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Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum

A dihydroxyanthraquinone and high-vacuum technology, which is used in the purification of pharmaceutical intermediates and dyes, can solve the problems of long sublimation time, energy waste, and exposed heating surface, and achieve no secondary pollution, high product purity, and exhaust rate big effect

Inactive Publication Date: 2016-08-24
马骋
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 2. The sublimation time is long, and most of the heating surface is exposed in the later stage of sublimation, resulting in energy waste
[0007] 3. The structure of the hydroxyl compound is not stable, and it will sublime for a long time at high temperature, which will increase the loss of thermal decomposition and reduce the yield
[0008] 4. The old method is difficult to remove slag
[0009] 5. This kind of sublimator with stirring must have a mechanical seal, which cannot achieve high vacuum

Method used

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  • Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum
  • Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum
  • Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum

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Embodiment 1

[0043] Raw material selection in this example: industrial grade 1, 4-dihydroxyanthraquinone; production unit: Jiangsu Yabang; purity: 94%, moisture: ≤1%, appearance brick red; testing unit: Jiangsu Yabang; feeding Jiangsu Yabang 2015-6-25 batch; feeding quality 400Kg;

[0044] Such as figure 1 Shown, the method for high vacuum sublimation purification 1,4-dihydroxyanthraquinone is prepared as follows:

[0045] Step 1) Feeding: put industrial grade 1, 4-dihydroxyanthraquinone into the trough, after compacting and scraping, put it into the sublimation tube of 10 or 12 parallel honeycomb sublimators;

[0046] The parallel honeycomb sublimator refers to the vacuum system on the adjacent honeycomb sublimator, and the heating system and the cooling system are arranged in parallel;

[0047] Step 2) Dehydration and melting: heat the industrial grade 1, 4-dihydroxyanthraquinone in the sublimation tube under non-vacuum conditions, turn on the heating system, control the temperature at...

Embodiment 2

[0059] The method for purifying 1, 4-dihydroxyanthraquinone by high vacuum sublimation, and the used honeycomb sublimator;

[0060] Such as figure 2 , image 3 , Figure 4 and Figure 5 As shown, the honeycomb sublimator includes a crystallization tank body 1, a heating tank body 2, a tank cover 3, a tube plate 2.1, a sublimation tube 2.2, a support plate 2.3 and a trough; in the crystallization tank body 1 A crystallization chamber 1.1 is provided; a heating chamber 2.4 is provided in the heating tank body 2; one end of the crystallization tank body 1 is connected to the non-closed end of the heating tank body 2 through a tube plate 2.1; the crystallization tank body 1 is another One end is hinged with the tank cover 3; the tube plate 2.1 is provided with a honeycomb through hole; the heating chamber 2.4 is provided with a support plate 2.3; the support plate 2.3 is provided with a honeycomb through hole with the tube plate 2.1 Corresponding through holes; the sublimatio...

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Abstract

The invention discloses a method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum. The method comprises the following preparation steps: feeding; dehydrating and fusing; purifying by sublimation; cooling and condensing; opening a tank, collecting and weighing after cooling is finished; and producing a next batch of 1, 4-dihydroxy anthraquinone. By the method provided by the invention, other chemical raw materials are not added, chemical reaction does not exist, waste water does not exist either, a small amount of waste gas can be adsorbed and removed by activated carbon, waste residues are incinerated by qualified units, and therefore, emission of the waste gas, the waste water and the waste residues is avoided basically. Compared with purification by a chemical method and a solvent method, the method has the advantages that the purity of the product is high (greater than or equal to 99%, the yield is high (greater than or equal to 97%), and is environmentally friendly; and secondary pollution is avoided. In addition, the invention further discloses a honeycomb sublimator which is designed according to the principle of infinitesimal. Compared with a reaction kettle type sublimator, the honeycomb sublimator has the features that sublimation time is shortened by more than 5 times, and energy is saved by 70%.

Description

technical field [0001] The invention relates to a method for purifying 1, 4-dihydroxyanthraquinone by high vacuum sublimation, belonging to the technical field of purification of dyes and pharmaceutical intermediates. Background technique [0002] The purity of industrially synthesized 1,4-dihydroxyanthraquinone is about 94%, which can generally meet the requirements of downstream products. Purity ≥ 99%) are in short supply; [0003] Relevant production companies in this field have long used a reactor-type sublimator with stirring and heating coils. The temperature is 260-300°C and the vacuum degree is 500-750mmHg, and the sublimation method is used to purify 1,4-dihydroxyanthraquinone. The following "Old Law" for short; [0004] In the actual production process of the old method, the main shortcomings are as follows: [0005] 1. The heating area of ​​the sublimator is small, the vacuum degree is low, and the sublimation speed is slow. Especially with the reduction of ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/10C07C50/34B01D7/02
CPCB01D7/02C07C46/10C07C50/34
Inventor 马骋
Owner 马骋
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