CN103274909A - High-purity dinaphthyl ether and preparation method thereof - Google Patents
High-purity dinaphthyl ether and preparation method thereof Download PDFInfo
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- CN103274909A CN103274909A CN2013102337528A CN201310233752A CN103274909A CN 103274909 A CN103274909 A CN 103274909A CN 2013102337528 A CN2013102337528 A CN 2013102337528A CN 201310233752 A CN201310233752 A CN 201310233752A CN 103274909 A CN103274909 A CN 103274909A
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Abstract
The invention relates to high-purity dinaphthyl ether and a preparation method thereof. Particularly, naphthalene halide and naphthol are taken as main raw materials and kept warm for 1-5 hours at a temperature of 80-180 DGE C in the presence of an acid-binding agent, a catalyst and a water absorbent, byproduct halide salt, unreacted raw materials, a liquid catalyst and the water absorbent are produced, the halide salt, the catalyst and the water absorbent are filtered, distillation and separation are performed, a fraction at the temperature of 250-255 DEG C is taken as the dinaphthyl ether, and the dinaphthyl ether with the purity larger than 99% is obtained.
Description
Technical field
The invention belongs to organic raw material intermediate manufacturing technology field, be specifically related to a kind of high purity dinaphthyl ether and preparation method thereof.
Background technology
This product dinaphthyl ether is important organic synthesis intermediate, can be used as the synthetic intermediate of products such as alkyl dinaphthyl ether and derivative thereof, medicine, industrial surface activity agent.I think that according to several years of product development and application experience this product will have purposes and market requirement situation more and more widely, so developed this product, product adopts Williamson's synthesis method to do the etherification reaction of this product, technology theory maturation, easy handling.
Summary of the invention
Goal of the invention: this product is gone and found out what's going on according to market, has increasing actual demand, but the reagent except import, difficulty sees that industrialization product appears on the market in market at home, for there is demand in this market of substituting but scale production is in the gaps in market of space state, for a kind of highly purified organic synthesis raw material dinaphthyl ether being provided for domestic chemical industrial enterprise, invented this product;
The invention provides a kind of preparation method of high purity dinaphthyl ether, specifically realize the present invention by following steps:
(1) adds 1-10mol naphthalene halide and 1-3mol naphthols successively to etherifying reactor, start stirring;
(2) add acid binding agent, water-retaining agent to etherifying reactor, nitrogen protection simultaneously, it is molten entirely to be stirred to acid binding agent at 30-100 ℃;
(3) add catalyzer under 80-180 ℃ of temperature condition, be incubated 1-5 hour, get the mixture of product dinaphthyl ether and by-product halogen and catalyzer, water-retaining agent;
(4) above-mentioned (3) are generated material filtering, filtering solid catalyst, halogen, water-retaining agent;
(5) above-mentioned (4) are leached material rectifying and get 250-255 ℃ of cut, get purity 99% above dinaphthyl ether product;
Effect of the present invention and benefit are:
(1) aspect synthetic technology: because the raw material boiling point is all higher, the process time of weak point is synthesized dinaphthyl ether, technology theory maturation under higher temperature to be beneficial to the etherificate route that adopts Williamson's synthesis method;
(2) aspect the economic benefit: not only select for domestic chemical enterprise provides many synthetic routes after this product production domesticization, and will purchase facility, economy.And because reaction is carried out easily, be conducive to obtain high product yield, market value such as the by-product Potassium Bromide of generation, Sodium Bromide are strong, and the added value height can two get at one stroke, and economic benefit is obvious;
(3) at the quality product aspect of performance: because the product purity height reaches more than 99%, be beneficial to the directly synthetic of Subscriber Unit, need not to purify again, improved production efficiency;
Embodiment further illustrates the present invention below by embodiment, and this embodiment only is the present invention is described and never limits the present invention:
Embodiment 1
Restraining naphthalene bromides with 600 is substrate, add about 30 grams of naphthols 114.16 grams and solid sodium hydroxide, add about 21 grams of solid potassium hydroxide, and under nitrogen protection, be heated to 80 ℃, to acid binding agent complete molten after, add anhydrous magnesium sulfate 8 grams, stirred 0.5 hour, add catalyzer cuprous chloride 10 grams, progressively be warming up to 180 ℃, react 1-5 as a child, reaction is entirely terminal point with naphthol reaction, the test reaction terminal point, after terminal point arrives, be cooled to 30-100 ℃ of filtration, remove copper salt catalyst and water-retaining agent, unreacted raw material is removed in the high temperature fractionation again, get the 250-255 cut and get dinaphthyl ether gram 269, products obtained therefrom purity is greater than 99%, and in naphthols, yield reaches more than 99%;
Embodiment 2
Restraining naphthalene chlorides with 500 is substrate; add about 30 grams of naphthols 114.16 grams and solid sodium hydroxide, add about 21 grams of solid potassium hydroxide, and under nitrogen protection, be heated to 80 ℃; to acid binding agent complete molten after; add anhydrous magnesium sulfate 8 grams, stirred 0.5 hour, add catalyzer cuprous chloride 10 grams; three (3; the 6-dioxo heptyl of mixing) amine 20 grams progressively are warming up to 180 ℃, and reaction 1-5 as a child; reaction is entirely terminal point with naphthol reaction; terminal point is cooled to 30-100 ℃ of filtration after arriving, and removes copper salt catalyst and water-retaining agent; the high temperature fractionation gets dinaphthyl ether gram 268 except getting the 250-255 cut again; products obtained therefrom purity is greater than 99%, and in naphthols, yield reaches more than 99%.
