CN101973964B - Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues - Google Patents
Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues Download PDFInfo
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- CN101973964B CN101973964B CN201010297232XA CN201010297232A CN101973964B CN 101973964 B CN101973964 B CN 101973964B CN 201010297232X A CN201010297232X A CN 201010297232XA CN 201010297232 A CN201010297232 A CN 201010297232A CN 101973964 B CN101973964 B CN 101973964B
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Abstract
The invention discloses a method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues. The method comprises the following steps of: firstly, steaming into the water and morpholine in a reflux ratio of 1:1 at 120 DEG C under normal pressure; then, steaming diethylene glycol in a reflux ratio of 1:1 to 1:10 at 165 DEG C under the vacuum of 4000 Pa; steaming a transition section in a reflex ratio of 1:5 to 1:10 at 165 DEG C under the vacuum of 130 Pa; and steaming a 2,2-dimorpholinyl diethyl ether product in a reflex ratio of 1:10 to 1:12 at 185 DEG C under 130 Pa and finally obtaining the 2,2-dimorpholinyl diethyl ether product according with the requirement of a polyurethane catalyst. The invention has the advantage of small investment scale, simple device and high separation efficiency and high product yield up to 85.5 percent.
Description
One, technical field
The present invention relates to a kind of organic separating and purifying method, be specifically related to from high-boiling-point morpholinium compound, separate and purify 2, the method for 2-dimorpholine base Anaesthetie Ether.
Two, background technology
2,2-dimorpholine base Anaesthetie Ether is a kind of catalyzer of synthesis of polyurethane, and external many patents have been described its compound method.Wherein representational have: U.S. Pat 6111100, a kind of compound method has been described, and promptly ammonia and glycol ether are under HTHP and in the presence of the hydrogenation catalyst, with hydrogen reaction preparation 2, the process of 2-dimorpholine base Anaesthetie Ether; Related plant investment is huge.European patent EP 0716084A1; Described a kind of compound method, in the presence of cobalt, copper metal catalyst and hydrogen, morpholine and glycol ether react under HTHP and generate 2; 2-dimorpholine base Anaesthetie Ether produces a large amount of single morpholinyl Anaesthetie Ether by products simultaneously.U.S. Pat 3817997A has described a kind of building-up process, in the presence of HTHP and hydrogenation catalyst, reacts the treated preparation 2 of product, the process of 2-dimorpholine base Anaesthetie Ether at ammonia and glycol ether.Reaction process uses metal oxide catalyst, and pressure is up to 7～20MPa.
The preparation process that above-mentioned document is involved all need be carried out under HTHP, and plant investment is big, and efficient is low.And in the process of suitability for industrialized production morpholine, produce a large amount of high boiling by products, and its by product is found to contain 2 through analyzing, 2-dimorpholine base Anaesthetie Ether, by weight, and 2, the content of 2-dimorpholine base Anaesthetie Ether reaches 15～46%.How from high-boiling-point morpholinium compound, to isolate and meet 2 of catalysts for polyurethanes requirement, 2-dimorpholine base Anaesthetie Ether, at present, also not seeing has bibliographical information.
Three, summary of the invention
Technical problem to be solved by this invention provides purifies 2 a kind of from high-boiling-point morpholinium compound, the separation, the method for 2-dimorpholine base Anaesthetie Ether, and according to method of the present invention, the finished product purity reaches 99%, and quality product meets the catalysts for polyurethanes requirement.
For solving the problems of the technologies described above; The present invention separates purification 2 from high-boiling-point morpholinium compound; The method of 2-dimorpholine base Anaesthetie Ether: earlier high-boiling-point morpholinium compound is put in the vaporizer that rectifying tower is housed, filling cy700 stainless steel ripple filler, theoretical plate number are no less than 60 in the said rectifying tower; Under the normal pressure, the evaporator temperature that slowly raises, control reflux ratio 1: 1, overhead collection water, morpholine reach 120 ℃ up to evaporator temperature, stop to heat up, and are cooled to 90 ℃; Under the 4000Pa vacuum, the evaporator temperature to 165 ℃ of slowly raising, control reflux ratio 1: 1～1: 10 is collected up to glycol ether and to be finished, and evaporator temperature is dropped to 140 ℃; Again under the 130Pa vacuum, the evaporator temperature to 165 ℃ of slowly raising, control reflux ratio 1: 5～1: 10; Steam single morpholinyl Anaesthetie Ether, the evaporator temperature to 185 ℃ of raising again, control reflux ratio 1: 10～1: 12; Collect transition section; And, detect 2,2-dimorpholine base Anaesthetie Ether content from the cat head sampling; In cat head sampling 2,2-dimorpholine base Anaesthetie Ether weight percent content reaches at 99% o'clock, begins to collect product, collects to finish to product and ends.
Because the present invention adopts the intermittent rectification under vacuum method, therefore, scale of investment is little, and device is simple, and separation efficiency is high, and product yield reaches 85.5%, and the finished product purity reaches 99%, and quality product meets the catalysts for polyurethanes requirement.
Four, embodiment
Make raw material with high-boiling-point morpholinium compound, through detecting, the result is following:
Production equipment is: 5001 still kettles (making still formula vaporizer), and tower diameter 300mm fills cy700 stainless steel ripple filler in the length 6m, tower; Cat head is the internal reflux condensing surface, band internal reflux and gear, receiving tank and vacuum pump.
