CN1683305A - Method for closed-ring synthesizing anthraquinone from o-benzoylbenzoic acid - Google Patents
Method for closed-ring synthesizing anthraquinone from o-benzoylbenzoic acid Download PDFInfo
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- CN1683305A CN1683305A CN 200410012233 CN200410012233A CN1683305A CN 1683305 A CN1683305 A CN 1683305A CN 200410012233 CN200410012233 CN 200410012233 CN 200410012233 A CN200410012233 A CN 200410012233A CN 1683305 A CN1683305 A CN 1683305A
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- benzoylbenzoic acid
- ring
- anthraquinone
- closed loop
- closure reaction
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Abstract
The process of close-ring synthesizing anthraquinone from o-benzoylbenzoic acid includes the following steps: A. heating o-benzoylbenzoic acid in close-ring reactor to eliminating surface water; B. adding fuming sulfuric acid with SO3 content of 16-24 % in 1.3-1.8 times weight of o-benzoylbenzoic acid and close-ring reaction at 138-200 deg.c for 1 hr; C. separating the reaction product in separating reactor, filtering, water washing, drying, etc. to obtain dry anthraquinone product. The present invention has less sulfuric acid consumption, low production cost, less exhausted waste acid, low power consumption and short reaction time.
Description
Technical field
The present invention relates to a kind of synthetic method of anthraquinone, specifically a kind of method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop.
Background technology
Anthraquinone is widely used in the DYE PRODUCTION enterprise as a kind of dyestuff intermediate.In the prior art, the synthesis technique of anthraquinone is that o-benzoylbenzoic acid is dropped into the ring-closure reaction still, after reactor temperature risen to 131 ℃, warming while stirring to 140 ℃, the surface water of confirming o-benzoylbenzoic acid has evaporated totally, extraordinarily going into concentration by 2.5 of o-benzoylbenzoic acid dry weight is 98% sulfuric acid, after adding temperature is risen to 138 ℃, is incubated 1 hour and gets final product.And then with resultant of reaction move to the segregation reactor in, thin up.Again products therefrom is moved to the suction strainer cylinder at last, after filtration, be washed to neutrality, be drying to obtain the dry product anthraquinone with the ordinary method discharging again.In this technology, the vitriolic usage quantity is big, not only causes the production cost height, and the sulfur waste acid number amount that produces in producing is also more relatively, the waste disposal cost of postorder is strengthened, and the one-tenth colour cast of gained anthraquinone is dark.
Summary of the invention
Purpose of the present invention is exactly that a kind of method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop will be provided, to reduce production costs improve production efficiency and product quality under the existing installation condition.
Method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop of the present invention realizes by following processing step:
A, o-benzoylbenzoic acid is dropped in the ring-closure reaction still, technology heats up and is incubated to o-benzoylbenzoic acid surface moisture content evaporate to dryness routinely;
B, in the ring-closure reaction still, add weight be o-benzoylbenzoic acid weight 1.3-1.8 doubly, SO
3Content be the oleum of 16-24%, add the back between 138 ℃-200 ℃, carry out 1 hour ring-closure reaction;
C, B is gone on foot products therefrom in the closed loop reactor moves into the segregation reactor, emanate, more after filtration, water Xian, drying and other steps promptly get the dry product anthraquinone.
In the method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop of the present invention, in reactor, add SO
3Content be the oleum of 16-24% after because reaction is violent, reacting liquid temperature rises to 175-180 ℃ rapidly, treat that oleum adds after, need not temperature control, reacting liquid temperature can remain between 138 ℃-200 ℃ voluntarily, carries out 1 hour ring-closure reaction.The add-on of oleum is 1.3-1.8 a times of o-benzoylbenzoic acid weight, is preferably 1.4-1.6 times of o-benzoylbenzoic acid weight.SO in the oleum
3Content be preferably 18-22%, more preferably 20%.
, B is gone on foot products therefrom put into the segregation reactor from the closed loop reactor and emanate by the o-benzoylbenzoic acid closed loop in the method for synthetic anthraquinone of the present invention, more after filtration, water Xian, drying and other steps promptly get the dry product anthraquinone.B is gone on foot products therefrom from the closed loop reactor put into the segregation reactor process, because the gained reactant concn is higher, denseness is bigger, therefore adopt with the air pump pressing mode ring-closure reaction still products therefrom is pressed in the segregation reactor, just obviously accelerated dispensing speed thus, the blowing time is shortened, enhance productivity.
In the method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop of the present invention, adopt SO
3Content be that to replace concentration be that 98% sulfuric acid carries out ring-closure reaction for the oleum (being commonly called as " 104 acid ") of 16-24%, its consumption only is 60% of 98% vitriol oil consumption, therefore not only reduced production cost, also reduce the quantity discharged of spent acid, correspondingly also reduced the cost of spent acid recycling in the subsequent handling.In addition, because the reaction of the vitriol oil of 104 acid ratios 98% is more strong, more impurity can be removed through oxidation, so just make that also the quality of gained dry product anthraquinone is better.Be exactly that therefore, the temperature of reaction solution can increase because the adding of 104 acid makes that the reaction of ring-closure reaction is more violent, and thermal discharge is more in addition.Like this, not only save original heating process process, saved the energy, and saved the time of heating up, correspondingly shortened the reaction times, improved production efficiency.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1:
Get moisture 10% commercially available o-benzoylbenzoic acid 1000kg and put into the ring-closure reaction still, warming while stirring to 140 ℃ is incubated 25 minutes again, makes the water evaporates on o-benzoylbenzoic acid surface clean.Cool the temperature to 125 ℃, add SO again
3Content is 17% oleum 1620kg (for 1.8 times of o-benzoylbenzoic acid dry weight).After adding, exothermic heat of reaction can make temperature rise to 178 ℃, carries out 1 hour ring-closure reaction subsequently.Products therefrom is got the yellowish dry product anthraquinone 738.4kg of color through segregation, filtration, water Xian, the drying and other steps of routine, and content is 99.05%.
