CN1065227C - Process for refining 2, 6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing - Google Patents
Process for refining 2, 6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing Download PDFInfo
- Publication number
- CN1065227C CN1065227C CN97122008A CN97122008A CN1065227C CN 1065227 C CN1065227 C CN 1065227C CN 97122008 A CN97122008 A CN 97122008A CN 97122008 A CN97122008 A CN 97122008A CN 1065227 C CN1065227 C CN 1065227C
- Authority
- CN
- China
- Prior art keywords
- dimethylnaphthalene
- refining
- technology
- present
- crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a technique for refining 2, 6-dimethylnaphthalene by an emulsion-crystallization method by stepwise temperature rise, which belongs to the field of the fine chemical industry of coal, and mainly solves the problems of the prior art for refining the 2, 6-dimethylnaphthalene, such as low yield of the 2, 6-dimethylnaphthalene and high production cost. The technique of the present invention is characterized in that water is used as a continuous phase, crude 2, 6-dimethylnaphthalene and water are emulsified into emulsion by stir under the actions of heating and a special emulsifying agent, and product is obtained by refrigeration, separation, washing and drying. The present invention has the advantages of simple technique and convenient operation, and the raw material of the crude 2, 6-dimethylnaphthalene with the purity over 33% can be easily refined into the refined 2, 6-dimethylnaphthalene with the purity over 96%; because tap water is used for replacing organic solvent, production cost is reduced, the yield of the refined 2, 6-dimethylnaphthalene is raised, and the work environment of workers is considerably improved; therefore, the present invention has high economical benefit and high social benefit.
Description
The present invention's emulsification crystallization that progressively heats up is refining 2, and 6-dimethylnaphthalene technology belongs to the coal field of fine chemical, relates to a kind ofly from from thick 2 the coal tar, and it is smart 2 that 6-dimethylnaphthalene feed purification becomes, the technology of 6-dimethylnaphthalene.
2, the 6-dimethylnaphthalene is an important source material of synthesizing new fragrance superpolymer, after its oxidation 2, the polyoxyethylene glycol naphthalene ester (PEN) that 6 naphthalene dicarboxylic acids and ethylene glycol polymerization make is a kind of new polyester type high polymer material, it is compared with the polyethyleneterephthalate (PET) that is widely used in manufacturing gear, building slab, fiber, film, beverage bottle etc. now, its intensity, elasticity are higher, thermotolerance is better, the video tape base band made from PEN, not only tough but also thin, thus audio-video time of unit mass (volume) increased.To 2, introduce after the functional group for 2,6 of the 6-dimethylnaphthalene, as the raw material of liquid crystalline polymers, also caused extensive attention, for example the polymkeric substance of 2-hydroxyl-6-naphthoic acid and P-hydroxy-benzoic acid reaction generation.Because such liquid crystalline polymers has height-oriented property as crystal in molten state, having high strength, snappiness, is a kind of new type functional macromolecular material that has good prospects, as the raw material of these novel high polymer materials, require 2, the 6-dimethylnaphthalene reaches the above purity of 95wt%.
At present both at home and abroad known 2,6-dimethylnaphthalene process for purification has: traditional crystallization process, absorption method (JP 5301830), absorption-crystallization process (JP 426635), rectifying-recrystallization method (GB 2247026A), complexing crystallization process (JP 578264), pressure crystallization process etc.But absorption-pressure crystallization process is to the equipment requirements height, though distillation-recrystallization method technology is simple, easy to operate, solvent can be recycled, and still has essence 2, problems such as 6-dimethylnaphthalene product yield is low, solvent loss is big, production cost height.Shortcomings such as the complexing crystallization process exists 2, and the purity of 6-dimethylnaphthalene and the rate of recovery are all lower.
The present invention's emulsification crystallization refining 2 that progressively heats up, 6-dimethylnaphthalene technology, purpose are to solve and have production cost height, essence 2, the problem that 6-dimethylnaphthalene product yield is low in the existing technology, providing a kind of is that the progressively emulsification crystallization of external phase is refining 2 with water, 6-dimethylnaphthalene technology.
