CN1623978A - Process for producing tertiary butylamine ethoxy ethyl alcohol with space steric effect - Google Patents
Process for producing tertiary butylamine ethoxy ethyl alcohol with space steric effect Download PDFInfo
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- CN1623978A CN1623978A CN 200310111092 CN200310111092A CN1623978A CN 1623978 A CN1623978 A CN 1623978A CN 200310111092 CN200310111092 CN 200310111092 CN 200310111092 A CN200310111092 A CN 200310111092A CN 1623978 A CN1623978 A CN 1623978A
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- tertiary butyl
- butyl amine
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Abstract
A process for preparing the tert-butylamino ethoxyethanol as the selective desulfurizing solvent with sterical hindering effect includes such steps as putting tert-butylamine, 2-chloroethyoxy ethanol and reaction medium in reactor, heating while reaction, alkali neutralizing, condensing to recover excessive tert-butylamine, filtering, distilling, and rectifying. Its advantages are high selectivity and absorptivity to H2S, high boilding point and high purification.
Description
Technical field
The invention belongs to a kind of production method of selective desulfurization solvent, particularly a kind of bulky amine desulfurization solvent TERTIARY BUTYL AMINE base oxethyl alcoholic acid production method with space steric effect.
Background technology
Tradition is used for removing CO from sour gas
2And H
2The solvent N methyldiethanol amine (MDEA) of S, though for a long time at home, be used widely outward, and for handling CO
2Relatively low (the CO of content
2/ H
2S＜1.0) gas or use under the condition of sour gas load less (acid gas/amine≤0.2) is to H
2S has good selection removal effect, can save energy about 40% than common amine solvent.But for handling CO
2Higher (the CO of content
2/ H
2S＞1.0) gas or acidity load be the gas of big (acid gas/amine＞0.2), and its selectivity obviously degenerates.And in recent years, high CO
2The gas of content is on the increase as coal gas, associated gas, refinery tail-gas, Sweet natural gas etc.N methyldiethanol amine (MDEA) also more and more can not satisfy higher CO as the selective desulfurization solvent
2The demand that the gas sweetening that content and sour gas load are bigger is handled.In traditional selective desulfurization solvent N methyldiethanol amine, add 5～20% amine solvent TERTIARY BUTYL AMINE base ethanol (TBE) with space steric effect at this situation applicant, then with its mixing and stirring, make compound organic desulfurization solvent, though have can be with to H for this solvent
2The selectivity of S improves about 30%, and energy-conservation 25% with first-class characteristics; But because TERTIARY BUTYL AMINE base alcoholic acid boiling point only is 90 ℃ (25mmHg), high volatility under the inoic acid gas sweetening temperature condition, will cause solvent to volatilize in a large number, increase to purify cost, reduction economic benefit.Therefore, this technology exists again that boiling point is low, the loss through volatilization amount is big, defectives such as use cost height.
Summary of the invention
The objective of the invention is defective at the background technology existence, study a kind of TERTIARY BUTYL AMINE base oxethyl alcoholic acid production method with space steric effect, to reach on the basis that keeps background technology selective desulfurization effect, improve the selective desulfurization solvent boiling point, enlarge use range, reduce use cost, purpose such as increase economic efficiency.
Solution of the present invention is to adopt TERTIARY BUTYL AMINE and 2-chloroethoxy ethanol in reaction medium, heat from pressing reaction, reactant again through the alkali neutralizing treatment, slightly heat up in a steamer, rectifying, and make desulfurization solvent TERTIARY BUTYL AMINE base oxethyl ethanol, thereby realize its goal of the invention with space steric effect.Therefore, processing method of the present invention comprises:
A, heating, press reaction certainly: at first with raw material 2-chloroethoxy ethanol, TERTIARY BUTYL AMINE and reaction medium water or/and methyl alcohol, ethanol class low-carbon alcohol on request ratio drop in the reactor, heat up, under 60～200 ℃ of temperature from pressing reaction 0.5～3.0 hour; The mol ratio that is added between the raw material is a 2-chloroethoxy ethanol: TERTIARY BUTYL AMINE=1: 1.0～4.0, and add reaction medium amount be 20～200wt% of the total charging capacity of raw material by weight percentage;
B, neutralization reaction: after above-mentioned reactant is cooled to 40～70 ℃, add the NaOH or the KOH of 1～1.25 times of 2-chloroethoxy ethanol molar weight, reactant was carried out neutralizing treatment 0.5～1.5 hour; Be cooled to 20～30 ℃ of condensations then and reclaim excessive TERTIARY BUTYL AMINE;
C, slightly heat up in a steamer: material filtering that will be after B handles, remove solid impurity after, filtrate placed under 150～180 ℃ temperature and the 0.01～0.05MPa pressure slightly heats up in a steamer;
D, rectifying: above-mentioned raw distillate is promptly got object TERTIARY BUTYL AMINE base oxethyl ethanol through rectification process again; 180～200 ℃ of rectification temperatures, pressure 0.01～0.05MPa.
