CN102775280A - New method for preparing tripropylene glycol - Google Patents
New method for preparing tripropylene glycol Download PDFInfo
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- CN102775280A CN102775280A CN2012102819475A CN201210281947A CN102775280A CN 102775280 A CN102775280 A CN 102775280A CN 2012102819475 A CN2012102819475 A CN 2012102819475A CN 201210281947 A CN201210281947 A CN 201210281947A CN 102775280 A CN102775280 A CN 102775280A
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- tripropylene glycol
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- dpg
- tubular reactor
- catalyzer
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Abstract
The invention discloses a new method for preparing tripropylene glycol and aims at providing a new tripropylene glycol preparation method which is simple in process, low in cost, high in product yield and purity and low in chroma. The new method is characterized by enabling dipropylene glycol, epoxy propane and a catalyst which have the mole ratio of 1:(0.1-1.45):(0.003-0.1) to undergo a reaction in a static tubular reactor under the condition of strong basicity, and obtaining a high-purity tripropylene glycol product by acid neutralization and decompressing rectification.
Description
Technical field
The present invention relates to a kind of novel method for preparing tripropylene glycol, belong to the fine chemistry industry production field.
Background technology
Tripropylene glycol (TPG); Molecular formula is
, and molecular weight is 192.25.Can be used as medical material; Make the midbody of dyestuff, fibre finish, anticorrosive additive etc.; Can make water-soluble paint base material, synthetic resins solvent; Also can make the tackiness agent of polyurethane elastomer, coating, be the main raw material of uv-curable monomer tri (propylene glycol) diacrylate (TPGD).
At present, the preparation method of tripropylene glycol is many, and 2-Ucar 35 and propylene oxide are raw material with 1, and the product that makes is the mixture of DPG and tripropylene glycol, and the content of tripropylene glycol is lower in the product that makes, color and luster is dark.The preparation tripropylene glycol all is with 1 among Chinese patent CN1803743, CN101250093 and the CN101941893A; The 2-Ucar 35 is a raw material; The catalyzer of just selecting is different; Adopt these methods to prepare tripropylene glycol, the yield of the product tripropylene glycol of producing is low, and then the manufacturing cost of product is increased.
Summary of the invention
The novel method that the purpose of this invention is to provide the preparation tripropylene glycol that a kind of technology is simple, cost is low, product yield is high, purity is high, colourity is low.
A kind of novel method for preparing tripropylene glycol of the present invention; Adopt following technical proposals: with DPG: propylene oxide: the mol ratio of catalyzer is that 1:0.1～1.45:0.0003～0.1 is in static tubular reactor, after the reaction, promptly getting the high purity tripropylene glycol through acid neutralization, rectification under vacuum under the strong alkaline condition.
Product.
In the technique scheme, static tubular reactor is established the static tubular reactor of many rotary fluids of single tube mixing head in being.
Adopt technique scheme; Owing to through establishing the static tubular reactor of many rotary fluids of single tube mixing head in adopting, make material diversion become team, produce the reverse rotation of intersection vortex simultaneously; With the reaction mass short mix; Shorten the reaction times greatly, reduce by three generations of by products such as four Ucar 35 of contracting, and can realize continuous production.
In the technique scheme, synthesis reaction temperature is controlled at 90～200 ℃.
In the technique scheme, catalyzer is any one in sodium methylate, the sodium ethylate.
In the technique scheme, DPG: propylene oxide: the preferred molar ratio of catalyzer is 1:0.4～0.7:0.002～0.003.
In sum; The invention has the beneficial effects as follows: with DPG, propylene oxide is that raw material reacts in static tubular reactor; The product of reaction is carried out rectification under vacuum promptly get the high purity tripropylene glycol after acid neutralization, adopt that this kind preparation method technology is simple, energy consumption is low; Because through establishing the static tubular reactor of many rotary fluids of single tube mixing head in adopting; Make material diversion become team, produce the reverse rotation of intersection vortex simultaneously, the reaction mass short mix; Shorten the reaction times greatly; Reduce by three generations of by products such as four Ucar 35 of contracting, and can realize continuous production, the product yield that makes is high, purity is high, colourity is low.
Embodiment
Below in conjunction with embodiment the present invention is further specified:
Embodiment one:
The raw material DPG is squeezed in the static tubular reactor to visual liquid level through pump; When it is warming up to 140 ℃; System begins continuously feeding; Wherein the material feeding amount is respectively: DPG (DPG) inlet amount is 5.36L/h, and propylene oxide (PO) inlet amount is 1.32L/h, and catalyzer sodium ethylate inlet amount is 2.47mL/h.Control reaction temperature does not have special qualification at 120～140 ℃ to reaction pressure, and discharging is controlled at about 6.8L/h.Detection level: DPG 43.2%, tripropylene glycol 54.1%, three four Ucar 35 2.0% that contract.