The present invention's emulsification crystallization refining 2 that progressively heats up, 6-dimethylnaphthalene technology, it is characterized in that: it be a kind of with water as external phase, the HLB value greater than 12 negatively charged ion, nonionic, positively charged ion, amphoterics or their mixture effect under, progressively with thick 2,6-dimethylnaphthalene and water and milk change into milk sap, and then through separating preparation smart 2, the technology of 6-dimethylnaphthalene, its technological process divide three steps to finish.The first step is the preparation of emulsifier solution, and second step was the preparation of milk sap, and the 3rd step was an essence 2, the preparation of 6-dimethylnaphthalene.At first with tap water or distilled water preparation emulsifier solution, the content of emulsifying agent is 0.05-3%.What will make from coal tar wash oil then is thick 2, and 6-dimethylnaphthalene and emulsifier solution mix, and is emulsified into milk sap through stirring progressively to heat up under heating, and temperature rise rate is 2-10 ℃/min, and final emulsifying temperature is at 80-100 ℃.Be cooled to room temperature making milk sap at last, obtain product through separation, washing, drying.
Emulsifier content in the aqueous solution of the first step preparation is 0.05-3%.
In the emulsion that forms in second step 2, the content of 6-dimethylnaphthalene is 5-20%.
In order to confirm the effect of technology of the present invention better, be illustrated with specific examples below.Use in the experiment thick 2, the 6-dimethylnaphthalene be that 260-265 ℃ of boiling range dimethylnaphthalene cut and M-NITROBENZOIC ACID complexing obtain in the washing oil thick 2, the 6-dimethylnaphthalene, thick 2,6-dimethylnaphthalene raw material and dried smart 2, the 6-dimethylnaphthalene is all by gas-chromatography (GC), use import pure 2,6-dimethylnaphthalene (Japan) calculates essence 2, the purity of 6-dimethylnaphthalene and yield for standard substance carries out quantitatively.
Embodiment 1:
Aqueous formulation: emulsifying agent: Sodium dodecylbenzene sulfonate 0.5g
Water: tap water 50ml
Emulsion ratio: thick 2,6-dimethylnaphthalene (purity 33.3%) the 5g aqueous solution: 50ml
Emulsifying temperature progressively heats up: the temperature rise rate from 16 ℃ to 90 ℃: 6 ℃/min
Gained essence 2,6-dimethylnaphthalene: 1.7g essence 2,6-dimethylnaphthalene purity: 96.50%
Essence 2,6-dimethylnaphthalene yield: 98.53%
Embodiment 2:
Aqueous formulation: emulsifying agent: OP-10 1.5ml
Water: tap water 112ml
Emulsion ratio: thick 2,6-dimethylnaphthalene (purity 33.3%) the 5.6g aqueous solution: 113.5ml
Emulsifying temperature progressively heats up: the temperature rise rate .4 ℃/min from 15 ℃ to 80 ℃
Gained essence 2,6-dimethylnaphthalene: 1.7g essence 2,6-dimethylnaphthalene purity: 97.01%
Essence 2,6-dimethylnaphthalene yield: 88.42%
By embodiment as seen, technology of the present invention can be easily content thick 2 more than 33%, more than the 6-dimethylnaphthalene feed purification to 97%, product yield surpasses 88%.
Process for refining 2,6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing of the present invention, with water as continuously Phase selects the HLB value greater than 12 surfactant, with thick 2, and the progressively emulsification of 6-dimethylnaphthalene and water After becoming emulsion, make smart 2,6-dimethylnaphthalene product through refrigerated separation. Do not use organic molten in the production Agent, have that process equipment is simple, processing ease, smart 2,6-dimethylnaphthalene yield height, production cost are low, The characteristics such as constant product quality is free from environmental pollution have very high economic benefit and social benefit.
Claims (4)
1. the emulsification crystallization that progressively heats up is refining 2,6-dimethylnaphthalene technology, and it divides three steps, and the first step is mixed with emulsifier aqueous solution with the HLB value greater than 12 negatively charged ion or nonionogenic tenside with tap water or distilled water; Second step was thick 2 with what make from coal tar, and 6-dimethylnaphthalene and emulsifier aqueous solution mix, and make milk sap through stirring under the heating rate of 2-10 ℃/min, and whole emulsification times was at 10-40 minute, and final emulsifying temperature is 80-100 ℃; The 3rd step was that the milk sap that second step prepared is cooled to room temperature, and separation, washing, drying obtain product.
2. refining 2 according to the described emulsification crystallization that progressively heats up of claim 1,6-dimethylnaphthalene technology is characterized in that the emulsifier content in the aqueous solution of described the first step preparation is 0.05-3%.
3. refining 2 according to the described emulsification crystallization that progressively heats up of claim 1,6-dimethylnaphthalene technology is characterized in that in the milk sap that described second step forms 2, and 6-dimethylnaphthalene content is 5-20%.
