CN105884592A - Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum - Google Patents
Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum Download PDFInfo
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- CN105884592A CN105884592A CN201610253528.9A CN201610253528A CN105884592A CN 105884592 A CN105884592 A CN 105884592A CN 201610253528 A CN201610253528 A CN 201610253528A CN 105884592 A CN105884592 A CN 105884592A
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- sublimation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
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
A kind of method that the present invention relates to fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone, belongs to dyestuff, medicine intermediate
Purification technique field.
Background technology
Commercial synthesis 1,4 dihydroxyanthraquinone purity about 94%, typically can meet downstream product requirement, but in recent years due to
The demands such as the updating and upgrading of a product, liquid dyes, outlet, high-purity 1 on market, 4-dihydroxyanthraquinone (purity >=99%) is well sold and in short supply；
This area associated production enterprise uses band stirring, the reaction autoclave sublimating apparatus of band heating coil for a long time, and temperature is at 260-300
DEG C, under vacuum 500-750mmHg process conditions, sublimed method purification 1,4-dihydroxyanthraquinone, hereinafter referred to as " old method "；
Old method, in actual production process, is primarily present shortcoming as follows:
1, the heating surface (area) (HS of sublimating apparatus is little, and vacuum is low, and rate of sublimation is slow.Reducing in particular with material in still, reactor presss from both sides
Set inner heating surface and heating coil are exposed more and more, and effective heating surface (area) (HS is fewer and feweri, and rate of sublimation is more and more slower.Once throw
Material 400Kg, distillation wants 24 ~ 30 hours.
2, sublimation time is long, and distillation later stage major part heating surface is exposed, causes energy waste.
3, hydroxy compounds structure is understable, at high temperature, distils for a long time, increases thermal decomposition loss, reduces yield.Always
Method product yield 85%.
4, old method slagging-off difficulty.
5, the sublimating apparatus of this band stirring, it is necessary to have mechanical seal, it is impossible to realize fine vacuum.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the present invention provides a kind of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxy-anthracene
The method (hereinafter referred to as " new method ") of quinone, prepares as follows:
Step 1) feeds intake: is loaded by technical grade Isosorbide-5-Nitrae-dihydroxyanthraquinone in hopper, after compacting strikes off, puts into by 10 or 12
In the sublimation pipe of honeycomb fashion sublimating apparatus in parallel；
Described honeycomb fashion sublimating apparatus in parallel refers to the vacuum system on adjacent honeycomb fashion sublimating apparatus, heating system and cooling
System arranges according to parallel way；
Step 2) it is dehydrated, melts: to the technical grade Isosorbide-5-Nitrae-dihydroxyanthraquinone in sublimation pipe, carry out heating under non-vacuum condition, open
Opening heating system, temperature controls at 210 ~ 220 DEG C, and the time controls at 30min, after discharging water vapour, and capping；
Step 3) sublimation purification: open vacuum system and cooling system simultaneously, progressively make vacuum pressure control in 30min
Below 100pa, heating and temperature control is at 220 DEG C, and the time controls at 240min；The organic exhaust gas that vacuum system is discharged, passes through 15m
High aiutage, discharges after utilizing activated carbon adsorption；
Step 4) cooling is sublimated: sublimation purification and cooling are sublimated and carried out simultaneously, subliming by heating out high-purity in sublimation pipe
Isosorbide-5-Nitrae-dihydroxyanthraquinone gas, is extracted in crystallisation chamber by vacuum system, condenses on crystallisation chamber inwall, the latent heat produced of sublimating
Heat exchange is carried out with sensible heat and cooling system；
After step 5) cooling terminates, close vacuum system, emptying, open cover, rewinding, weigh；Cleaning hopper does not distil residue,
Carrying out next batch production again, the residue that the most do not distils is entrusted has qualification unit to burn.
Described honeycomb fashion sublimating apparatus includes crystallizing tank body, heats tank body, cover, tube sheet, sublimation pipe, support plate and material
Groove；It is provided with crystallisation chamber in described crystallizer body；It is provided with heating chamber in described heating tank body；Described crystallization tank body one end leads to
Cross tube sheet to be connected with heating tank body non-close end；The described crystallization tank body other end is hinged with cover；Set on described tube sheet
There is honeycomb through hole；It is provided with support plate in described heating chamber；Described support plate is provided with the honeycomb through hole corresponding with tube sheet；Institute
The sublimation pipe stated is along heating tank body axis direction through honeycomb through hole and the honeycomb through hole of support plate of tube sheet；Described sublimation pipe
For hollow pipe；Described sublimation pipe is blind end through one end of support plate；The described sublimation pipe other end is non-close end；Institute
The hopper stated is placed in sublimation pipe；
The external side of described crystallizer is provided with cooling jacket；Cooling exchange it is provided with between described crystallization tank body and cooling jacket
Room；Described top, cooling jacket top is provided with and cools down the cooling water outlet pipe that switch room is connected；At the bottom of described cooling jacket
End bottom is provided with and cools down the cooling water inlet pipe that switch room is connected；The top, top of described crystallization tank body is provided through cooling
The vacuum connection tube of chuck；Described vacuum connection tube is connected with crystallisation chamber；Described vacuum connection tube is connected with vacuum system；
Described vacuum system is made up of the lobe pump of an oilless vacuum pump and two different speed of exhausts, makes distillation in fine vacuum
Run under (≤100 handkerchief) state.