Drop into above-mentioned material 250kg in the still kettle;
Under the normal pressure, the still temperature that slowly raises, overhead collection water, morpholine; Reach 120 ℃ up to the still temperature, stop to heat up, be cooled to 90 ℃;
Open water jet pump, vacuum pressure is at 4000Pa, the still temperature to 165 that slowly raises ℃, and the overhead collection glycol ether, at this moment, the beginning reflux ratio is 1: 1; Later stage is slowly heightened 1: 10 with reflux ratio; Finish up to the glycol ether collection; With still temperature drop to 140 ℃; Start two-stage Lodz pump, vacuum pressure rises still temperature to 165 ℃ when 130Pa, and reflux ratio 1: 5～1: 10 steams single morpholinyl Anaesthetie Ether; Elevated temperature to 185 ℃ again, reflux ratio 1: 10 is collected transition section, and from the cat head sampling, detects 2,2-dimorpholine base Anaesthetie Ether content;
When the cat head sampling reaches 99%, begin to collect product; Collect product 62kg altogether; Yield 85.5%.Through detection, product 2, the weight percent content of 2-dimorpholine base Anaesthetie Ether is 99.5%.
The device that arrives involved in the present invention comprises vaporizer, rectifying tower, condensing surface, return tank, vacuum receiving tank and vacuum pump.
Vaporizer involved in the present invention can be various ways such as falling-film evaporator, climbing-film evaporator, still formula vaporizer.
Rectifying tower involved in the present invention is filled efficient cy700 stainless steel ripple filler in it, theoretical stage reaches more than 60.
Vacuum pump involved in the present invention is multi-level combined pump.Forepump is water jet pump or water-ring pump, and final vacuum is 400Pa; Two stage pump and triplex are the Lodz pump, and final vacuum is 10pa.
Claims (1)
1. one kind is separated purification 2, the method for 2-dimorpholine base Anaesthetie Ether from high-boiling-point morpholinium compound: earlier high-boiling-point morpholinium compound is put in the vaporizer that rectifying tower is housed, filling cy700 stainless steel ripple filler, theoretical plate number are no less than 60 in the said rectifying tower; Under the normal pressure, the evaporator temperature that slowly raises, control reflux ratio 1: 1, overhead collection water, morpholine reach 120 ℃ up to evaporator temperature, stop to heat up, and are cooled to 90 ℃; Under the 4000Pa vacuum, the evaporator temperature to 165 ℃ of slowly raising, control reflux ratio 1: 1～1: 10 is collected up to glycol ether and to be finished, and evaporator temperature is dropped to 140 ℃; Again under the 130Pa vacuum, the evaporator temperature to 165 ℃ of slowly raising, control reflux ratio 1: 5～1: 10; Steam single morpholinyl Anaesthetie Ether, the evaporator temperature to 185 ℃ of raising again, control reflux ratio 1: 10～1: 12; Collect transition section; And, detect 2,2-dimorpholine base Anaesthetie Ether content from the cat head sampling; In cat head sampling 2,2-dimorpholine base Anaesthetie Ether weight percent content reaches at 99% o'clock, begins to collect product, collects to finish to product and ends.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010297232XA CN101973964B (en) | 2010-09-26 | 2010-09-26 | Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues |
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| CN201010297232XA CN101973964B (en) | 2010-09-26 | 2010-09-26 | Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues |
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| CN101973964A CN101973964A (en) | 2011-02-16 |
| CN101973964B true CN101973964B (en) | 2012-08-22 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4095022A (en) * | 1975-06-02 | 1978-06-13 | Texaco Development Corporation | Production of bis-(morpholino-n-alkyl) ethers |
| CN1304920A (en) * | 2001-02-13 | 2001-07-25 | 安徽阜阳化工总厂 | Process for removing diglycol from high-boiling-point morpholinium compound |
| CN1332142A (en) * | 2001-02-13 | 2002-01-23 | 安徽阜阳化工总厂 | Diglycol material for preparing morpholine |
-
2010
- 2010-09-26 CN CN201010297232XA patent/CN101973964B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4095022A (en) * | 1975-06-02 | 1978-06-13 | Texaco Development Corporation | Production of bis-(morpholino-n-alkyl) ethers |
| CN1304920A (en) * | 2001-02-13 | 2001-07-25 | 安徽阜阳化工总厂 | Process for removing diglycol from high-boiling-point morpholinium compound |
| CN1332142A (en) * | 2001-02-13 | 2002-01-23 | 安徽阜阳化工总厂 | Diglycol material for preparing morpholine |
Non-Patent Citations (3)
| Title |
|---|
| 徐铁军 等.吗啉副产物的开发利用.《广州化工》.2007,第37卷(第9期),161-162. * |
| 王之德.吗啉副产物和废液的综合利用及废水处理.《化工环保》.1991,第11卷339-343. * |
| 郑学明 等.双吗啉基二乙基醚（DMDEE）的合成.《现代化工》.2007,第27卷198-199. * |
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| CN101973964A (en) | 2011-02-16 |
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Addressee: Dong Jinlong Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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Address after: 246300 Qianshan County, Anqing City, the town of Peng Peng Ling Industrial Zone Patentee after: Anhui Hyea Aromas Co., Ltd. Address before: 246300 Peng Ling industrial area, Qianshan County, Anhui Patentee before: Anhui Hyea Chemical Co., Ltd. |