CN1332142A - Diglycol material for preparing morpholine - Google Patents
Diglycol material for preparing morpholine Download PDFInfo
- Publication number
- CN1332142A CN1332142A CN 01108204 CN01108204A CN1332142A CN 1332142 A CN1332142 A CN 1332142A CN 01108204 CN01108204 CN 01108204 CN 01108204 A CN01108204 A CN 01108204A CN 1332142 A CN1332142 A CN 1332142A
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- China
- Prior art keywords
- glycol ether
- diglycol
- morpholine
- purity
- fine fodder
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- 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.)
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Abstract
The diglycol material consists of diglycol with 98 % over high purity not less than 30 % and diglycol with 60-85 % purity recovered from high boiling point morpholine mixture not more than 70 %. The present invention makes it possible to utilize effectively recovered diglycol for saving resource and lowering production cost.
Description
The present invention relates to be used to prepare the diglycol material of morpholine.
Morpholine claims 1,4 morpholine again, molecular formula C
4H
9NO.Be colourless oil liquid, have water absorbability, strong basicity, the ammonia flavor is arranged that energy and organic solution are miscible, are insoluble to strong base solution, and is inflammable, is important organic synthesis reagent.Raw material mainly as rubber accelerator NOBS, OTOS etc.In industries such as medicine, weaving, paint, also have been widely used.
In the prior art, according to national standard, the preparation of morpholine must be a raw material at the glycol ether fine fodder more than 98% with purity, and glycol ether, liquefied ammonia and hydrogen enter reactor through heating after the vaporization.Under High Temperature High Pressure, carry out gas through catalyst---the solid catalysis aminating reaction, the gaseous mixture that leaves reactor enters gas-liquid separator after heat exchange condensation, cooling, gas stream recycles, liquid stream enters the separation and purification system, by three tower continuous still batterys, isolate the morpholine product, discharge high boiling material simultaneously.In this type of high boiling material, except containing reaction intermediate, single morpholinyl glycol ether, two morpholinyl glycol ether and other liquid, solid impurities such as not isolated on a small quantity morpholine, diglycolamine, still contain the glycol ether of not participating in reaction up to 40%-60%.Along with high boiling material as the waste material burning disposal.Not only bring environmental pollution, more cause the great wave on the resource useless.Cause the production cost of morpholine high.
The objective of the invention is to avoid above-mentioned weak point of the prior art, a kind of diglycol material that is used to prepare morpholine with rational proportion is provided.By effectively utilizing the recovery glycol ether of high-boiling-point morpholinium compound, economize on resources, reduce production costs.
Purpose of the present invention is achieved through the following technical solutions.
Characteristics of the present invention are to form with the recovery glycol ether proportioning of being extracted in high purity glycol ether fine fodder and the high-boiling-point morpholinium compound.
Characteristics of the present invention also are to get purity at the glycol ether fine fodder more than 98% and the purity recovery glycol ether at 60%-85%, and its proportioning is: the glycol ether fine fodder is no less than 30%, reclaims glycol ether and is not higher than 70%.
Compared with the prior art, advantage of the present invention is to reclaim glycol ether by reasonable utilization, is guaranteeing under the morpholine product quality premise, greatly reduce morpholine production cost, economize on resources, reduce trash discharge.The present invention does not change original production technique, by increase the high-boiling-point morpholinium compound retrieving arrangement is set, and the glycol ether that reclaims directly can be transmitted back to stock yard, makes it enter the recurrent state of sealing on production line.
Accompanying drawing is the glycol ether retrieving arrangement synoptic diagram of high-boiling-point morpholinium compound.
By the following examples, in conjunction with the accompanying drawings the present invention is further described.
Embodiment:
Present embodiment is to form with the recovery glycol ether proportioning of being extracted in high purity glycol ether fine fodder and the high-boiling-point morpholinium compound.In concrete the enforcement, get purity at the glycol ether fine fodder 98% or more and the purity recovery glycol ether at 60%-85%, its proportioning is: the glycol ether fine fodder is no less than 30%, and the recovery glycol ether is not higher than 70%.
In concrete the enforcement, be 70% recovery glycol ether at purity, can glycol ether accounts for 45% by reclaiming, the glycol ether fine fodder accounts for 55% proportioning and prepare burden.
