CN103305024A - High-yield preparation process of yellow dye for coloring of electronic liquid crystal material - Google Patents
High-yield preparation process of yellow dye for coloring of electronic liquid crystal material Download PDFInfo
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- CN103305024A CN103305024A CN2013101058876A CN201310105887A CN103305024A CN 103305024 A CN103305024 A CN 103305024A CN 2013101058876 A CN2013101058876 A CN 2013101058876A CN 201310105887 A CN201310105887 A CN 201310105887A CN 103305024 A CN103305024 A CN 103305024A
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Abstract
The invention relates to a high-yield manufacturing process of a yellow dye for coloring of an electronic liquid crystal material. The ratio of 1,8-anhydride naphthalene to liquid chlorine to 2,4-dimethylaniline to liquid ammonia is 1:(1-1.5):(1-2):(2-3). The preparation process disclosed by the invention comprises the steps of: forming anhydride from the1,8-anhydride naphthalene by chlorination under an alkaline condition, wherein the III chlorination temperature is 5-20 DEG C; carrying out imidization acetic acid serving as a solvent and the 2,4-dimethylaniline, wherein the reaction temperature is 116-120 DEG C, and the time is 8-14 hours; leading the liquid ammonia by taking n-amyl alcohol as a solvent under high temperature and high pressure under the condition that a catalyst is not needed; and reacting to directly obtain solvent yellow 44, wherein the temperature is 200-230 DEG C, the pressure is 3.5-6 MPA, and the time is 6-14 hours. The obtained solvent yellow 44 is over 96% in content, does not need to refine, and is high in yield; and the yield can be up to 85% and over 10% higher than that of the other processes. The high-yield preparation process has the advantages that compared with the traditional process, the high-yield preparation process is high in yield, low in cost and small in consumption and pollution; n-amyl alcohol with a high boiling point is adopted as the solvent to remove a one-step refining process.
Description
Technical field
The present invention relates to painted, azoic dyestuff intermediate, the preparation high-visibility pigment of electronic liquid crystal material.
Background technology
Existing 1, acenaphthene is nitrated, oxidation, reduction, imidization method
2, the 4-bromo-1,8-naphthalene acid anhydride imidization ammonolysis process
3, the 4-bromo-1,8-naphthalene acid anhydride imidization ammonolysis process
The quality of more several techniques, acenaphthene is nitrated, oxidation, reduction, imidization method, and oxygenant dichromate or permanganate are poisonous, adopt iron powder reducing, and aftertreatment difficulty cost is high.
4-bromo-1,8-naphthalene acid anhydride imidization ammonolysis process and 4-bromo-1,8-naphthalene acid anhydride imidization ammonolysis process, because needing to add catalyzer copper or cuprous chloride in the ammonia solution, solvent DMF required in the purification reclaims difficulty, and environmental hazard is large and yield is not high.
Summary of the invention
In order to overcome defects, the purpose of this invention is to provide a kind of high yield manufacturing process for the painted yellow dye of electronic liquid crystal material.
To achieve these goals, the present invention adopts following technical scheme:
A kind of high yield manufacturing process for the painted yellow dye of electronic liquid crystal material: 1,8-naphthalene acid anhydride: liquid chlorine: 2,4-xylidine: liquefied ammonia=1:1-1.5:1-2:2-3.Preparation technology of the present invention is: adopt 1,8 naphthalene acid anhydrides become acid anhydride through chlorination under alkaline condition, III chlorination temperature 5-20 degree, carry out imidization, its temperature of reaction 116-120 degree take acetic acid as solvent with 2,4-xylidine again, time 8-14 hour, need not to pass into liquefied ammonia take Pentyl alcohol under the solvent High Temperature High Pressure under the condition of catalyzer, reaction directly obtains solvent yellow 44, its temperature 200-230 degree, pressure 3.5 to 6MPA, 6 to 14 hours.Solvent yellow 44 content that obtain need not to make with extra care more than 96%, and yield is higher, reaches 85%, and are higher more than 10% than the yield of other techniques.
1, selects suitable solvent, improve purity and the yield of product.
2, select suitable temperature, be beneficial to react optimization, improve yield and production efficiency.
3, select suitable proportioning raw materials and pressure parameter, improve positive reaction speed, ammonification need not under the condition of catalyzer, and reaction obtains content and need not the bloom 44 made with extra care more than 96%.
?
Advantage of the present invention is: compare with traditional technology, having that yield is high, cost is not high and adopted the relatively high Pentyl alcohol of boiling point is that solvent has saved again an one-step refining, energy consumption and pollute all less.