Embodiment 2:
Get moisture 10% commercially available o-benzoylbenzoic acid 1000kg and put into the ring-closure reaction still, warming while stirring to 140 ℃ is incubated 25 minutes again, makes the water evaporates on o-benzoylbenzoic acid surface clean.Cool the temperature to 125 ℃, add SO again
3Content is 22% oleum 1350kg (for 1.5 times of o-benzoylbenzoic acid dry weight).After adding, temperature rises to 179 ℃, carries out 1 hour ring-closure reaction subsequently.Again through processing steps such as the segregation of routine, filtration, water Xian, dryings, get final product the yellowish dry product anthraquinone 778.8kg of color, content is 99.07%.
Embodiment 3:
Get moisture 10% commercially available o-benzoylbenzoic acid 1000kg and put into the ring-closure reaction still, warming while stirring to 140 ℃ is incubated 25 minutes again, makes the water evaporates on o-benzoylbenzoic acid surface clean.Cool the temperature to 125 ℃, add SO again
3Content is 20% oleum 1440kg (for 1.6 times of o-benzoylbenzoic acid dry weight).After adding, temperature rises to 179 ℃, carries out 1 hour ring-closure reaction subsequently.Reaction finishes, and utilizes air pump that products therefrom in the ring-closure reaction still is pressed in the segregation reactor, and segregation, filtration, water Xian, the drying and other steps through routine gets the yellowish dry product anthraquinone 791.2kg of color again, and content is 99.09%.
Comparative example 1:
Get moisture 10% commercially available o-benzoylbenzoic acid 1000kg and put into the ring-closure reaction still, warming while stirring to 140 ℃ is incubated 25 minutes again, makes the water evaporates on o-benzoylbenzoic acid surface clean.Cool the temperature to 125 ℃, add concentration again and be 98% sulfuric acid 2250kg (o-benzoylbenzoic acid dry weight 2.5 times).After adding, temperature is 118 ℃, and temperature is risen to 140 ℃, is incubated 1 hour and carries out ring-closure reaction, and products therefrom is got the yellowish dry product anthraquinone 773.4kg of color through segregation, filtration, water Xian, the drying and other steps of routine, and content is 99.03%.
Claims (5)
1, a kind of method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop is characterized in that the processing step of this method is:
A, o-benzoylbenzoic acid is dropped in the ring-closure reaction still, technology heats up and is incubated to o-benzoylbenzoic acid surface moisture content evaporate to dryness routinely;
B, in the ring-closure reaction still, add weight be o-benzoylbenzoic acid weight 1.3-1.8 doubly, SO
3Content be the oleum of 16-24%, add the back between 138 ℃-200 ℃, carry out 1 hour ring-closure reaction;
C, B is gone on foot products therefrom in the closed loop reactor moves into the segregation reactor, emanate, more after filtration, water Xian, drying and other steps promptly get the dry product anthraquinone.
2, the method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop as claimed in claim 1 is characterized in that the B 1.4-1.6 that the add-on of oleum is preferably o-benzoylbenzoic acid weight in the step doubly.
3, the method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop as claimed in claim 2 is characterized in that SO in the oleum
3The preferred of content be 18-22%.
4, the method by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop as claimed in claim 3 is characterized in that SO in the oleum
3Content more preferably 20%.
5,, it is characterized in that C was pressed into ring-closure reaction still products therefrom in the segregation reactor with pressuring method in the step as claim 1,2,3 or 4 described methods by the synthetic anthraquinone of o-benzoylbenzoic acid closed loop.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012233 CN1683305A (en) | 2004-04-16 | 2004-04-16 | Method for closed-ring synthesizing anthraquinone from o-benzoylbenzoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012233 CN1683305A (en) | 2004-04-16 | 2004-04-16 | Method for closed-ring synthesizing anthraquinone from o-benzoylbenzoic acid |
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| CN1683305A true CN1683305A (en) | 2005-10-19 |
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| CN 200410012233 Pending CN1683305A (en) | 2004-04-16 | 2004-04-16 | Method for closed-ring synthesizing anthraquinone from o-benzoylbenzoic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241579A (en) * | 2011-07-07 | 2011-11-16 | 辽宁石油化工大学 | Method for synthesizing anthraquinone |
| CN106045838A (en) * | 2016-06-04 | 2016-10-26 | 江阴市长江化工有限公司 | 2-EAQ (2-ethylanthraquinone) synthesis device and technology |
-
2004
- 2004-04-16 CN CN 200410012233 patent/CN1683305A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241579A (en) * | 2011-07-07 | 2011-11-16 | 辽宁石油化工大学 | Method for synthesizing anthraquinone |
| CN102241579B (en) * | 2011-07-07 | 2014-04-16 | 辽宁石油化工大学 | Method for synthesizing anthraquinone |
| CN106045838A (en) * | 2016-06-04 | 2016-10-26 | 江阴市长江化工有限公司 | 2-EAQ (2-ethylanthraquinone) synthesis device and technology |
| CN106045838B (en) * | 2016-06-04 | 2019-02-01 | 江阴市长江化工有限公司 | The synthesizer and technique of 2- ethyl hydrazine |
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