CN103242175A - Preparation method of monoethanol diisopropanolamine - Google Patents
Preparation method of monoethanol diisopropanolamine Download PDFInfo
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- CN103242175A CN103242175A CN2013101193238A CN201310119323A CN103242175A CN 103242175 A CN103242175 A CN 103242175A CN 2013101193238 A CN2013101193238 A CN 2013101193238A CN 201310119323 A CN201310119323 A CN 201310119323A CN 103242175 A CN103242175 A CN 103242175A
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Abstract
The invention discloses a preparation method of monoethanol diisopropanolamine. The monoethanol diisopropanolamine is prepared by mixing and reacting diisopropanolamine and epoxyethane in a reaction kettle. The method does not adopt the traditional synthesis reaction of liquid ammonia with epoxyethane and epoxypropane, but creatively reacts the raw material diisopropanolamine with epoxyethane to obtain the product. The invention has the advantages of high yield, short reaction time, mild reaction conditions and controllable process; one active position on the ammonia molecule is substituted by epoxyethane, so that the molecular structure of the product can be controlled more easily; and by using the high-content diisopropanolamine as the raw material, the product has better smell, color and reaction time than that of an ammonia process.
Description
Technical field
The present invention relates to a kind of preparation method of an ethanol diisopropanolamine.
Background technology
At present, in Cement industry, lot of energy consumption is on the grinding of raw material and grog thereof; In the grinding process, cement particle surface free charge density increases, the free energy of solid surface increases, add the mutual collision between the particle, the probability that particle is reunited, adhered to increases, if cement granules further is broken, just need add the trend of this reunion of factors disrupt, adhesion, using grinding aid then is the most simple and convenient method.Add grinding aid less investment, instant effect, and can effectively improve the cement quality in kind.At present, more common organic substance grinding aid is alkanol amine and poly-hydroxy alcohols, for example trolamine, diethanolamine, multicondensed ethylene glycol, tri-isopropanolamine etc. both at home and abroad.Trolamine is the very strong hydramine of polarity, the aqueous solution is alkalescence, metal ion in can chelating cement and mineral substance interact, when usually using and polyvalent alcohol etc. composite, cement there is certain grinding-aid effect, and early strength that can very fast raising cement, but the cement later strength is undesirable, need use tri-isopropanolamine to the raising of later strength.Be a kind of in the cement grinding aid industry, rising gradually in the end of the year 2010 with an ethanol diisopropanolamine, it is reported, the cement grinding aid that has added an ethanol diisopropanolamine not only promotes to some extent to the early strength of cement, later strength also is significantly improved, be the characteristic that has had trolamine and tri-isopropanolamine concurrently, have very high economic worth.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of yield height, and the reaction times is short, reaction conditions gentleness, the preparation method of an ethanol diisopropanolamine that is easy to control.
For addressing the above problem, the present invention adopts following technical scheme: the preparation method of an a kind of ethanol diisopropanolamine of the present invention, and a described ethanol diisopropanolamine is by diisopropanolamine (DIPA) and oxyethane gained after the hybrid reaction in reactor; Its preparation process is as follows:
A) add raw material diisopropanolamine (DIPA) (about content 90%) in reactor, the reaction mass viscosity is appropriate, and the mol ratio of diisopropanolamine (DIPA) and water is 1.2: 1 in the described raw material, is beneficial to carrying out and the control of reaction process.
B) reactor is heated to proper temperature (60～70 ℃) and vacuumizing, add raw material oxyethane in proportion with after oxygen is found time in the reactor, adopt the outer circulation reactor to carry out circulating reaction down in temperature (60～70 ℃), the time of described circulating reaction is 2～5h, and the mol ratio of described propylene oxide and mixed solution is 0.9: 1～1.3: 1.
C) with after the gained mixed solution cooling cooling in the step b), the discharging can namely gets an ethanol diisopropanolamine finished product.
The preparation method's of the present invention's one ethanol diisopropanolamine beneficial effect is: the reaction that present method does not adopt traditional liquefied ammonia and oxyethane, propylene oxide to synthesize, but the employing diisopropanolamine (DIPA) of novelty is raw material, obtain product by the reaction with oxyethane, its advantage is: 1. yield height, and the reaction times is short; 2. reaction conditions gentleness, process are easier to control, and an activity site is replaced by propylene oxide on the amino molecule, the molecular structure of easier control product; 3. the diisopropanolamine (DIPA) of using high-content is as raw material, and the smell of product, color and luster, reaction times all are better than ammonia process.