Embodiment two:
The raw material DPG is squeezed in the static tubular reactor to visual liquid level through pump; When it is warming up to 125 ℃; System begins continuously feeding; Wherein the material feeding amount is respectively: DPG (DPG) inlet amount is 0.48m3/h, and propylene oxide (PO) inlet amount is 0.17m3/h, and catalyzer sodium methylate inlet amount is 2.00L/h.Control reaction temperature does not have special qualification at 110～130 ℃ to reaction pressure, and discharging is controlled at about 0.6 m3/h.Detection level: DPG 36.6%, tripropylene glycol 61.3%, three four Ucar 35 1.7% that contract.
Embodiment three:
The raw material DPG is squeezed in the static tubular reactor to visual liquid level through pump; When it is warming up to 150 ℃; System begins continuously feeding; Wherein the material feeding amount is respectively: DPG (DPG) inlet amount is 0.83m3/h, and propylene oxide (PO) inlet amount is 0.28m3/h, and catalyzer sodium methylate inlet amount is 3.44L/h.Control reaction temperature does not have special qualification at 150～160 ℃ to reaction pressure, and discharging is controlled at about 1.1 m3/h.Detection level: DPG 37.1%, tripropylene glycol 60.4%, three four Ucar 35 2.4% that contract.
Claims (5)
1. novel method for preparing tripropylene glycol; It is characterized in that: with DPG: propylene oxide: the mol ratio of catalyzer is that 1:0.1～1.45:0.0003～0.1 is in static tubular reactor, after the reaction, promptly getting the high purity tripropylene glycol through acid neutralization, rectification under vacuum under the strong alkaline condition.
2. a kind of novel method for preparing tripropylene glycol according to claim 1 is characterized in that: said static tubular reactor is established the static tubular reactor of many rotary fluids of single tube mixing head in being.
3. a kind of novel method for preparing tripropylene glycol according to claim 1 is characterized in that: synthesis reaction temperature is controlled at 90～250 ℃.
4. a kind of novel method for preparing tripropylene glycol according to claim 1 is characterized in that: said catalyzer is any one in sodium methylate, the sodium ethylate.
5. according to claim 1 or 3 described a kind of novel methods that prepare tripropylene glycol, it is characterized in that: DPG: propylene oxide: the mol ratio of catalyzer is 1:0.4～0.6:0.002～0.003.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102819475A CN102775280A (en) | 2012-08-09 | 2012-08-09 | New method for preparing tripropylene glycol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102819475A CN102775280A (en) | 2012-08-09 | 2012-08-09 | New method for preparing tripropylene glycol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102775280A true CN102775280A (en) | 2012-11-14 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102819475A Pending CN102775280A (en) | 2012-08-09 | 2012-08-09 | New method for preparing tripropylene glycol |
Country Status (1)
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| CN (1) | CN102775280A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170046A (en) * | 2015-07-23 | 2015-12-23 | 百川化工(如皋)有限公司 | DMP neutralizing treatment method |
| CN106831358A (en) * | 2017-01-18 | 2017-06-13 | 东营市海科新源化工有限责任公司 | A kind of preparation method of dipropylene glycol |
| CN110655454A (en) * | 2018-06-29 | 2020-01-07 | 东营市海科新源化工有限责任公司 | Method and system for preparing dipropylene glycol with high selectivity |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1133588A (en) * | 1993-10-22 | 1996-10-16 | 陶氏化学公司 | Alkylene glycols having a higher primary hydroxyl content |
| CN1803743A (en) * | 2006-01-16 | 2006-07-19 | 宜兴市宏博乳化剂有限公司 | Tripropylene glycol synthesis method |
| CN101250093A (en) * | 2008-03-22 | 2008-08-27 | 江苏三木集团 | Preparation method of tripropylene glycol |
| CN101941893A (en) * | 2010-08-24 | 2011-01-12 | 浙江皇马科技股份有限公司 | Method for synthesizing tripropylene glycol |
-
2012
- 2012-08-09 CN CN2012102819475A patent/CN102775280A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1133588A (en) * | 1993-10-22 | 1996-10-16 | 陶氏化学公司 | Alkylene glycols having a higher primary hydroxyl content |
| CN1803743A (en) * | 2006-01-16 | 2006-07-19 | 宜兴市宏博乳化剂有限公司 | Tripropylene glycol synthesis method |
| CN101250093A (en) * | 2008-03-22 | 2008-08-27 | 江苏三木集团 | Preparation method of tripropylene glycol |
| CN101941893A (en) * | 2010-08-24 | 2011-01-12 | 浙江皇马科技股份有限公司 | Method for synthesizing tripropylene glycol |
Non-Patent Citations (1)
| Title |
|---|
| 方诒胜: "醇钠法合成一缩二丙二醇的工艺过程控制", 《安徽化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170046A (en) * | 2015-07-23 | 2015-12-23 | 百川化工(如皋)有限公司 | DMP neutralizing treatment method |
| CN106831358A (en) * | 2017-01-18 | 2017-06-13 | 东营市海科新源化工有限责任公司 | A kind of preparation method of dipropylene glycol |
| CN106831358B (en) * | 2017-01-18 | 2020-03-03 | 东营市海科新源化工有限责任公司 | Preparation method of dipropylene glycol |
| CN110655454A (en) * | 2018-06-29 | 2020-01-07 | 东营市海科新源化工有限责任公司 | Method and system for preparing dipropylene glycol with high selectivity |
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Application publication date: 20121114 |