CN103013169B - A kind of spray drying method of azo organic dye aqueous solution - Google Patents

A kind of spray drying method of azo organic dye aqueous solution Download PDF

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CN103013169B
CN103013169B CN201210552077.0A CN201210552077A CN103013169B CN 103013169 B CN103013169 B CN 103013169B CN 201210552077 A CN201210552077 A CN 201210552077A CN 103013169 B CN103013169 B CN 103013169B
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dye
aqueous solution
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organic dye
azo
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CN103013169A (en
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张晓东
刘馨
崔敏
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Qingdao University
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Abstract

本发明公开一种偶氮类有机染料水溶液的喷雾干燥方法,其特点是按下述步骤实施:定量称取待喷雾干燥的偶氮类有机染料水溶液,开动搅拌,加入适量水溶性防焦化剂,充分搅拌混合均匀后,送喷雾干燥器进行干燥。该方法可以克服常规偶氮类有机染料水溶液因喷雾干燥所造成的染料色光发暗,染料强度下降的缺点,并且工艺简单,易于实现。The invention discloses a spray-drying method of an azo-type organic dye aqueous solution, which is characterized in that it is carried out according to the following steps: quantitatively weigh the azo-type organic dye aqueous solution to be spray-dried, start stirring, add an appropriate amount of water-soluble anti-coking agent, After fully stirring and mixing evenly, send it to a spray dryer for drying. The method can overcome the disadvantages of dull dye color and decreased dye strength caused by spray drying of the conventional azo organic dye aqueous solution, and the process is simple and easy to realize.

Description

一种偶氮类有机染料水溶液的喷雾干燥方法A kind of spray drying method of azo organic dye aqueous solution

技术领域technical field

本发明涉及有机染料的干燥方法;特别是涉及一种偶氮类有机染料水溶液的喷雾干燥方法。The invention relates to a drying method of organic dyes; in particular, it relates to a spray drying method of an azo organic dye aqueous solution.

背景技术Background technique

偶氮类染料种类较多,色谱齐全,物美价廉,主要应用于纺织和造纸行业。近年来,染料行业的竞争日趋激烈,因此促使各染料生产企业都在不断优化生产工艺,力图降低生产成本,使自己在市场竞争中占据有利地位。在偶氮类染料的生产工艺中,所制备的染料水溶液通常经过盐析、过滤,浓缩或干燥等工艺而最终制成粉状染料或者高浓液体染料。传统的染料生产工艺主要采用盐析分离染料成分,不仅产品纯度不高,不同批次的产品质量存在批间差,很难保证产品质量的稳定,而且在盐析过程还使用了无机盐,因此在过滤过程中产生了大量含盐废水,这些废水的排放对环境造成了极大的污染,严重制约着染料工业的可持续发展。近年来,为了避免染料生产过程中排放大量含盐染料废水,同时确保染料产品质量稳定,避免产品批间差,国内外众多染料企业纷纷采用喷雾干燥工艺对合成制备的染料水溶液进行干燥,其中直接染料喷雾干燥工艺参数通常选择:进口空气温度为220℃~280℃,出口空气温度为90℃~110℃.由于获得的染料产品具有颗粒状,无尘且易于分散溶解,产品质量稳定等特点,因此喷雾干燥技术深获染料企业青睐,在染料行业得到了广泛推广应用。然而偶氮类染料高温热稳定性相对较差,在采用喷雾干燥技术干燥过程中,高温空气会导致偶氮类染料发生热分解而产生焦化现象,从而导致染料产品色光发暗,染料强度明显降低的缺点。因此,如何避免偶氮类染料在喷雾干燥过程中发生热分解,确保提高染料品质和强度,是染料行业当前急需解决的问题之一。There are many types of azo dyes, complete color spectrum, high quality and low price, and are mainly used in textile and paper making industries. In recent years, the competition in the dye industry has become increasingly fierce, so all dye manufacturers are constantly optimizing the production process, trying to reduce production costs, so that they can occupy a favorable position in the market competition. In the production process of azo dyes, the prepared dye aqueous solution is usually salted out, filtered, concentrated or dried to finally be made into powdery dyes or high-concentration liquid dyes. The traditional dye production process mainly uses salting-out to separate the dye components. Not only is the product purity not high, but there are batch-to-batch differences in the product quality of different batches, it is difficult to ensure the stability of product quality, and inorganic salts are also used in the salting-out process, so A large amount of salty wastewater is produced during the filtration process, and the discharge of these wastewaters has caused great pollution to the environment, seriously restricting the sustainable development of the dye industry. In recent years, in order to avoid the discharge of a large amount of salt-containing dye wastewater during the dye production process, while ensuring stable dye product quality and avoiding product batch differences, many dye companies at home and abroad have adopted spray drying technology to dry the synthetically prepared dye aqueous solution. The parameters of the dye spray drying process are usually selected: the inlet air temperature is 220°C-280°C, and the outlet air temperature is 90°C-110°C. Because the obtained dye product is granular, dust-free, easy to disperse and dissolve, and the product quality is stable, etc., Therefore, the spray drying technology is deeply favored by dye companies and has been widely promoted and applied in the dye industry. However, azo dyes are relatively poor in high-temperature thermal stability. During the drying process using spray drying technology, high-temperature air will cause thermal decomposition of azo dyes and cause coking, which will lead to dark color of dye products and a significant reduction in dye strength. Shortcomings. Therefore, how to avoid the thermal decomposition of azo dyes during the spray drying process and ensure the improvement of dye quality and strength is one of the urgent problems in the dye industry.