Description of drawings
In order to be easy to explanation, the present invention is done to describe in detail by following specific embodiment and accompanying drawing.
Fig. 1 is the preparation method's of the present invention's one ethanol diisopropanolamine process flow sheet;
Fig. 2 is the present invention one ethanol diisopropanolamine structural formula figure.
Embodiment
Embodiment 1
Consult illustrated in figures 1 and 2, the preparation method of an a kind of ethanol diisopropanolamine of the present invention, a described ethanol diisopropanolamine is by diisopropanolamine (DIPA) (about content 90%) and oxyethane gained after the hybrid reaction in reactor; Its preparation process is as follows:
A) in reactor, add raw material diisopropanolamine (DIPA) 328.0g.
B) reactor is heated to 70 ℃ of temperature, then with reaction kettle for vacuumizing, adds raw material oxyethane 88.0g in proportion, adopt the outer circulation reactor to carry out circulating reaction down 70 ℃ of temperature, circulating reaction 5 hours gets an ethanol diisopropanolamine, and an ethanol diisopropanolamine yield is 89.7%.
C) with after the one ethanol diisopropanolamine mixed solution of gained in the step b) cooling cooling, the discharging can gets final product.
Embodiment 2
Consult illustrated in figures 1 and 2, the preparation method of an a kind of ethanol diisopropanolamine of the present invention, a described ethanol diisopropanolamine is by diisopropanolamine (DIPA) (about content 90%) and oxyethane gained after the hybrid reaction in reactor; Its preparation process is as follows:
A) in reactor, add raw material diisopropanolamine (DIPA) 295.6g.
B) reactor is heated to 60 ℃ of temperature, then with reaction kettle for vacuumizing, adds raw material oxyethane 92.4g in proportion, adopt the outer circulation reactor to carry out circulating reaction down 60 ℃ of temperature, circulating reaction 3 hours gets an ethanol diisopropanolamine, and an ethanol diisopropanolamine yield is 96.6%.
C) with after the one ethanol diisopropanolamine mixed solution of gained in the step b) cooling cooling, the discharging can gets final product.
Embodiment 3
Consult illustrated in figures 1 and 2, the preparation method of an a kind of ethanol diisopropanolamine of the present invention, a described ethanol diisopropanolamine is by diisopropanolamine (DIPA) (about content 90%) and oxyethane gained after the hybrid reaction in reactor; Its preparation process is as follows:
A) in reactor, add raw material diisopropanolamine (DIPA) 295.6g.
B) reactor is heated to 65 ℃ of temperature, then with reaction kettle for vacuumizing, adds raw material oxyethane 114.3g in proportion, adopt the outer circulation reactor to carry out circulating reaction down 65 ℃ of temperature, circulating reaction 2 hours gets an ethanol diisopropanolamine, and an ethanol diisopropanolamine yield is 95.8%.
C) with after the one ethanol diisopropanolamine mixed solution of gained in the step b) cooling cooling, the discharging can gets final product.
The preparation method's of the present invention's one ethanol diisopropanolamine beneficial effect is: the reaction that present method does not adopt traditional liquefied ammonia and oxyethane, propylene oxide to synthesize, but the employing diisopropanolamine (DIPA) of novelty is raw material, obtain product by the reaction with oxyethane, its advantage is: 1. yield height, and the reaction times is short; 2. reaction conditions gentleness, process are easier to control, and an activity site is replaced by propylene oxide on the amino molecule, the molecular structure of easier control product; 3. the diisopropanolamine (DIPA) of using high-content is as raw material, and the smell of product, color and luster, reaction times all are better than ammonia process.
The above only is the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any variation or replacement of expecting without creative work all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (1)
1. the preparation method of an ethanol diisopropanolamine is characterized in that: a described ethanol diisopropanolamine is by diisopropanolamine (DIPA) and oxyethane gained after the hybrid reaction in reactor; Its preparation process is as follows:
A) add raw material diisopropanolamine (DIPA) (about content 90%) in reactor, the reaction mass viscosity is appropriate, and the mol ratio of diisopropanolamine (DIPA) and water is 1.2: 1 in the described raw material, is beneficial to carrying out and the control of reaction process.
