E, and the reaction 将偶合液用盐酸溶液调整至PH = 6-6. 5,搅拌10-20分钟;f、干燥将e步骤的溶液喷雾干燥得式(I)化合物。 The coupling was washed with hydrochloric acid solution was adjusted to PH = 6-6 5, stirred for 10-20 minutes;. F, spray drying the solution of the compound of formula e drying step (I).
  4. 4.根据权利要求2或3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- 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;C、重氮化反应在烧杯中加水,然后加入邻甲氧基间位酯,搅拌10-20分钟;将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,维持温度O〜5 4. The method of claim 2 or claim 3, 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 , the number of moles of considerable mass of 2,3-dibromo-propionyl chloride and 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, weight nitridation reaction with water in a beaker, and then added interproximal methoxy-ester, stirred for 10-20 min; 30% hydrochloric acid solution was added, the ice directly adjusting a solution temperature of less than 0 ° C, adjusted mass / volume concentration of 0. 055g / ml, ensuring the reaction solution at a pH of less than 2, the number of moles of considerable mass of a 30% sodium nitrite solution was added quickly, maintaining the temperature O~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、中和反应将偶合反应液用30%盐酸溶液调整至pH = 6-6. 5,搅拌10-20分钟;f、干燥将e步骤的溶液加入到料液预热器中,调整好喷雾塔进口温度进行喷雾干燥,得式(I) 化合物。 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, the pH adjusted with sodium carbonate = 7, heated to IO0C, maintaining a temperature of 10-30 ° C, maintaining pH = 5-8, 3_5 hours to obtain a reaction fluid coupling; E, in the coupling reaction and the reaction with 30% hydrochloric acid solution was adjusted to pH = 6-6 5, stirred for 10-20 minutes; F, drying the solution of step e was added to a feed preheater, adjusting the spray tower inlet temperature is a good 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
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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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