4. make with extra care 2 according to the described emulsification crystallization that progressively heats up of claim 1,6-dimethylnaphthalene technology, wherein anion surfactant is a Sodium dodecylbenzene sulfonate, nonionogenic tenside is an alkylphenol polyoxyethylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97122008A CN1065227C (en) | 1997-12-15 | 1997-12-15 | Process for refining 2, 6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97122008A CN1065227C (en) | 1997-12-15 | 1997-12-15 | Process for refining 2, 6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1183400A CN1183400A (en) | 1998-06-03 |
| CN1065227C true CN1065227C (en) | 2001-05-02 |
Family
ID=5176611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97122008A Expired - Fee Related CN1065227C (en) | 1997-12-15 | 1997-12-15 | Process for refining 2, 6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1065227C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066903B (en) * | 2006-05-01 | 2011-06-08 | 株式会社晓星 | Method for separating and purifying 2,6-dimethylnaphthalene |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643155B (en) * | 2012-04-27 | 2014-05-28 | 太原理工大学 | Method for preparing refined naphthalene from industrial naphthalene utilizing microwave and ultrasonic wave |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057252A (en) * | 1991-07-12 | 1991-12-25 | 唐山市焦化厂 | A kind of production method of refined naphthalene |
| CN1078966A (en) * | 1992-05-19 | 1993-12-01 | 太原工业大学 | Technology for producing fine naphthalene by emulsifying crystalization |
-
1997
- 1997-12-15 CN CN97122008A patent/CN1065227C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057252A (en) * | 1991-07-12 | 1991-12-25 | 唐山市焦化厂 | A kind of production method of refined naphthalene |
| CN1078966A (en) * | 1992-05-19 | 1993-12-01 | 太原工业大学 | Technology for producing fine naphthalene by emulsifying crystalization |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066903B (en) * | 2006-05-01 | 2011-06-08 | 株式会社晓星 | Method for separating and purifying 2,6-dimethylnaphthalene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1183400A (en) | 1998-06-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2021004069A1 (en) | Method for recycling waste polyester material | |
| CN108558644B (en) | Production process and device of industrial oleic acid | |
| CN1944484A (en) | Method for removing aluminum trichloride and purifying products in C5 petroleum resin production process | |
| CN114031526A (en) | Continuous preparation method of fatty acyl amino acid type surfactant by one-step condensation method | |
| CN1065227C (en) | Process for refining 2, 6-dimethylnaphthalene by stepwise temp rising emulsifying crystallizing | |
| CN103848739A (en) | Production method of high-purity dimethyl fumarate | |
| CN1150065A (en) | Process for preparing fluorite collector agent | |
| CN1343531A (en) | Process for preparing floatation catcher of iron ore | |
| US5024772A (en) | Method of producing HPN and mixtures thereof | |
| CN1062292C (en) | Process for preparation of pure acenaphthene by gradually heating emulsification crystallization | |
| CN1035760C (en) | Technology for producing fine naphthalene by emulsifying crystalization | |
| CN1030386C (en) | Technology for processing formylic acid with methyl formate hydrolytic decomposition | |
| CN113480401A (en) | Synthesis method of chloro-n-pentane | |
| CN101838222B (en) | Preparation method of N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine | |
| CN1037342C (en) | Synthetic method for methyl cedrone | |
| CN1249135C (en) | Method for recovering perfluoro caprylic acid from waste liquid of producing teflon resin | |
| CN110357762B (en) | Preparation method for continuously producing alpha-phenethyl alcohol | |
| CN114874086B (en) | Treatment method of alkyl naphthalene acylation reaction liquid | |
| CN1033854C (en) | Synthetic process of triethyl orthoformate | |
| CN105669369B (en) | A kind of tert-butyl alcohol-propyl formate azeotropic mixture extraction rectifying method | |
| CN1097576C (en) | Production process of aromatic binary carboxylic acid | |
| CN112694639B (en) | Method and device for purifying polymerization liquid in EVOH production process | |
| CN113501744A (en) | Synthesis method of chloro-sec-butyl alkane | |
| CN111995550B (en) | Preparation method of sodium cocoyl isethionate | |
| CN116254156A (en) | Improved urea inclusion process for the enrichment of polyunsaturated fatty acids |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20010502 Termination date: 20151215 |
|
| EXPY | Termination of patent right or utility model |