Above-mentioned raw materials TERTIARY BUTYL AMINE, 2-chloroethoxy ethanol and reaction medium methyl alcohol, ethanol, and the purity of NaOH, KOH (content) is technical grade purity.And described reaction medium, when it is water and methyl alcohol or/and during the alcoholic acid mixture, the ratio between each composition can be arbitrary proportion.
The product that the present invention produced its boiling point after testing is 117 ℃ (10mmHg), steric hindrance coefficient-Es=2.1, reactivity coefficient PKa=10.3.Being used for can be than background technology economizer investment 30% to the desulfurization of coal gas, Sweet natural gas, refinery tail-gas, liquid hydrocarbon etc., and the solvent cycle amount reduces 30～35%, and steam consumption reduces by 30～40%, but save operation expense 20～30%; H in the purified gas
2S content 10≤ppm.Thereby it is good to have desulfuration selectivity, the specific absorption height, and applied range, solvent boiling point is higher, and internal circulating load is few, and use cost is low, to characteristics such as gas cleaning benefit height.
Embodiment 1
A, be 2 liters of 97% ethanol with purity, content 95% 〉=TERTIARY BUTYL AMINE 657g, 2-chloroethoxy ethanol 450g drop in the reactor, be heated to 100～120 ℃, press reaction 2.0 hours certainly;
B, above-mentioned reactant is cooled to 60 ℃ after, add content and be 95% KOH 220g, neutralization reaction after 1.0 hours under refluxad, be cooled to≤30 ℃ reclaim excessive TERTIARY BUTYL AMINE;
C, above-mentioned solution filtrate filtered placed under 160 ℃ of temperature and the 0.03MPa vacuum slightly heat up in a steamer;
D, will place again under the empty vacuum condition of 190 ℃ of temperature and 0.03MPa after the rectifying by C gained raw distillate, TERTIARY BUTYL AMINE base oxethyl alcohol product 442g, this product is through stratographic analysis, content 95.8%.
Embodiment 2
The processing step of present embodiment is identical with embodiment 1.
At first 91g TERTIARY BUTYL AMINE, 2-chloroethoxy ethanol 62g and 200ml (milliliter) methanol mixed of technical purity are packed in 600 liters of reactors, certainly pressing reaction after 1.5 hours under 145 ℃ of temperature, be cooled to about 50 ℃, add 22g content again and be 98% NaOH and neutralizing treatment 1.0 hours under refluxad, be cooled to the excessive TERTIARY BUTYL AMINE of recovery about 25 ℃ then; Again after filtration, decompression is slightly heated up in a steamer, after the rectifying, TERTIARY BUTYL AMINE base oxethyl alcohol product 62g, product content 95.6%.
Embodiment 3
Present embodiment is made reaction medium with water, 46g TERTIARY BUTYL AMINE, 31g2-chloroethoxy ethanol (being technical pure) and 30ml water are mixed, place steel bomb, 160 ℃ of temperature of reaction, pressure are 0.6～0.7MPa, react after 50 minutes, be cooled to 65 ℃ together with reactor, added 11g content again and be 98% NaOH neutralizing treatment 45 minutes, and after cooling the temperature to room temperature (about 28 ℃) and reclaiming excessive TERTIARY BUTYL AMINE, reactant was filtered; Filtrate is slightly heated up in a steamer under 170 ℃ of temperature and 0.04MPa pressure; It is 98.1% product 33g that overhead product places rectifying under 190 ℃, 0.04MPa pressure condition to get content again.The present embodiment speed of response is fast, effective, and medium need not reclaim, and technical economic benefit is obvious.
Embodiment 4
Present embodiment is with methyl alcohol: ethanol: the mixed solution 48ml of water=1: 1: 1 is as reaction medium, place in the reactor together with 48g TERTIARY BUTYL AMINE, 32g2-chloroethoxy ethanol, under 162 ℃ of temperature, reacted 55 minutes from pressing, add NaOH (content 98%) 12g after being cooled to 65 ℃, neutralizing treatment 1 hour is cooled to 25 ℃ again and reclaims excessive TERTIARY BUTYL AMINE; Then solution is filtered, at last by the condition of embodiment 3 slightly heat up in a steamer, after the rectifying content is 98.2% product 31g.