发明内容Contents of the invention

本发明的目的是提供一种偶氮类有机染料水溶液的喷雾干燥生产方法。该方法可以克服上述不足之处。The object of the present invention is to provide a spray-drying production method of an azo organic dye aqueous solution. This method can overcome the disadvantages mentioned above.

本发明的目的是通过以下技术方案来实现的:一种偶氮类有机染料水溶液的喷雾干燥方法,其特征在于按下述步骤实施:定量称取待喷雾干燥的偶氮类有机染料水溶液,开动搅拌,加入适量水溶性防焦化剂,充分搅拌混合均匀后,送喷雾干燥器进行干燥。The object of the present invention is achieved by the following technical solutions: a spray drying method of an azo organic dye aqueous solution is characterized in that it is implemented according to the following steps: quantitatively weigh the azo organic dye aqueous solution to be spray-dried, start Stir, add an appropriate amount of water-soluble anti-scorching agent, fully stir and mix evenly, and send it to a spray dryer for drying.

上述技术方案中所述的染料水溶液的染料浓度为1~50%;The dye concentration of the dye aqueous solution described in the above technical scheme is 1-50%;

上述技术方案中所述的喷雾干燥器,其进口空气温度为200℃~280℃,出口空气温度为90℃~110℃;The spray dryer described in the above technical solution has an inlet air temperature of 200°C to 280°C and an outlet air temperature of 90°C to 110°C;

上述技术方案中所述的水溶性防焦化剂为亚硫酸钠,亚硫酸氢钠,氨基磺酸,或焦亚硫酸钠中的一种或其混合物;The water-soluble anti-coking agent described in the above-mentioned technical scheme is sodium sulfite, sodium bisulfite, sulfamic acid, or one or its mixture in sodium metabisulfite;

上述技术方案中所述的加入适量水溶性防焦化剂,其加入量为合成制备的偶氮染料水溶液中有机染料的重量的0.1%~2%;The addition of an appropriate amount of water-soluble anti-scorching agent described in the above technical scheme, its addition is 0.1% to 2% of the weight of the organic dye in the synthetically prepared azo dye aqueous solution;

本发明与现有技术相比有许多优点和积极效果Compared with the prior art, the present invention has many advantages and positive effects

1、本发明的一种偶氮类有机染料水溶液的喷雾干燥方法,可以克服现有偶氮类有机染料生产过程中因喷雾干燥造成的染料产品色光发暗,强度降低的缺点。1. The spray-drying method of a kind of azo-type organic dye aqueous solution of the present invention can overcome the shortcoming that the color of the dye product caused by spray-drying in the existing azo-type organic dye production process is dark and the intensity is reduced.

2、本发明工艺简单、合理,便于实施和推广。2. The process of the present invention is simple and reasonable, and is convenient for implementation and popularization.

具体实施方式Detailed ways

本发明的一种偶氮类有机染料水溶液的喷雾干燥方法,是按下述步骤实施:定量称取待喷雾干燥的偶氮类有机染料水溶液,开动搅拌,加入适量水溶性防焦化剂,充分搅拌混合均匀后,送喷雾干燥器进行干燥。The spray-drying method of a kind of azo organic dye aqueous solution of the present invention is implemented according to the following steps: quantitatively weigh the azo organic dye aqueous solution to be spray-dried, start stirring, add an appropriate amount of water-soluble anti-coking agent, and fully stir After mixing evenly, send it to a spray dryer for drying.

下面通过实施例来进一步详细说明本发明。The present invention will be further described in detail below by way of examples.

