CN102250060A - Preparation method of 2,4-diethyl thioxanthone - Google Patents
Preparation method of 2,4-diethyl thioxanthone Download PDFInfo
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- CN102250060A CN102250060A CN2011101404795A CN201110140479A CN102250060A CN 102250060 A CN102250060 A CN 102250060A CN 2011101404795 A CN2011101404795 A CN 2011101404795A CN 201110140479 A CN201110140479 A CN 201110140479A CN 102250060 A CN102250060 A CN 102250060A
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- diethyl thioxanthone
- diethylbenzene
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- salicylic acid
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Abstract
The invention relates to a preparation method of 2,4-diethyl thioxanthone. The preparation method of the 2,4-diethyl thioxanthone is characterized by finally obtaining a product, i.e. the 2,4-diethyl thioxanthone, through the processes of condensation, extraction, washing, caustic washing, distillation, dissolution and crystallization, centrifugation, drying, and the like by taking o-diethylbenzene and dithio-salicylic acid as main raw materials and sulphuric acid, toluene, sodium carbonate, methanol, and the like as auxiliary raw materials. The preparation method of the 2,4-diethyl thioxanthone, which is disclosed by the invention, has the advantages of higher yield reaching 85 percent through experimental determination, little acid pollution, easy aftertreatment, moderate reaction condition and capability of reducing the energy consumption because the distillation is not needed by the aftertreatment of the product.
Description
Technical field
The present invention relates to a kind of 2, the preparation method of 4-diethyl thioxanthone.
Background technology
2, the 4-diethyl thioxanthone is the important component part in the UV curing system.Can avoid the influence of pigment because it has long uv-absorbing wavelength, be applicable to that the UV that contains pigment is coating material solidified, in printing ink and the tackiness agent ultraviolet absorption.Prepare 2 in the prior art, directly use the vitriol oil more than 98% during the 4-diethyl thioxanthone, react more violent, cause the product color dark simultaneously, yield is low, and yield only is about 80%; And the aftertreatment of product need the distillation, technology is more complicated, the energy consumption height.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, provide that a kind of technology is more reasonable, productive rate is higher, acid pollution is little, aftertreatment is simple, reaction conditions is gentle 2, the preparation method of 4-diethyl thioxanthone.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of 2, the preparation method of 4-diethyl thioxanthone, be characterized in, its step is as follows: the vitriol oil that drips concentration be in an amount of water more than 98% is mixed with the vitriol oil that concentration is 88%-90%, diethylbenzene and dithio-salicylic acid between treating to add after temperature is reduced to 5 ℃, be incubated and be warming up to 85-95 ℃ of reaction 10-18 hour after 0.5-1.5 hour, temperature reduces to after 70 ℃ that to add weight ratio be that water and the toluene of 1:0.5-2 carries out extracting operation, branch vibration layer, organic phase is successively by washing and be not less than 30% liquid caustic soda with mass percent concentration and carry out alkali cleaning and remove spent acid, distill precipitation then, reclaim toluene; The thick product of gained is with 45-55 ℃ of dissolve with methanol, then reduces to below 10 ℃ product is separated out, and oven dry gets product after the centrifugation; The mass ratio of the raw material vitriol oil of participation reaction, a diethylbenzene, dithio-salicylic acid is 180:30-35:32-37.
Above-described 2, among the preparation method of 4-diethyl thioxanthone: the preferred mass of the raw material vitriol oil, a diethylbenzene, dithio-salicylic acid that participates in reaction is than being 180:32.8:35.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described 2, in preparation method's technical scheme of 4-diethyl thioxanthone, preferred technical characterictic is: between adding behind diethylbenzene and the dithio-salicylic acid, be incubated and be warming up to 90 ℃ of reactions 14 hours after 1 hour, temperature reduces to after 70 ℃ that to add weight ratio be that water and the toluene of 1:1 carries out extracting operation.
