阅读说明：本技术 一种1,4-二羟基蒽醌纳米有机分散颜料的制备方法 (Preparation method of 1, 4-dihydroxy anthraquinone nano organic dispersion pigment ) 是由 童勇军 于 2019-09-02 设计创作，主要内容包括：本发明公开了一种1,4-二羟基蒽醌纳米有机分散颜料的制备方法,(1)将1,4-二羟基蒽醌投入导热油加热反应釜内,升温使其融化汽化；(2)将汽化的1,4-二羟基蒽醌通过气体快速冷却,分散,使1,4-二羟基蒽醌在分子状态下被急剧冷却为固体,得固体1,4-二羟基蒽醌纳米有机分散颜料；(3)将冷却的固体1,4-二羟基蒽醌纳米有机分散颜料经机械粉碎,得1,4-二羟基蒽醌纳米有机分散颜料。本发明通过将1,4-二羟基蒽醌在高温环境下汽化,冷却,收集得到纳米大小的颜料微粒,所述颜料用于塑料制品,涂料,纺织油墨等,该方法过程简单、成本低,所制备的纳米有机分散颜料具有着色能力强,使用量少、颗粒更细,更均匀、颜色更艳,特别在塑料制品染色具有面粒径小,颜料用量少,色泽均一的特点。(The invention discloses a preparation method of 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment, (1) 1, 4-dihydroxy anthraquinone is put into a heat conducting oil heating reaction kettle, and the temperature is raised to melt and vaporize the heat conducting oil heating reaction kettle; (2) rapidly cooling and dispersing the vaporized 1, 4-dihydroxy anthraquinone by gas to rapidly cool the 1, 4-dihydroxy anthraquinone into solid in a molecular state, thereby obtaining the solid 1, 4-dihydroxy anthraquinone nano organic dispersion pigment; (3) and mechanically crushing the cooled solid 1, 4-dihydroxy anthraquinone nano organic dispersion pigment to obtain the 1, 4-dihydroxy anthraquinone nano organic dispersion pigment. The method has the advantages of simple process and low cost, and the prepared nano organic dispersion pigment has the characteristics of strong coloring capability, small using amount, finer particles, more uniformity and more brilliant color, and particularly has the characteristics of small surface particle size, small using amount of pigment and uniform color when the plastic product is dyed.)

1. A preparation method of 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment is characterized in that:

(1) 1, 4-dihydroxy anthraquinone is put into a heat-conducting oil heating reaction kettle, and the temperature is raised to melt and vaporize the heat-conducting oil heating reaction kettle;

(2) Rapidly cooling and dispersing the vaporized 1, 4-dihydroxy anthraquinone by gas to rapidly cool the 1, 4-dihydroxy anthraquinone into solid in a molecular state, thereby obtaining the solid 1, 4-dihydroxy anthraquinone nano organic dispersion pigment;

(3) And mechanically crushing the cooled solid 1, 4-dihydroxy anthraquinone nano organic dispersion pigment to obtain the 1, 4-dihydroxy anthraquinone nano organic dispersion pigment.

2. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the volume of the reaction kettle is 3-5L.

3. the method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the charging coefficient of the reaction kettle is 0.4-0.8.

4. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the reaction kettle is circularly heated by hot oil.

5. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the temperature of hot oil outside the reaction kettle is 200-350 ℃.

6. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the heat conducting oil direction of the reaction kettle adopts a mode from bottom to top.

7. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the temperature rise rate in the reaction kettle is 3-10 ℃/min.

8. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the vaporization temperature of the organic dispersion pigment is 250-300 ℃.

9. The method for preparing the 1, 4-dihydroxy anthraquinone nanometer organic dispersion pigment according to claim 1, characterized in that: the cooling mode adopts gas cooling, and the gas is air or nitrogen.

Technical Field

The invention belongs to the technical field of pigments, and relates to a preparation method of a mechanically dispersed pigment.

Background

The dispersion pigment has bright color tone, has the performance characteristics of tinting strength, hiding power, light resistance, weather resistance and the like, and is widely applied to the industries of paint, printing ink, printing and dyeing, plastic products, papermaking, rubber products, ceramics and the like. With the rapid development of downstream industries, the demand for pigments is continuously expanded, and the development prospect of the Chinese pigment industry is very wide. The existing dispersed pigment is mechanically crushed, particles are uneven and easy to agglomerate, so that the distribution is uneven, the chromaticity is deviated, a nozzle is easy to block, the diameter of the pigment is large, the ink is unstable, and the pigment is often micronized in practical application; meanwhile, the micro-scale and nano-scale pigments can enhance the covering power, saturation, adhesive force, glossiness and flexibility of the coating, wherein the enhancement of the covering power is beneficial to reducing the thickness of the coating, reducing the pigment consumption and lowering the product cost.

In order to achieve the best use effect of the product, generations of people are always exploring, pursuing and innovating the ultrafine grinding process. It is known that for a long period of time, most pigment and dye enterprises at home and abroad adopt a grinding and crushing process (a sand grinding pot and glass beads). However, the method takes a long time, and the product has residual glass bead powder, which greatly reduces the product quality. Later, the advent of high speed sand mills has greatly shortened grinding times, increased production efficiency, and significantly improved product quality. (Yangqiao, Qianwei. superfine and nano-grade dye crushing technology progress [ J ]. Shanghai dye 2014, 42 (5): 69-75.)