Accompanying drawing shows the retrieving arrangement of glycol ether.As shown in the figure, with the high boiling material that generates in the morpholine preparation process is raw material, high boiling material basin 1 is set, by pan feeding pump 2 high boiling material is continuously pumped into rectifying tower 4, rectifying tower 4 is steam heating under vacuum state, its vacuum tightness is set to below the 0.1Mpa, heating steam is 1.5-4.0Mpa, keeps 150-250 ℃ of the glycol ether boiling temperature of rectifying tower tower top temperature under corresponding vacuum tightness, like this, tower still temperature can be lower than 300 ℃, thereby has guaranteed steam-heated feasibility.The overhead condensate that comes from condenser 6 is through return tank 3, again pumped into rectifying tower by reflux pump 5, form circulation, when glycol ether purity is brought up to 60%-85%, the single, double morpholinyl glycol ether of its contained harm morpholine reaction and solid impurity are extremely micro-, extraction rectifying thing is promptly finished the recovery of glycol ether.
In concrete the enforcement, the glycol ether shown in the figure can be recovered in the morpholine preparation and form closed cycle.Promptly directly pump into the rectification under vacuum tower shown in the figure from the high boiling material in the morpholine preparation, the glycol ether that rectifying is reclaimed is sent into morpholine and is prepared stock yard, and directly metering comes into operation.Through surveying, because the recycling of glycol ether, the glycol ether consumption of producing morpholine per ton is reduced to below 1.7 tons for white original 1.9 tons.
Claims (2)
1, a kind of diglycol material that is used to prepare morpholine is characterized in that forming with the recovery glycol ether proportioning of being extracted in high purity glycol ether fine fodder and the high-boiling-point morpholinium compound.
2, the diglycol material that is used to prepare morpholine according to claim 1, it is characterized in that getting purity at the glycol ether fine fodder more than 98% and purity recovery glycol ether at 60%-85, its proportioning is: the glycol ether fine fodder is no less than 30%, reclaims glycol ether and is not higher than 70%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011082046A CN1166610C (en) | 2001-02-13 | 2001-02-13 | Diglycol material for preparing morpholine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011082046A CN1166610C (en) | 2001-02-13 | 2001-02-13 | Diglycol material for preparing morpholine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1332142A true CN1332142A (en) | 2002-01-23 |
| CN1166610C CN1166610C (en) | 2004-09-15 |
Family
ID=4657087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011082046A Expired - Lifetime CN1166610C (en) | 2001-02-13 | 2001-02-13 | Diglycol material for preparing morpholine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1166610C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973964A (en) * | 2010-09-26 | 2011-02-16 | 安徽华业化工有限公司 | Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues |
| CN103214433A (en) * | 2013-04-11 | 2013-07-24 | 安徽昊源化工集团有限公司 | Raw liquid ammonia for producing morpholine |
| CN104262177A (en) * | 2014-09-02 | 2015-01-07 | 安徽昊源化工集团有限公司 | Separation and purification method of coarse diglycolamine |
-
2001
- 2001-02-13 CN CNB011082046A patent/CN1166610C/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973964A (en) * | 2010-09-26 | 2011-02-16 | 安徽华业化工有限公司 | Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues |
| CN101973964B (en) * | 2010-09-26 | 2012-08-22 | 安徽华业化工有限公司 | Method for separating and extracting 2,2-dimorpholinyl diethyl ether from high-boiling morpholine residues |
| CN103214433A (en) * | 2013-04-11 | 2013-07-24 | 安徽昊源化工集团有限公司 | Raw liquid ammonia for producing morpholine |
| CN104262177A (en) * | 2014-09-02 | 2015-01-07 | 安徽昊源化工集团有限公司 | Separation and purification method of coarse diglycolamine |
| CN104262177B (en) * | 2014-09-02 | 2015-10-28 | 安徽昊源化工集团有限公司 | A kind of separation purification method of thick diglycolamine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1166610C (en) | 2004-09-15 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: ANHUI HAO SOURCE CHEMICAL GROUP CO., LTD. Free format text: FORMER NAME OR ADDRESS: FUYANG CHEMICAL GENERAL PLANT, ANHUI |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 236028 Anhui province Fuyang Fukang Road No. 1 Patentee after: Anhui Haoyuan Chemical Industry (Group) Co., Ltd. Address before: 236028 Anhui province Fuyang Fukang Road No. 1 Patentee before: Fuyang Chemical General Plant, Anhui |
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| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20040915 |