Principal reaction equation of the present invention is as follows:
Compared with prior art, the present invention 2, and the preparation method of 4-diethyl thioxanthone has the productive rate advantage of higher, can reach 85% through its productive rate of measuring, and acid pollution is little, aftertreatment is simple, reaction conditions temperature, product aftertreatment do not need distillation, have reduced energy consumption.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.A kind of 2, the preparation method of 4-diethyl thioxanthone, its step is as follows: dripping concentration and be the vitriol oil more than 98% in an amount of water, to be mixed with concentration be 88% the vitriol oil, diethylbenzene and dithio-salicylic acid between treating to add after temperature is reduced to 5 ℃, be incubated and be warming up to 85 ℃ of reactions 10 hours after 0.5 hour, temperature reduces to after 70 ℃ that to add weight ratio be that water and the toluene of 1:0.5 carries out extracting operation, branch vibration layer, organic phase is successively by washing and be not less than 30% liquid caustic soda with mass percent concentration and carry out alkali cleaning and remove spent acid, distill precipitation then, reclaim toluene; The thick product of gained is with 45 ℃ of dissolve with methanol, then reduces to below 10 ℃ product is separated out, and oven dry gets product after the centrifugation; The mass ratio of the raw material vitriol oil of participation reaction, a diethylbenzene, dithio-salicylic acid is 180:30:32.
Embodiment 2.A kind of 2, the preparation method of 4-diethyl thioxanthone, its step is as follows: dripping concentration and be the vitriol oil more than 98% in an amount of water, to be mixed with concentration be 90% the vitriol oil, diethylbenzene and dithio-salicylic acid between treating to add after temperature is reduced to 5 ℃, be incubated and be warming up to 95 ℃ of reactions 18 hours after 1.5 hours, temperature reduces to after 70 ℃ that to add weight ratio be that water and the toluene of 1:2 carries out extracting operation, branch vibration layer, organic phase is successively by washing and be not less than 30% liquid caustic soda with mass percent concentration and carry out alkali cleaning and remove spent acid, distill precipitation then, reclaim toluene; The thick product of gained is with 55 ℃ of dissolve with methanol, then reduces to below 10 ℃ product is separated out, and oven dry gets product after the centrifugation; The mass ratio of the raw material vitriol oil of participation reaction, a diethylbenzene, dithio-salicylic acid is 180:35:37.
Embodiment 3.A kind of 2, the preparation method of 4-diethyl thioxanthone, its step is as follows: dripping concentration and be the vitriol oil more than 98% in an amount of water, to be mixed with concentration be 89% the vitriol oil, diethylbenzene and dithio-salicylic acid between treating to add after temperature is reduced to 5 ℃, be incubated and be warming up to 90 ℃ of reactions 14 hours after 1 hour, temperature reduces to after 70 ℃ that to add weight ratio be that water and the toluene of 1:1 carries out extracting operation, branch vibration layer, organic phase is successively by washing and be not less than 30% liquid caustic soda with mass percent concentration and carry out alkali cleaning and remove spent acid, distill precipitation then, reclaim toluene; The thick product of gained is with 50 ℃ of dissolve with methanol, then reduces to below 10 ℃ product is separated out, and oven dry gets product after the centrifugation; The mass ratio of the raw material vitriol oil of participation reaction, a diethylbenzene, dithio-salicylic acid is 180:32.8:35.
Claims (3)
1. one kind 2, the preparation method of 4-diethyl thioxanthone, it is characterized in that, its step is as follows: the vitriol oil that drips concentration be in an amount of water more than 98% is mixed with the vitriol oil that concentration is 88%-90%, diethylbenzene and dithio-salicylic acid between treating to add after temperature is reduced to 5 ℃, be incubated and be warming up to 85-95 ℃ of reaction 10-18 hour after 0.5-1.5 hour, temperature reduces to after 70 ℃ that to add weight ratio be that water and the toluene of 1:0.5-2 carries out extracting operation, branch vibration layer, organic phase is successively by washing and be not less than 30% liquid caustic soda with mass percent concentration and carry out alkali cleaning and remove spent acid, distill precipitation then, reclaim toluene; The thick product of gained is with 45-55 ℃ of dissolve with methanol, then reduces to below 10 ℃ product is separated out, and oven dry gets product after the centrifugation; The mass ratio of the raw material vitriol oil of participation reaction, a diethylbenzene, dithio-salicylic acid is 180:30-35:32-37.