Described heating top, tank body top is provided with the conduction oil flowline being connected with heating chamber；Described heating tank body is low
End bottom is provided with conduction oil drain line and conduction oil oil inlet pipe.
Described honeycomb through hole is made up of 37 circular holes, and by positive triangle arrangement.
The first half of described crystallization tank body cross section is quincunx or gear shape or semicircle, and lower half is semicircle.
Described hopper cross section is semicircle, and matches with sublimation pipe.
Beneficial effect of the present invention
1, the present invention provides method of purification, and without other industrial chemicals, also without chemical reaction, without waste water, a small amount of waste gas can lead to
Crossing activated carbon adsorption to remove, a small amount of waste residue is entrusted has qualification unit to burn, and basic three-waste free discharge carries with chemical method, solvent method
Pure not only product purity height (>=99%) of comparing, yield height (>=97%), and also more environmentally friendly, non-secondary pollution.
2, the heating surface (area) (HS of the sublimation apparatus of one group of 12 honeycomb fashion sublimating apparatuss composition is than a 1500L jacketed reactor
Big 12 times of formula sublimating apparatus heating surface (area) (HS；
3, using vacuum pump set ratio to use reciprocating vacuum pump evacuation, deflation rate is big, and vacuum is high.
Reaction autoclave sublimating apparatus, owing to there being stirring, needs mechanical seal, it is impossible to realize fine vacuum, typically 720 ~
Distil under 750mmHg, be equivalent to 5000 ~ 1300Pa distillation；Using vacuum pump set is in≤100Pa distillation；Vacuum improves number
Ten times, greatly speed up rate of sublimation.Production practices prove, improve vacuum ratio and improve temperature, to improving rate of sublimation more
Effectively.
4, the Overlay that honeycomb fashion sublimating apparatus and high vacuum condition combine is used；
Owing to heating surface is greatly improved, vacuum is greatly improved, the most once feed intake 400Kg: Xin Fa and old method exist following the brightest
Aobvious technique effect；
Sublimation time is greatly shortened, old method more than 24 hours, new method 4 hours, and monthly output improves 5 times.
Product yield is greatly improved, and hydroxy compounds structure is understable, and at high temperature easily dehydroxylation decomposes.New method is owing to adding
Hot side is big, and vacuum improves, and makes reduction sublimation temperature be possibly realized, and sublimation temperature is down to new method 220 by average 280 DEG C of old method
℃.Owing to sublimation temperature is greatly reduced, sublimation time shortens again, reduces and decomposes loss, and product yield is improved by old method average 85%
To new method 97%.
New method is energy-conservation, old method coal consumption 1000Kg, new method coal consumption 280Kg, old method power consumption 1500 degree, new method power consumption 300 degree, always
Energy consumption can save 70%.
New method solves the hard nut to crack that slagging-off is difficult, and old method typically uses vacuum sucking-off residue, and some residues are attached to
Still wall, stirring is difficult to sucking-off, and new method residue and residual exists in hopper, outwells.
