CN1092632C - Process for preparing refined 1,4-dihydroxyl anthraquinone - Google Patents
Process for preparing refined 1,4-dihydroxyl anthraquinone Download PDFInfo
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- CN1092632C CN1092632C CN 99123829 CN99123829A CN1092632C CN 1092632 C CN1092632 C CN 1092632C CN 99123829 CN99123829 CN 99123829 CN 99123829 A CN99123829 A CN 99123829A CN 1092632 C CN1092632 C CN 1092632C
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- dihydroxyanthraquinone
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Abstract
The present invention relates to a technology for producing a fine product of 1, 4-dihydroxyanthraquinone. The present invention is characterized in that a, when a filter cake of 1, 4-dihydroxyanthraquinone is dried, the water content is smaller than 60%, the temperature of the filter cake entering a flash evaporation drier is from 180 to 280 DEG C, the temperature of the filter cake coming out of the flash evaporation drier is from 70 to 150 DEG C, and the time of the material passing through the drier is less than 20 minutes; b, during sublimation, a crude product with the water content smaller than 5.0% is put into a sublimator, and is stirred and trapped under the conditions of the vacuum degree of 500 mmHg to 755 mmHg and the temperature of 250 to 310DEGC, and thus, the fine product of 1, 4-dihydroxyanthraquinone is prepared. The method of the present invention has the advantage that the product purity is more than 99.5%; the sublimation yield is more than 98%; the method is suitable for industrial production; the land occupation area of the dryness technology is little; the operating conditions of workers are improved; the sublimation technological devices are simple; the investment is little.
Description
The present invention relates to 1, the production technique of 4-dihydroxyanthraquinone, particularly elaboration 1,4-dihydroxyanthraquinone production technique.
1, the 4-dihydroxyanthraquinone is important organic synthesis intermediate, this as Disperse Brown GL, be used to make EX-SF DISPERSE BLUE EX-SF 300 SR, EX-SF DISPERSE BLUE EX-SF 300 B, DISPERSE NAVY BLUE EXSF 300﹠ BLUE 56 100 RB, acid anthraquinone blue R, weak acid brilliant blue raw, weak acid green gs, Vat Grey BG, Vat Brown BR, and be used for producing intermediate 1, the 4-diamino-anthraquinone is widely used in dyestuffs such as synthetic dispersion, acidity, activity, reduction.At present, 1, the industrialized preparing process of 4-dihydroxyanthraquinone has Resorcinol and two kinds of methods of para-chlorophenol, adopts the Resorcinol method, because of the tight valency height of Resorcinol goods, dry back product yield only about 80%, content about 94%, 189 ℃ of fusing points, of poor quality, production cost is higher; The para-chlorophenol method, the branch that sulfuric acid and oleum are arranged again, no matter oleum is from cost, yield, still environmental protection, all be better than using the vitriol oil, yield is more than 86% behind the rake type dryer intermittently drying, and content is about 95%, and fusing point is about 192 ℃, there is the energy consumption height equally in this method, the deficiency that the working environment of workers difference and labour intensity are big, " chemical reagent " 1995.17 (1) .56 report adopts organic solvent chlorobenzene and acid to purify, though this method quality can improve, but yield is low, the cost height has only lab scale, unsuitable industrialization promotion; U.S. Pat P4.141.799 report adopts helical screw feeder that crude product is sent into well heater through fusing, enters the flake evaporation device, is rotated distillation, a part becomes liquid state condensation again, and tell columnar product through the secondary spiral, a part is separated in rectifying column and is refluxed the extraction salable product, after the liquid product condensation, go out columnar product through spiral, this technology is loaded down with trivial details, equipment is complicated, and investment is big, operation easier is big, is not suitable for China's industrialization promotion.
The object of the present invention is to provide a kind of elaboration 1,4-dihydroxyanthraquinone production technique, this technology can be avoided the deficiency of above-mentioned technology, seeks a kind ofly can improve 1 4-dihydroxyanthraquinone quality, method that again can suitability for industrialized production.
The present invention realizes that by following technical scheme this method comprises filter cake elaboration 1, and the dry and distillation production technique of 4-dihydroxyanthraquinone is characterized in that:
A, filter cake 1, cake moisture was less than 60% when the 4-dihydroxyanthraquinone carried out drying, entered 180-280 ℃ of the temperature control of moisture eliminator, when going out the flash distillation dryer main frame 70-150 ℃, the time of material process moisture eliminator, dry back crude product moisture content was less than 3.0% less than 20 minutes.
B, distillation the time are moisture content less than 5.0% crude product batch to feed intake into sublimer, and vacuum tightness is at 500mmHg-755mmHg, and temperature 250-310 ℃ was stirred 8-20 hour in sublimer, caught at least one of trap ,≤200 ℃ of its temperature controls through trap.
Way be with water content less than 60% 1,4-dihydroxyanthraquinone filter cake is sent into flash distillation dryer through spiral propeller, enter expansion drying main frame temperature and be controlled at 180 ℃-280 ℃, when going out the expansion drying main frame temperature 70-150 ℃, the material process moisture eliminator time was less than 20 minutes, after super-dry, advance spiral organ from the trap bottom of circling round, moisture content less than 3.0% crude product.Qualified crude product is dropped in the sublimer in batches, and vacuum tightness is at 500mmHg-755mmHg, temperature 250-310 ℃.In sublimer, stirred 8-20 hour,, but enter the trap of heat exchange through sublimer and top tubing string sublimation separation thereof, trap temperature≤200 ℃, distillation finishes, and feeds indifferent gas, remove vacuum, open the trap raw material and get high-purity elaboration 1,4-dihydroxyanthraquinone.In the equipment used, sublimer is that sublimer top is connected with tubing string with trap top with the trap mode of connection, being connected to last bottom between each trap is connected with tubing string with a back top, trap platform number is the 1-5 platform, in tubing string, separate distillation, but sublimer electricity consumption, steam, heat conduction solvent heat, and trap used vapour, water and solvent, gas come heat exchange.