2. according to claim 12, the preparation method of 4-diethyl thioxanthone is characterized in that: participate in the raw material vitriol oil, a diethylbenzene of reaction, the mass ratio of dithio-salicylic acid is 180:32.8:35.
3. according to claim 12, the preparation method of 4-diethyl thioxanthone, it is characterized in that: between adding behind diethylbenzene and the dithio-salicylic acid, be incubated and be warming up to 90 ℃ of reactions 14 hours after 1 hour, temperature reduces to that to add weight ratio after 70 ℃ be that water and the toluene of 1:1 carries out extracting operation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101404795A CN102250060A (en) | 2011-05-27 | 2011-05-27 | Preparation method of 2,4-diethyl thioxanthone |
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| CN2011101404795A CN102250060A (en) | 2011-05-27 | 2011-05-27 | Preparation method of 2,4-diethyl thioxanthone |
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| CN2011101404795A Pending CN102250060A (en) | 2011-05-27 | 2011-05-27 | Preparation method of 2,4-diethyl thioxanthone |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558141A (en) * | 2012-02-23 | 2012-07-11 | 兰州石化职业技术学院 | Method for refining 2,4-diethyl thioxathone |
| CN102617538A (en) * | 2012-03-08 | 2012-08-01 | 南京大学 | Xanthone type small molecule with effect of broad spectrum regulation on micro ribonucleic acid and synthesis method and application thereof |
| CN108069935A (en) * | 2017-12-25 | 2018-05-25 | 天津瑞岭化工有限公司 | A kind of preparation method of 2,4- diethyl thioxanthones |
| CN108424409A (en) * | 2018-03-16 | 2018-08-21 | 吉安市东庆精细化工有限公司 | A kind of method of solid acid catalysis synthesis photoinitiator 2,4- diethyl thioxanthones |
| CN110845471A (en) * | 2019-11-20 | 2020-02-28 | 吉安市东庆精细化工有限公司 | Process for synthesizing photoinitiator 2,4-diethyl thioxanthone by one-pot method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4450279A (en) * | 1981-03-16 | 1984-05-22 | Nippon, Kayaku, Kabushiki, Kaisha | Dialkylthioxanthones |
-
2011
- 2011-05-27 CN CN2011101404795A patent/CN102250060A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4450279A (en) * | 1981-03-16 | 1984-05-22 | Nippon, Kayaku, Kabushiki, Kaisha | Dialkylthioxanthones |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558141A (en) * | 2012-02-23 | 2012-07-11 | 兰州石化职业技术学院 | Method for refining 2,4-diethyl thioxathone |
| CN102617538A (en) * | 2012-03-08 | 2012-08-01 | 南京大学 | Xanthone type small molecule with effect of broad spectrum regulation on micro ribonucleic acid and synthesis method and application thereof |
| CN108069935A (en) * | 2017-12-25 | 2018-05-25 | 天津瑞岭化工有限公司 | A kind of preparation method of 2,4- diethyl thioxanthones |
| CN108424409A (en) * | 2018-03-16 | 2018-08-21 | 吉安市东庆精细化工有限公司 | A kind of method of solid acid catalysis synthesis photoinitiator 2,4- diethyl thioxanthones |
| CN110845471A (en) * | 2019-11-20 | 2020-02-28 | 吉安市东庆精细化工有限公司 | Process for synthesizing photoinitiator 2,4-diethyl thioxanthone by one-pot method |
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Application publication date: 20111123 |