Claims (7)
1. high purity dinaphthyl ether and preparation method thereof is characterized in that comprising following synthesis step and processing condition:
(1) adds 1-10mol naphthalene halide and 1-3mol naphthols successively to etherifying reactor, start stirring;
(2) add acid binding agent, water-retaining agent to etherifying reactor, nitrogen protection simultaneously, it is molten entirely to be stirred to acid binding agent at 30-100 ℃;
(3) add catalyzer under 80-180 ℃ of temperature condition, be incubated 1-5 hour, get the mixture of product dinaphthyl ether and by-product halogen and catalyzer, water-retaining agent;
(4) above-mentioned (3) are generated material filtering, filtering solid catalyst, halogen, water-retaining agent;
(5) above-mentioned (4) are leached material rectifying and get 250-255 ℃ of cut, get purity 99% above dinaphthyl ether product.
2. a kind of high purity dinaphthyl ether according to claim 1 and preparation method thereof is characterized in that main raw material is: naphthalene halide, naphthols.
3. a kind of high purity dinaphthyl ether according to claim 1 and preparation method thereof is characterized in that: synthesis material naphthalene halide: naphthols: the mol ratio of acid binding agent is 1-10: 1-3: 1-3.
4. a kind of high purity dinaphthyl ether according to claim 1 and preparation method thereof, it is characterized in that: described naphthalene halide comprises: naphthalene chloride, naphthalene bromide, naphthalene iodide, naphthalene fluoride.
5. a kind of high purity dinaphthyl ether according to claim 1 and preparation method thereof, it is characterized in that: described acid binding agent can be sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate.
6. a kind of high purity dinaphthyl ether according to claim 1 and preparation method thereof, it is characterized in that: described catalyzer is: benzo pyridine quinoline or three (3,6-dioxo octyl) amine, three (3, the 6-dioxo heptane base of mixing) catalyzer of amine and mantoquita series, the catalyzer of mantoquita series can be the hydrosulfate of copper, the muriate of copper, the oxide compound of copper, and ingredient proportion is the 1-10% of naphthalene halide and naphthols total amount.
7. a kind of high purity dinaphthyl ether according to claim 1 and preparation method thereof, it is characterized in that: the described water-retaining agent of described dinaphthyl ether synthesis technique is the sulfation salt anhydride of magnesium, and dosage is the 1-10% of naphthalene halide and naphthols total amount.
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| CN2013102337528A CN103274909A (en) | 2013-06-13 | 2013-06-13 | High-purity dinaphthyl ether and preparation method thereof |
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| CN2013102337528A CN103274909A (en) | 2013-06-13 | 2013-06-13 | High-purity dinaphthyl ether and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1207092A (en) * | 1995-11-17 | 1999-02-03 | 拜尔公司 | Biphenyl ether oxazolines and their use as pest-control agents |
| CN101450958A (en) * | 2008-12-29 | 2009-06-10 | 天津理工大学 | Synthetic method of isoflavone 7-O-glucose glycoside |
| CN101948394A (en) * | 2010-09-20 | 2011-01-19 | 浙江博华化学有限公司 | Method for synthesizing tris(dioxa-3,6-heptyl)amine |
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2013
- 2013-06-13 CN CN2013102337528A patent/CN103274909A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1207092A (en) * | 1995-11-17 | 1999-02-03 | 拜尔公司 | Biphenyl ether oxazolines and their use as pest-control agents |
| CN101450958A (en) * | 2008-12-29 | 2009-06-10 | 天津理工大学 | Synthetic method of isoflavone 7-O-glucose glycoside |
| CN101948394A (en) * | 2010-09-20 | 2011-01-19 | 浙江博华化学有限公司 | Method for synthesizing tris(dioxa-3,6-heptyl)amine |
Non-Patent Citations (2)
| Title |
|---|
| YOKO SHIBASAKI ET AL.: "Decomposition reactions of plastic model compounds in sub- and supercritical water", 《POLYMER DEGRADATION AND STABILITY》, vol. 83, 31 December 2004 (2004-12-31), pages 481 - 485, XP004490474, DOI: doi:10.1016/j.polymdegradstab.2003.09.010 * |
| 陶英丕等: "常压法合成二苯醚", 《精细化工》, vol. 11, no. 3, 31 December 1994 (1994-12-31), pages 37 - 39 * |
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Application publication date: 20130904 |