Accompanying drawing explanation
Fig. 1 is that sublimed method of the present invention purifies 1,4-dihydroxyanthraquinone process flow diagram；
Fig. 2 is honeycomb fashion sublimating apparatus cross-sectional view of the present invention；
Fig. 3 is honeycomb fashion sublimating apparatus vacuum system of the present invention, cooling water and the turnover schematic diagram of conduction oil；
Fig. 4 is honeycomb fashion sublimating apparatus A-A section structure schematic diagram of the present invention；
Fig. 5 is honeycomb fashion sublimating apparatus B-B section structure schematic diagram of the present invention；
Fig. 6 is bin design schematic diagram of the present invention；
In figure: 1-crystallizes tank body；1.1-crystallisation chamber；1.2-cooling jacket；1.3-cools down switch room；2-heats tank body；2.1-pipe
Plate；2.2-sublimation pipe；2.3-support plate；2.4-heating chamber；3-cover；4-cooling water inlet pipe；5-cooling water outlet pipe；6-is true
Empty connecting tube；7-conduction oil drain line；8-conduction oil oil inlet pipe；9-conduction oil flowline.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
The present embodiment raw material is selected: technical grade 1,4-dihydroxyanthraquinone；Production unit: Asia, Jiangsu nation；Purity；94%, moisture :≤
1%, outward appearance is brick-red；Detection unit: Asia, Jiangsu nation；Feed intake Asia, Jiangsu nation 2015-6-25 batch；Feed intake quality 400Kg；
As it is shown in figure 1, the method for fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone, prepare as follows:
Step 1) feeds intake: is loaded by technical grade Isosorbide-5-Nitrae-dihydroxyanthraquinone in hopper, after compacting strikes off, puts into by 10 or 12
In the sublimation pipe of honeycomb fashion sublimating apparatus in parallel；
Described honeycomb fashion sublimating apparatus in parallel refers to the vacuum system on adjacent honeycomb fashion sublimating apparatus, heating system and cooling
System arranges according to parallel way；
Step 2) it is dehydrated, melts: to the technical grade Isosorbide-5-Nitrae-dihydroxyanthraquinone in sublimation pipe, carry out heating under non-vacuum condition, open
Opening heating system, temperature controls at 210 ~ 220 DEG C, and the time controls at 30min, after discharging water vapour, and capping；
Step 3) sublimation purification: open vacuum system and cooling system simultaneously, progressively make vacuum pressure control in 30min
Below 100pa, heating and temperature control is at 220 DEG C, and the time controls at 240min；The organic exhaust gas that vacuum system is discharged, passes through 15m
High aiutage, discharges after utilizing activated carbon adsorption；
Step 4) cooling is sublimated: sublimation purification and cooling are sublimated and carried out simultaneously, subliming by heating out high-purity in sublimation pipe
Isosorbide-5-Nitrae-dihydroxyanthraquinone gas, is extracted in crystallisation chamber by vacuum system, condenses on crystallisation chamber inwall, the latent heat produced of sublimating
Heat exchange is carried out with sensible heat and cooling system；
After step 5) cooling terminates, close vacuum system, emptying, open cover, rewinding, weigh；Cleaning hopper does not distil residue,
Carrying out next batch production again, the residue that the most do not distils is entrusted has qualification unit to burn.
After sublimation purification terminates, obtain the high-purity Isosorbide-5-Nitrae-dihydroxyanthraquinone of product；Purity 99.4%；Moisture 0.03%；Outward appearance is gorgeous
Red；Production unit: Xuzhou distils；Detection unit: Asia, Jiangsu nation；Weighing products Xuzhou distillation 2015-8-1 batch, rewinding claims
Weight 368Kg；
The present embodiment product yield calculates: material purity 94%, and after sublimation purification, purity is 99.4%, then product yield is:
≈97.28%。
Raw material, QPL (qualified products list), be shown in Table 1；Production technology and periodic chart (6 hours), be shown in Table 2.
Table 1
Table 2
| Operation | Inlet oil temperature DEG C | Vacuum system | Time (minute) | Remarks |
| Input and output material | 210~220 | Shut down | 60 | |
| Dehydration melting | 220 | Shut down | 30 | |
| Distillation | 220 | Three machines | 240 | |
| Cooling | 210 | Three machines | 30 |
Embodiment 2
The method of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone, honeycomb fashion sublimating apparatus used；
As shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5, described honeycomb fashion sublimating apparatus, it includes crystallizing tank body 1, heats tank body 2, cover
3, tube sheet 2.1, sublimation pipe 2.2, support plate 2.3 and hopper；It is provided with crystallisation chamber 1.1 in described crystallization tank body 1；Described heating
Heating chamber 2.4 it is provided with in tank body 2；Described crystallization tank body 1 one end is connected with heating tank body 2 non-close end by tube sheet 2.1；Institute
Crystallization tank body 1 other end stated is hinged with cover 3；Described tube sheet 2.1 is provided with honeycomb through hole；Described heating chamber 2.4
Inside it is provided with support plate 2.3；Described support plate 2.3 is provided with the through hole corresponding with tube sheet 2.1 honeycomb through hole；Described sublimation pipe
2.2 pass the honeycomb through holes of tube sheet 2.1 and the through hole of support plate 2.3 along heating tank body 2 axis direction；Described hopper is placed on
In sublimation pipe 2.2；
As in figure 2 it is shown, be provided with cooling jacket 1.2 outside described crystallization tank body 1；Described crystallization tank body 1 and cooling jacket 1.2
Between be provided with cooling switch room 1.3；Described top, cooling jacket 1.2 top is provided with and cools down the cooling that switch room 1.3 is connected
Water outlet pipe 5；Described bottom, cooling jacket 1.2 bottom is provided with and cools down the cooling water inlet pipe 4 that switch room 1.3 is connected；Institute
The top, top of the crystallization tank body 1 stated is provided through the vacuum connection tube 6 of cooling jacket 1.2；Described vacuum connection tube 6 and knot
Brilliant room 1.1 is connected；Described vacuum connection tube 6 is connected with vacuum system；
As in figure 2 it is shown, described heating top, tank body 2 top is provided with the conduction oil flowline 9 being connected with heating chamber 2.4；Described
Heating tank body 2 low side bottom be provided with conduction oil drain line 7 and conduction oil oil inlet pipe 8.