B) reactor is heated to proper temperature (60～70 ℃) and vacuumizing, add raw material oxyethane in proportion with after oxygen is found time in the reactor, adopt the outer circulation reactor to carry out circulating reaction down in temperature (60～70 ℃), the time of described circulating reaction is 2～5h, and the mol ratio of described oxyethane and mixed solution is 0.9: 1～1.3: 1.
C) with after the gained mixed solution cooling cooling in the step b), the discharging can namely gets an ethanol diisopropanolamine finished product.
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| CN2013101193238A CN103242175A (en) | 2013-03-28 | 2013-03-28 | Preparation method of monoethanol diisopropanolamine |
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| CN2013101193238A CN103242175A (en) | 2013-03-28 | 2013-03-28 | Preparation method of monoethanol diisopropanolamine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435499A (en) * | 2013-08-19 | 2013-12-11 | 济南大学 | Novel preparation method for mono ethanol diisopropanolamine |
| CN105236796A (en) * | 2015-10-26 | 2016-01-13 | 南京永能新材料有限公司 | Limestone-cement liquid grinding aid and preparation method thereof |
| CN108147699A (en) * | 2017-12-28 | 2018-06-12 | 湖北鑫统领万象科技有限公司 | A kind of cement grinding aid and its application |
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| JPS61100550A (en) * | 1984-10-23 | 1986-05-19 | Daicel Chem Ind Ltd | Preparation of dialkylaminoethanol |
| US4847418A (en) * | 1983-12-13 | 1989-07-11 | Union Carbide Corporation | Continuous process for preparing alkanolamines |
| JP2006171357A (en) * | 2004-12-15 | 2006-06-29 | Asahi Glass Co Ltd | Photoresist stripping solution |
| CN101735077A (en) * | 2009-12-11 | 2010-06-16 | 广西壮族自治区化工研究院 | Production method and production equipment for synthesizing ethanolamine by ethylene oxide |
| CN101786957A (en) * | 2010-03-24 | 2010-07-28 | 山东东大一诺威新材料有限公司 | Isopropanolamine producing method |
| CN102924301A (en) * | 2012-11-01 | 2013-02-13 | 史才军 | Preparation method of N,N-bis(2-hydroxyethyl)isopropanolamine |
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2013
- 2013-03-28 CN CN2013101193238A patent/CN103242175A/en active Pending
Patent Citations (6)
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| US4847418A (en) * | 1983-12-13 | 1989-07-11 | Union Carbide Corporation | Continuous process for preparing alkanolamines |
| JPS61100550A (en) * | 1984-10-23 | 1986-05-19 | Daicel Chem Ind Ltd | Preparation of dialkylaminoethanol |
| JP2006171357A (en) * | 2004-12-15 | 2006-06-29 | Asahi Glass Co Ltd | Photoresist stripping solution |
| CN101735077A (en) * | 2009-12-11 | 2010-06-16 | 广西壮族自治区化工研究院 | Production method and production equipment for synthesizing ethanolamine by ethylene oxide |
| CN101786957A (en) * | 2010-03-24 | 2010-07-28 | 山东东大一诺威新材料有限公司 | Isopropanolamine producing method |
| CN102924301A (en) * | 2012-11-01 | 2013-02-13 | 史才军 | Preparation method of N,N-bis(2-hydroxyethyl)isopropanolamine |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435499A (en) * | 2013-08-19 | 2013-12-11 | 济南大学 | Novel preparation method for mono ethanol diisopropanolamine |
| CN103435499B (en) * | 2013-08-19 | 2015-07-08 | 济南大学 | Novel preparation method for mono ethanol diisopropanolamine |
| CN105236796A (en) * | 2015-10-26 | 2016-01-13 | 南京永能新材料有限公司 | Limestone-cement liquid grinding aid and preparation method thereof |
| CN108147699A (en) * | 2017-12-28 | 2018-06-12 | 湖北鑫统领万象科技有限公司 | A kind of cement grinding aid and its application |
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Application publication date: 20130814 |