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High-vacuum sublimation purification method of 1,4-dihydroxyanthraquinone

A dihydroxyanthraquinone and high-vacuum technology, which is applied in the purification of pharmaceutical intermediates and the field of dyes, can solve the problems of increased thermal decomposition loss, high cost, and low vacuum degree, so as to increase the sublimation speed, shorten the production cycle, and increase the vacuum ratio. Effect

Inactive Publication Date: 2017-07-21
马骋
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The heating area of ​​the sublimator is small and the vacuum degree is low. Because of stirring, high vacuum cannot be achieved, and the sublimation speed is slow
Especially with the reduction of materials in the kettle, more and more heating surfaces and heating coils in the jacket of the reaction kettle are exposed, the effective heating area is getting smaller and smaller, and the sublimation speed is getting slower and slower; sublimation takes 24 to 30 hours
[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, not only low output, high cost, but also 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, which is a long-standing problem in production
[0009] 5. This kind of sublimator with stirring must have a mechanical seal, which cannot achieve high vacuum

Method used

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  • High-vacuum sublimation purification method of 1,4-dihydroxyanthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Example 1 (New Law 1)

[0058] The method for purifying 1,4-dihydroxyanthraquinone by high vacuum sublimation is prepared according to the following steps and process conditions:

[0059] Step 1), charging and feeding: Pour the industrial-grade 1.4-dihydroxyanthraquinone (content about 94%, moisture ≤ 1%) synthesized from hydroquinone and phthalic anhydride on the charging platform, and use a special The stainless steel trough is loaded, compacted, scraped, and placed on the feeding cart; the trough is put into the sublimation tube of each honeycomb sublimator, and the trough is required to be aligned and pushed into the sublimation tube; 12 parallel The sublimation tubes of the honeycomb sublimator are all filled, and a total of 400kg is fed.

[0060] Step 2), dehydration and melting: the heat source is supplied by a gas-fired heat-conducting oil furnace, and the temperature is controlled at 210-220°C. After a small amount of water is discharged, the material begins t...

Embodiment 2

[0068] Example 2 (new method 2)

[0069] The sublimation equipment is the same as in Example 1; it is prepared according to the following steps and process conditions:

[0070] Step 1), charging and feeding: Pour the industrial-grade (content about 92%, moisture ≤ 1%) 1.4-dihydroxyanthraquinone material synthesized from p-chlorophenol and phthalic anhydride on the charging platform, and use a special stainless steel Fill the trough, compact it, scrape it flat, and place it on the feeding cart; put the trough into the sublimation tube of each honeycomb sublimator. The sublimation tubes of the 12 honeycomb sublimators are all filled, and a total of 250kg is fed.

[0071] Step 2), dehydration, melting: the heat source is supplied by a gas-fired heat-conducting oil furnace, and the temperature is controlled at 240-245°C. After a small amount of water in the raw material is discharged, the material begins to melt. After the material is completely melted, close the cover and tighte...

Embodiment 3

[0086] The method for purifying 1, 4-dihydroxyanthraquinone by high vacuum sublimation, and the used honeycomb sublimator;

[0087] Such as figure 2 , image 3 , Figure 4 with 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 separately 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 sublimat...

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Abstract

The invention discloses a high-vacuum sublimation purification method of 1,4-dihydroxyanthraquinone, comprising the steps of feeding, dewatering and melting, purifying by sublimation, cooling and desublimating, cooling, opening a tank, collecting, weighing, and producing a next batch. The high-vacuum sublimation purification method of 1,4-dihydroxyanthraquinone provided herein adds no other chemical materials and is free of chemical reaction or wastewater, little waste gas may be adsorbed and removed by activated carbon, qualified nuts are entrusted for the incineration of waste residue, and emission of three wastes is basically zero; compared with chemical methods and solvent methods for purification, the method has the advantages of high product purity (> / =99%), high yield (> / =97%), better environmental friendliness and zero secondary pollution; in addition, the invention also discloses a honeycomb sublimator designed according to calculus principle; compared with reactor-type sublimators, the honeycomb sublimator has the advantages that sublimation time is shortened by 5 times and higher 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] Industrial synthesis of 1,4-dihydroxyanthraquinone, including 1.4-dihydroxyanthraquinone synthesized from hydroquinone and phthalic anhydride, with an industrial-grade raw material content of about 94%; and 1.4-dihydroxyanthraquinone synthesized from p-chlorophenol and phthalic anhydride Quinone, the content of industrial-grade raw materials is about 92%. The above-mentioned two kinds of industrial-grade raw materials can generally meet the needs of downstream products. Quinone (purity ≥ 99%) is 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 i...

Claims

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Application Information

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