Embodiment
Further specify below by embodiment:
Embodiment 1, a kind of high yield manufacturing process for the painted yellow dye of electronic liquid crystal material, 1,8-naphthalene acid anhydride: liquid chlorine: 2,4-xylidine: liquefied ammonia=1:1-1.5:1-2:2-3.Preparation technology of the present invention is: adopt 1,8 naphthalene acid anhydrides become acid anhydride through chlorination under alkaline condition, chlorination temperature 5-20 degree, again take acetic acid as solvent with 2, the 4-xylidine carries out imidization, its temperature of reaction 116-120 degree time 8-14 hour, need not to pass into liquefied ammonia take Pentyl alcohol under the solvent High Temperature High Pressure under the condition of catalyzer, reaction directly obtains solvent yellow 44, its temperature 200-230 degree, pressure 3.5 to 6MPA, 6 to 14 hours.Solvent yellow 44 content that obtain need not to make with extra care more than 96%, and yield is higher, reaches 85%, and are higher more than 10% than the yield of other techniques.
Claims (1)
1. high yield manufacturing process that is used for the painted yellow dye of electronic liquid crystal material, it is characterized in that: 1,8-naphthalene acid anhydride: liquid chlorine: 2,4-xylidine: liquefied ammonia=1:1-1.5:1-2:2-3, preparation technology of the present invention is: adopt 1,8 naphthalene acid anhydrides become acid anhydride through chlorination under alkaline condition, III chlorination temperature 5-20 degree, carry out imidization, its temperature of reaction 116-120 degree take acetic acid as solvent with 2,4-xylidine again, time 8-14 hour, need not to pass into liquefied ammonia take Pentyl alcohol under the solvent High Temperature High Pressure under the condition of catalyzer, reaction directly obtains solvent yellow 44, its temperature 200-230 degree, pressure 3.5 to 6MPA, 6 to 14 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101058876A CN103305024A (en) | 2013-03-29 | 2013-03-29 | High-yield preparation process of yellow dye for coloring of electronic liquid crystal material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101058876A CN103305024A (en) | 2013-03-29 | 2013-03-29 | High-yield preparation process of yellow dye for coloring of electronic liquid crystal material |
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| CN103305024A true CN103305024A (en) | 2013-09-18 |
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| CN2013101058876A Pending CN103305024A (en) | 2013-03-29 | 2013-03-29 | High-yield preparation process of yellow dye for coloring of electronic liquid crystal material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3895944A (en) * | 1972-08-14 | 1975-07-22 | Hoechst Ag | Electrophotographic recording material having a layered structure of charge generating and charge transport layers |
| US3992205A (en) * | 1973-10-26 | 1976-11-16 | Hoechst Aktiengesellschaft | Electrophotographic recording material containing a plurality of dyes with different spectral absorbtion characteristics |
| JP2007069527A (en) * | 2005-09-08 | 2007-03-22 | General Technology Kk | Heat-sensitive transfer medium |
-
2013
- 2013-03-29 CN CN2013101058876A patent/CN103305024A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3895944A (en) * | 1972-08-14 | 1975-07-22 | Hoechst Ag | Electrophotographic recording material having a layered structure of charge generating and charge transport layers |
| US3992205A (en) * | 1973-10-26 | 1976-11-16 | Hoechst Aktiengesellschaft | Electrophotographic recording material containing a plurality of dyes with different spectral absorbtion characteristics |
| JP2007069527A (en) * | 2005-09-08 | 2007-03-22 | General Technology Kk | Heat-sensitive transfer medium |
Non-Patent Citations (5)
| Title |
|---|
| 《现代化工》 19970420 严宏宾等 6,7-二氨基-2-(2',4'-二甲基)苯基-1H-苯并[de]异喹啉-1,3(2H)-二酮的合成 25-27 1 , 第04期 * |
| 严宏宾等: "6,7-二氨基-2-(2′,4′-二甲基)苯基-1H-苯并[de]异喹啉-1,3(2H)-二酮的合成", 《现代化工》, no. 04, 20 April 1997 (1997-04-20), pages 25 - 27 * |
| 严宏宾等: "C.I.溶剂黄44的合成工艺改进", 《染料工业》, vol. 34, no. 01, 15 February 1997 (1997-02-15) * |
| 周增勇: "C.I.溶剂染料黄44工业化合成技术研究", 《浙江工业大学硕士学位论文》, 1 April 2011 (2011-04-01), pages 22 * |
| 王鹏等: "C.I.溶剂黄44清洁合成工艺的研究", 《染料与染色》, vol. 45, no. 01, 26 February 2008 (2008-02-26), pages 11 - 13 * |
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Application publication date: 20130918 |