实施例1Example 1

称取直接耐晒黑G商品染料(染料强度100%),用去离子水配置浓度为13%的直接耐晒黑G染料溶液备用;称取直接耐晒黑G商品染料(染料强度100%),用去离子水配置浓度为13%的染料溶液,再加入占染料含量0.5%的亚硫酸钠,搅拌均匀后,得加剂浓度为12%的直接耐晒黑G染料溶液备用;启动LPG型高速离心喷雾干燥机,控制高速离心喷雾烘干机进口空气温度为270±5℃,出口空气温度为100±5℃干燥上述配置的染料溶液,分别得干燥的直接耐晒黑G染料粉末和加剂直接耐晒黑G染料粉末。按照国家标准GB/T6688-2008测试所得染料粉末的相对强度,结果表明:未加剂直接耐晒黑G染料的相对强度为85%,加亚硫酸钠的直接耐晒黑G染料的相对强度为95%.Take by weighing Direct Fast Black G commercial dye (dye strength 100%), and use deionized water configuration concentration to be 13% Direct Fast Black G dye solution for subsequent use; Weigh Direct Fast Black G commercial dye (dye strength 100%) , use deionized water to prepare a dye solution with a concentration of 13%, then add sodium sulfite accounting for 0.5% of the dye content, and stir evenly to obtain a direct sunfast black G dye solution with an additive concentration of 12% for use; start the LPG type high-speed centrifuge Spray dryer, control the inlet air temperature of the high-speed centrifugal spray dryer to 270±5°C, and the outlet air temperature to 100±5°C to dry the above-mentioned dye solution to obtain dry direct sunfast black G dye powder and additive direct Fast Black G Dye Powder. According to the national standard GB/T6688-2008, the relative strength of the obtained dye powder is tested, and the results show that the relative strength of direct sunfast black G dye without additives is 85%, and the relative strength of direct sunfast black G dye with sodium sulfite is 95%. .

实施例2Example 2

与实施例1基本相同,只是将高速离心喷雾烘干机进口空气温度调整为240±5℃,结果表明:未加剂直接耐晒黑G染料的相对强度为91%,加剂直接耐晒黑G染料的相对强度为96%.It is basically the same as in Example 1, except that the inlet air temperature of the high-speed centrifugal spray dryer is adjusted to 240±5°C. The results show that the relative strength of the direct sunfast black G dye without additives is 91%, and the direct sunfast black with additives is 91%. The relative intensity of G dye is 96%.

实施例3Example 3

与实施例2基本相同,只是将直接耐晒黑G商品染料(染料强度100%)换成直接黑22(染料强度150%)),结果表明:未加剂直接黑22的染料相对强度为138%,加剂直接耐晒黑22染料的相对强度为144%.It is basically the same as in Example 2, except that direct sunfast black G commercial dye (100% dye strength) is replaced with direct black 22 (dye strength 150%)), and the results show that the relative strength of the dyestuff without additive direct black 22 is 138 %, the relative strength of additive Direct Fast Black 22 dye is 144%.

实施例4Example 4

与实施例2基本相同,只是将直接耐晒黑G商品染料(染料强度100%)换成直接耐酸大红4BS(染料强度200%),结果表明:未加剂直接耐酸大红4BS的染料相对强度为182%,加剂直接耐酸大红4BS染料的相对强度为192%.It is basically the same as in Example 2, except that the direct sunfast black G commercial dye (100% dye strength) is replaced by direct acid-fast scarlet 4BS (dye strength 200%), and the results show that the relative strength of the dyestuff without adding any direct acid-fast scarlet 4BS is 182%, and the relative strength of direct acid-fast scarlet 4BS dye with additive is 192%.

实施例5Example 5

与实施例2基本相同,只是将直接耐晒黑G商品染料(染料强度100%)水溶液的染料浓度提高到20%,结果表明未加剂的直接耐晒黑G染料的相对强度为91%,加剂直接耐晒黑G染料的相对强度为96%.Substantially the same as Example 2, only the dye concentration of the direct sunfast black G commercial dye (100% dye strength) aqueous solution is increased to 20%, the result shows that the relative intensity of the direct sunfast black G dye without additive is 91%, The relative strength of the additive Direct Fast Black G dye is 96%.

实施例6Example 6

与实施例3基本相同,只是将亚硫酸钠换成亚硫酸氢钠,结果表明:未加剂直接黑22染料的相对强度为140%,加剂直接黑22染料的相对强度为148%.It is basically the same as Example 3, except that sodium sulfite is replaced by sodium bisulfite, and the results show that the relative intensity of direct black 22 dye without additive is 140%, and the relative intensity of direct black 22 dye with additive is 148%.