As it is shown in figure 5, described honeycomb through hole is made up of 37 circular holes, and by positive triangle arrangement.
As shown in Figure 4, the first half of described crystallization tank body 1 cross section is quincunx or gear shape or semicircle, lower half
Portion is semicircle.
Described sublimation pipe 2.2 is hollow pipe；Described sublimation pipe 2.2 is blind end through one end of support plate 2.3；Institute
Sublimation pipe 2.2 other end stated is non-close end.
As shown in Figure 6, described hopper cross section is semicircle, and matches with sublimation pipe 2.2.
Claims (6)
1. the method for fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone, it is characterised in that: prepare as follows:
Step 1) feeds intake: is loaded by technical grade Isosorbide-5-Nitrae-dihydroxyanthraquinone in hopper, after compacting strikes off, puts into by 10 or 12
In the sublimation pipe of honeycomb fashion sublimating apparatus in parallel；
Described honeycomb fashion sublimating apparatus in parallel refers to the vacuum system on adjacent honeycomb fashion sublimating apparatus, heating system and cooling
System arranges according to parallel way；
Step 2) it is dehydrated, melts: to the technical grade Isosorbide-5-Nitrae-dihydroxyanthraquinone in sublimation pipe, carry out heating under non-vacuum condition, open
Opening heating system, temperature controls at 210 ~ 220 DEG C, and the time controls at 30min, after discharging water vapour, and capping；
Step 3) sublimation purification: open vacuum system and cooling system simultaneously, progressively make vacuum pressure control in 30min
Below 100pa, heating and temperature control is at 220 DEG C, and the time controls at 240min；The organic exhaust gas that vacuum system is discharged, passes through 15m
High aiutage, discharges after utilizing activated carbon adsorption；
Step 4) cooling is sublimated: sublimation purification and cooling are sublimated and carried out simultaneously, subliming by heating out high-purity in sublimation pipe
Isosorbide-5-Nitrae-dihydroxyanthraquinone gas, is extracted in crystallisation chamber by vacuum system, condenses on crystallisation chamber inwall, the latent heat produced of sublimating
Heat exchange is carried out with sensible heat and cooling system；
After step 5) cooling terminates, close vacuum system, emptying, open cover, rewinding, weigh；Cleaning hopper does not distil residue,
Carrying out next batch production again, the residue that the most do not distils is entrusted has qualification unit to burn.
The method of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone the most according to claim 1, it is characterised in that: described
Honeycomb fashion sublimating apparatus, it include crystallize tank body (1), heating tank body (2), cover (3), tube sheet (2.1), sublimation pipe (2.2),
Board (2.3) and hopper；It is provided with crystallisation chamber (1.1) in described crystallization tank body (1)；It is provided with in described heating tank body (2) and adds
Hot cell (2.4)；Described crystallization tank body (1) one end is connected with heating tank body (2) non-close end by tube sheet (2.1)；Described
Crystallization tank body (1) other end is hinged with cover (3)；Described tube sheet (2.1) is provided with honeycomb through hole；Described heating chamber
(2.4) support plate (2.3) it is provided with in；Described support plate (2.3) is provided with the through hole corresponding with tube sheet (2.1) honeycomb through hole；
Described sublimation pipe (2.2) is along heating tank body (2) axis direction through the honeycomb through hole of tube sheet (2.1) and support plate (2.3)
Through hole；Described hopper is placed in sublimation pipe (2.2)；
Described crystallization tank body (1) outside is provided with cooling jacket (1.2)；Described crystallization tank body (1) and cooling jacket (1.2) it
Between be provided with cooling switch room (1.3)；Described cooling jacket (1.2) top, top is provided with and cools down what switch room (1.3) was connected
Cooling water outlet pipe (5)；Described cooling jacket (1.2) bottom, bottom is provided with and cools down the cooling water that switch room (1.3) is connected
Water inlet pipe (4)；The top, top of described crystallization tank body (1) is provided through the vacuum connection tube (6) of cooling jacket (1.2)；Institute
The vacuum connection tube (6) stated is connected with crystallisation chamber (1.1)；Described vacuum connection tube (6) is connected with vacuum system；
Described heating tank body (2) top, top is provided with the conduction oil flowline (9) being connected with heating chamber (2.4)；Described adds
Hot tank body (2) low side bottom is provided with conduction oil drain line (7) and conduction oil oil inlet pipe (8).