Adopt technique scheme, by filter cake 1,4-dihydroxyanthraquinone dry and crude product sublimation process and equipment such as employing sublimer and trap, the purity of product is reached more than 99.5%, fusing point 〉=194 ℃, yield and was suitable for suitability for industrialized production more than 98% after filter cake carried out drying sublimation technology, in addition, also have the following advantages:
1, the drying process floor space is little, the energy successive drying, and processing power is big, and energy consumption is low, and outside the crude product that is gone out
See.
2, owing to adopt expansion drying, workman's operating environment and labour intensity all are improved.
3, sublimation process equipment is simple, easy to operate, and investment is also few.
For further specifying technique scheme, select for use two embodiment to describe with reference to Fig. 1:
Fig. 1 is technical process and equipment synoptic diagram.
Example 1: with the filter cake of 1200Kg water content 30%, joined in the spiral propeller (1) with 3 hours, and be sent to flash distillation dryer (2), enter place's temperature at 180-200 ℃, going out flash distillation dryer (2) temperature is 80-85 ℃, through super-dry, advance spiral organ (4) discharging from the trap that circles round (3) bottom, get moisture 2.1% crude product 866Kg; The 866Kg crude product is dropped in the sublimer (5), vacuum is risen to 600-650mmHg, temperature 295-310 ℃, stirred 18 hours, and, entered a trap (7) through sublimer (5) top tubing string (6) sublimation separation, temperature is less than 80 ℃, and the distillation time up feeds CO
2Gas is removed vacuum, opens trap (7), goes out finished product 827.3Kg yield 98.5%, 195 ℃ of fusing points, and content 99.1%, outward appearance is orange.
Example 2: with the filter cake 1100Kg of water content 21%, joined in the spiral propeller (1) with 3 hours, and be sent in the flash distillation dryer (2), 200-210 ℃ of its main frame temperature, go out 94-100 ℃ of flash distillation dryer main frame drying temperature, advancing spiral organ (4) from the trap that circles round (3) bottom through super-dry must water content be 0.6%, crude product 860Kg; The 860Kg crude product is dropped in the sublimer (5), vacuum tightness is risen to about 740mmHg temperature 290-310 ℃, stirred 10 hours, and separated distillation, enter four traps (7) through sublimer (5) top tubing string (6), temperature is less than 150 ℃, and the distillation time up feeds CO
2Gas is removed vacuum, opens trap (7), goes out finished product 857Kg, yield 98.6%, 194.5 ℃ of fusing points, content 99.5%, outward appearance orange.
Claims (5)
1, a kind of elaboration 1, the production technique of 4-dihydroxyanthraquinone comprises filter cake 1, the dry and distillation production technique of 4-dihydroxyanthraquinone is characterized in that:
A, filter cake 1, cake moisture was less than 60% when the 4-dihydroxyanthraquinone carried out drying, entered 180-280 ℃ of the temperature control of moisture eliminator, when going out the flash distillation dryer main frame 70-150 ℃, the time of material process moisture eliminator, dry back crude product moisture content was less than 3.0% less than 20 minutes.
B, when distillation moisture content batch to feed intake into sublimer, vacuum tightness is at 500mmHg-755mmHg less than 5.0% crude product, temperature 250-310 ℃ was stirred 8-20 hour in sublimer, caught at least one of trap ,≤200 ℃ of its temperature controls through trap.
2, by the described elaboration 1 of claim 1, the production technique of 4-hydroxyanthraquinone, it is characterized in that: in the equipment used, sublimer is that sublimer top is connected with tubing string with trap top with the trap mode of connection, is connected to last bottom between each trap and is connected with tubing string with a back top.
3, by the described elaboration 1 of claim 1, the production technique of 4-dihydroxyanthraquinone is characterized in that: trap platform number is the 1-5 platform.
4, by the described elaboration 1 of claim 2, the production technique of 4-dihydroxyanthraquinone is characterized in that: carry out sublimation separation in sublimer and tubing string.
5, by the described elaboration 1 of claim 2, the production technique of 4-dihydroxyanthraquinone is characterized in that: but sublimer electricity consumption, steam, heat conduction solvent heat, trap used vapour, water and solvent, gas come heat exchange.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99123829 CN1092632C (en) | 1999-11-15 | 1999-11-15 | Process for preparing refined 1,4-dihydroxyl anthraquinone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99123829 CN1092632C (en) | 1999-11-15 | 1999-11-15 | Process for preparing refined 1,4-dihydroxyl anthraquinone |
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| CN1257858A CN1257858A (en) | 2000-06-28 |
| CN1092632C true CN1092632C (en) | 2002-10-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 99123829 Expired - Fee Related CN1092632C (en) | 1999-11-15 | 1999-11-15 | Process for preparing refined 1,4-dihydroxyl anthraquinone |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104497617B (en) * | 2014-11-29 | 2016-08-24 | 萧县凯奇化工科技有限公司 | A kind of reducing dye palm fibre GG and preparation method |
| CN105884592A (en) * | 2016-04-22 | 2016-08-24 | 马骋 | Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum |
| CN110540760A (en) * | 2019-09-02 | 2019-12-06 | 娄底彤艳新材料科技有限公司 | Preparation method of 1, 4-dihydroxy anthraquinone nano organic dispersion pigment |
| CN113137833A (en) * | 2021-04-28 | 2021-07-20 | 河南省华中食品有限公司 | Gas protection anti-oxidation process in vacuum drying or freeze-drying process |
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