实施例7Example 7

与实施例3基本相同,只是将亚硫酸钠换成氨基磺酸,结果表明:未加剂直接黑22染料的相对强度为134%,加剂直接黑22染料的相对强度为143%.It is basically the same as in Example 3, except that sodium sulfite is replaced with sulfamic acid, and the results show that the relative intensity of direct black 22 dye without additive is 134%, and the relative intensity of direct black 22 dye with additive is 143%.

实施例8Example 8

与实施例2基本相同,只是将亚硫酸钠换成重量比1∶1的亚硫酸钠与亚硫酸氢钠,结果表明:未加剂直接黑22染料的相对强度为135%,加剂直接黑22染料的相对强度为144%.It is basically the same as Example 2, except that sodium sulfite is changed into sodium sulfite and sodium bisulfite in a weight ratio of 1: 1, the results show that: the relative strength of the direct black 22 dye without additive is 135%, and the relative strength of the direct black 22 dye with additive is 135%. Strength is 144%.

实施例9Example 9

与实施例3基本相同,只是将亚硫酸钠换成重量比1∶1的亚硫酸钠与氨基磺酸,结果表明:未加剂直接黑22染料的相对强度为131%,加剂直接黑22染料的相对强度为144%.Substantially the same as in Example 3, except that sodium sulfite is replaced by sodium sulfite and sulfamic acid in a weight ratio of 1:1, the results show that the relative intensity of direct black 22 dye without additive is 131%, and the relative intensity of direct black 22 dye with additive is 144%.

实施例10Example 10

与实施例3基本相同,只是将亚硫酸钠换成重量比1∶1的亚硫酸氢钠与氨基磺酸,结果表明:未加剂直接黑22染料的相对强度为130%,加剂直接黑22染料的相对强度为143%.It is basically the same as in Example 3, except that sodium sulfite is replaced by sodium bisulfite and sulfamic acid with a weight ratio of 1: 1. The results show that the relative strength of the direct black 22 dye without additive is 130%, and the direct black 22 dye with additive is 130%. The relative strength of 143%.

当然,上述说明并非是对本发明的限制,本发明也并不限于上述举例,本技术领域的普通技术人员,在本发明的实质范围内,作出的变化、改型、添加或替换,都应属于本发明的保护范围。Of course, the above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Any changes, modifications, additions or substitutions made by those skilled in the art within the scope of the present invention shall all belong to protection scope of the present invention.

Claims (1)

1.一种偶氮类有机染料水溶液的喷雾干燥方法,其特点是按下述步骤实施:定量称取待喷雾干燥的偶氮类有机染料水溶液,开动搅拌,加入适量水溶性防焦化剂,充分搅拌混合均匀后,送喷雾干燥器进行干燥,得粉状染料产品,上述技术方案中所述的喷雾干燥器,其进口空气温度为200℃~280℃,出口空气温度为90℃~110℃;上述技术方案中所述的染料水溶液的染料浓度为1~50%;上述所述的水溶性防焦化剂为亚硫酸钠,亚硫酸氢钠,氨基磺酸,或焦亚硫酸钠中的一种或其混合物;其加入量为偶氮类有机染料水溶液中有机染料重量的0.1%~2%。1. a spray-drying method of an azo organic dye aqueous solution is characterized in that it is implemented in the following steps: quantitatively take the azo organic dye aqueous solution to be spray-dried, start stirring, add an appropriate amount of water-soluble anti-coking agent, fully After stirring and mixing evenly, send it to a spray dryer for drying to obtain a powdery dye product. The spray dryer described in the above technical solution has an inlet air temperature of 200°C to 280°C and an outlet air temperature of 90°C to 110°C; The dye concentration of the dye aqueous solution described in the above technical solution is 1-50%; the above-mentioned water-soluble anti-scorching agent is one of sodium sulfite, sodium bisulfite, sulfamic acid, or sodium metabisulfite or a mixture thereof; The added amount is 0.1%-2% of the weight of the organic dye in the azo organic dye aqueous solution.
CN201210552077.0A 2012-12-06 2012-12-06 A kind of spray drying method of azo organic dye aqueous solution Expired - Fee Related CN103013169B (en)

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CN101580643B (en) * 2009-03-31 2012-11-28 天津市亚东化工染料厂 Pollution-free production technology of direct fast black G
CN101580650A (en) * 2009-03-31 2009-11-18 天津市亚东化工染料厂 Direct spray drying preparation technology of direct fast black 22
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