The method of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone the most according to claim 2, it is characterised in that: described
Honeycomb through hole be made up of 37 circular holes, and by positive triangle arrangement.
The method of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone the most according to claim 2, it is characterised in that: described
The first half of crystallization tank body (1) cross section be quincunx or gear shape or semicircle, lower half is semicircle.
The method of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone the most according to claim 2, it is characterised in that: described
Sublimation pipe (2.2) be hollow pipe；Described sublimation pipe (2.2) is blind end through one end of support plate (2.3)；Described liter
China's pipe (2.2) other end is non-close end.
The method of fine vacuum sublimation purification Isosorbide-5-Nitrae-dihydroxyanthraquinone the most according to claim 2, it is characterised in that: described
Hopper cross section be semicircle, and match with sublimation pipe (2.2).
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610253528.9A CN105884592A (en) | 2016-04-22 | 2016-04-22 | Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum |
| CN201710146185.0A CN106966885B (en) | 2016-04-22 | 2017-03-13 | Method for purifying 1, 4-dihydroxy anthraquinone by high vacuum sublimation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610253528.9A CN105884592A (en) | 2016-04-22 | 2016-04-22 | Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum |
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| CN201610253528.9A Pending CN105884592A (en) | 2016-04-22 | 2016-04-22 | Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum |
| CN201710146185.0A Expired - Fee Related CN106966885B (en) | 2016-04-22 | 2017-03-13 | Method for purifying 1, 4-dihydroxy anthraquinone by high vacuum sublimation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966885A (en) * | 2016-04-22 | 2017-07-21 | 马骋 | The method of the dihydroxy anthraquinone of high vacuum sublimation purification 1,4 |
| CN107376394A (en) * | 2017-08-04 | 2017-11-24 | 贵州自然生物科技有限公司 | Sublimed method pyrogallic acid automatically adjusts speed of exhaust retracting device |
| 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 |
| CN113604899A (en) * | 2021-09-08 | 2021-11-05 | 许绝电工股份有限公司 | Continuous production method of polyimide fibers |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109928925A (en) * | 2018-12-19 | 2019-06-25 | 重庆康乐制药有限公司 | The sublimation purification method of one kind 4,7- dichloroquinoline |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2637689C3 (en) * | 1976-08-21 | 1980-09-25 | Bayer Ag, 5090 Leverkusen | Process for cleaning swelling organic products |
| CN1092632C (en) * | 1999-11-15 | 2002-10-16 | 湖北楚源精细化工集团股份有限公司 | Process for preparing refined 1,4-dihydroxyl anthraquinone |
| CN103664567A (en) * | 2012-09-03 | 2014-03-26 | 彭泽兴达化工有限公司 | Novel process for producing 1,4-dihydroxy anthraquinone |
| CN105884592A (en) * | 2016-04-22 | 2016-08-24 | 马骋 | Method for purifying 1, 4-dihydroxy anthraquinone by sublimation under high vacuum |
-
2016
- 2016-04-22 CN CN201610253528.9A patent/CN105884592A/en active Pending
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2017
- 2017-03-13 CN CN201710146185.0A patent/CN106966885B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966885A (en) * | 2016-04-22 | 2017-07-21 | 马骋 | The method of the dihydroxy anthraquinone of high vacuum sublimation purification 1,4 |
| CN106966885B (en) * | 2016-04-22 | 2020-04-21 | 马骋 | Method for purifying 1, 4-dihydroxy anthraquinone by high vacuum sublimation |
| CN107376394A (en) * | 2017-08-04 | 2017-11-24 | 贵州自然生物科技有限公司 | Sublimed method pyrogallic acid automatically adjusts speed of exhaust retracting device |
| 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 |
| CN113604899A (en) * | 2021-09-08 | 2021-11-05 | 许绝电工股份有限公司 | Continuous production method of polyimide fibers |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106966885A (en) | 2017-07-21 |
| CN106966885B (en) | 2020-04-21 |
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Application publication date: 20160824 |