Claims (3)
1, a kind of TERTIARY BUTYL AMINE base oxethyl alcoholic acid production method with space steric effect; It is characterized in that this method comprises:
A, heating, press reaction certainly: at first with raw material 2-chloroethoxy ethanol, TERTIARY BUTYL AMINE and reaction medium water or/and methyl alcohol, ethanol class low-carbon alcohol on request ratio drop in the reactor, heat up, under 60～200 ℃ of temperature from pressing reaction 0.5～3.0 hour; The mol ratio that is added between the raw material is a 2-chloroethoxy ethanol: TERTIARY BUTYL AMINE=1: 1.0～4.0, and add the amount of answering inverse medium and be 20～200wt% of the total charging capacity of raw material by weight percentage;
B, neutralization reaction: after above-mentioned reactant is cooled to 40～70 ℃, add the NaOH or the KOH of 1～1.25 times of 2-chloroethoxy ethanol molar weight, reactant was carried out neutralizing treatment 0.5～1.5 hour; Be cooled to 20～30 ℃ of condensations then and reclaim excessive TERTIARY BUTYL AMINE;
C, slightly heat up in a steamer: material filtering that will be after B handles, remove solid impurity after, filtrate placed under 150～180 ℃ temperature and the 0.01～0.05MPa pressure slightly heats up in a steamer;
D, rectifying: above-mentioned raw distillate is promptly got object TERTIARY BUTYL AMINE base oxethyl ethanol through rectification process again; 180～200 ℃ of rectification temperatures, pressure 0.01～0.05MPa.
2, by the described TERTIARY BUTYL AMINE base oxethyl of claim 1 alcoholic acid production method; It is characterized in that described raw material TERTIARY BUTYL AMINE, 2-chloroethoxy ethanol and reaction medium methyl alcohol, ethanol, and the purity of NaOH, KOH is technical grade purity.
3, by the described TERTIARY BUTYL AMINE base oxethyl of claim 1 alcoholic acid production method; It is characterized in that described reaction medium, when it is water and methyl alcohol or/and during the alcoholic acid mixture, the ratio between each composition can be arbitrary proportion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111092 CN1623978A (en) | 2003-12-05 | 2003-12-05 | Process for producing tertiary butylamine ethoxy ethyl alcohol with space steric effect |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111092 CN1623978A (en) | 2003-12-05 | 2003-12-05 | Process for producing tertiary butylamine ethoxy ethyl alcohol with space steric effect |
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| Publication Number | Publication Date |
|---|---|
| CN1623978A true CN1623978A (en) | 2005-06-08 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104353326A (en) * | 2014-10-21 | 2015-02-18 | 西南石油大学 | Steric hindrance amine desulfurizing agent and preparation method thereof |
| CN116751130A (en) * | 2023-05-09 | 2023-09-15 | 浙江恒逸石化研究院有限公司 | A kind of preparation method of sterically hindered amine |
| CN118405984A (en) * | 2024-04-23 | 2024-07-30 | 四川精事达科技有限公司 | A kind of tert-butylaminoethoxyethanol, its derivatives and catalytic synthesis method |
| CN119425356A (en) * | 2025-01-08 | 2025-02-14 | 淄博凯美可工贸有限公司 | Preparation method of corrosion-inhibiting energy-saving high-efficiency desulfurizer |
-
2003
- 2003-12-05 CN CN 200310111092 patent/CN1623978A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104353326A (en) * | 2014-10-21 | 2015-02-18 | 西南石油大学 | Steric hindrance amine desulfurizing agent and preparation method thereof |
| CN116751130A (en) * | 2023-05-09 | 2023-09-15 | 浙江恒逸石化研究院有限公司 | A kind of preparation method of sterically hindered amine |
| CN118405984A (en) * | 2024-04-23 | 2024-07-30 | 四川精事达科技有限公司 | A kind of tert-butylaminoethoxyethanol, its derivatives and catalytic synthesis method |
| CN118405984B (en) * | 2024-04-23 | 2025-02-07 | 四川精事达科技有限公司 | A kind of tert-butylaminoethoxyethanol, its derivatives and catalytic synthesis method |
| CN119425356A (en) * | 2025-01-08 | 2025-02-14 | 淄博凯美可工贸有限公司 | Preparation method of corrosion-inhibiting energy-saving high-efficiency desulfurizer |
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