However, the high-speed sand mill is not free from the requirement of users on the fineness of the pigment and dye particles to be further increased to the nanometer level. Shanghai Yipin pigment Ltd (Yanbo, Shaoweifeng. black high temperature resistant manganese ferrite pigment production process research [ J ]. Chinese coating, 2012, 27 (8): 33-40.) adopts a Raymond mill to be used in the grinding process of the black high temperature resistant manganese ferrite pigment, and the grinding process has the advantages of best process comprehensive performance, high yield, good fineness, high tinting strength of a final product and excellent color developability.

The high-pressure homogenizer has the advantages of small volume, small occupied area, low price, electricity and labor conservation and continuous production, thereby gradually replacing a sand grinding pot and a sand grinder and promoting the rapid development of the post-treatment ultrafine grinding process in the dye and pigment industry. Technical personnel in Shanghai Donghua high-pressure homogenizer factories continuously strive to increase the use pressure of the high-pressure homogenizer to 150MPa, so that the particle size of the processed pigment and dye particles is increased from micron to nanometer (Yan Legionella, Zhang Liang, application and prospect of the high-pressure homogenizer in the dye and pigment post-processing technology [ J ] dye and dyeing, 2011, 48 (1): 59-62).

the chrome green pigment refining process is optimized by hole vibration (hole vibration, Yang Li Xiang, Yuan Yong, and the like.) in the specification of the chrome green pigment refining process [ J ] Chinese powder technology, 2017 (6): 71-77.) the micro-scale and nano-scale powder is prepared by adopting a wet grinding method, and the chrome green pigment with the grain diameter of about 336nm and narrow distribution is prepared at the rotating speed of 3000r/min, the grinding time of 4h, the filling rate of a grinding medium of 85 percent and the grain diameter of the grinding medium of 0.7 mm.

A method for producing fine particles of a pigment having an anthraquinone structure, and fine particles of a pigment having an anthraquinone structure obtained by the method, which are produced by Fuji film Co., Ltd. (Antenhao, Eryu, Kagaku Co., Ltd.). CN 101365758A [ P ]. 2009-2-11.) are characterized in that a pigment having an anthraquinone structure is dissolved in a good solvent to form a pigment A solution, a poor solvent which is miscible with the good solvent and is a pigment is a B solution, and A, B solution is mixed to produce the pigment having an anthraquinone structure into fine particles having a nano size.

in the process of nano-refining the pigment particles, no matter mechanical grinding and homogenization are adopted for refining the pigment particles, or a solvent is used for refining the pigment particles, the problems still exist in the industrial mass production process. For example, when the pigment is finely pulverized by a physical treatment method such as grinding, the pigment dispersion liquid tends to have a disadvantage of high viscosity, which is disadvantageous in the steps of packaging, transportation, storage, and the like. When the good solvent and the poor solvent are adopted to treat the pigment, the operation process is complicated, and the production cost and the environmental protection pressure are increased due to the large use of the organic solvent. Therefore, it is of great significance to find a method with simple treatment process, low cost and good pigment micronizing effect.

Disclosure of Invention

The invention aims to provide a preparation method of 1, 4-dihydroxy anthraquinone nano organic dispersion pigment.

The technical scheme of the invention is as follows: a preparation method of 1, 4-dihydroxy anthraquinone nano organic dispersion pigment,

(1) 1, 4-dihydroxy anthraquinone is put into a heat-conducting oil heating reaction kettle, and the temperature is raised to melt and vaporize the heat-conducting oil heating reaction kettle;

(2) Rapidly cooling and dispersing the vaporized 1, 4-dihydroxy anthraquinone by gas to rapidly cool the 1, 4-dihydroxy anthraquinone into solid in a molecular state, thereby obtaining the solid 1, 4-dihydroxy anthraquinone nano organic dispersion pigment;

(3) And mechanically crushing the cooled solid 1, 4-dihydroxy anthraquinone nano organic dispersion pigment to obtain the 1, 4-dihydroxy anthraquinone nano organic dispersion pigment.

The volume of the reaction kettle is 3-5L.

the charging coefficient of the reaction kettle is 0.4-0.8;

The reaction kettle is circularly heated by hot oil.

The temperature of hot oil outside the reaction kettle is 200-350 ℃.

The heat conducting oil direction of the reaction kettle adopts a mode from bottom to top.

The temperature rise rate in the reaction kettle is 3-10 ℃/min.

The vaporization temperature of the organic dispersion pigment is 250-300 ℃.

The cooling mode adopts gas cooling, and the gas is air or nitrogen.

The invention has the following technical effects that 1, 4-dihydroxy anthraquinone is vaporized and cooled in a high-temperature environment, and nanometer pigment particles are collected and obtained, wherein the pigment is used for plastic products, coatings, textile printing ink and the like.

Detailed Description