CN101633620A - Normal-temperature continuous production technology for cetane number improver - Google Patents
Normal-temperature continuous production technology for cetane number improver Download PDFInfo
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- CN101633620A CN101633620A CN200810138578A CN200810138578A CN101633620A CN 101633620 A CN101633620 A CN 101633620A CN 200810138578 A CN200810138578 A CN 200810138578A CN 200810138578 A CN200810138578 A CN 200810138578A CN 101633620 A CN101633620 A CN 101633620A
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Abstract
The invention discloses normal-temperature continuous production technology for a cetane number improver, which belongs to the technical field of the preparation of organic nitrate ester compounds, and comprises the steps of using nitramine or nitric acid and isooctanol to react under the action of a catalyst. The normal-temperature continuous production technology for the cetane number improver is characterized by changing concentrated sulfuric acid as the catalyst, using different proportions of the concentrated sulfuric acid, concentrated nitric acid and water to control different reaction temperatures and realize continuous production, returning waste acid to an acid distribution post for acid mixing according to the content of the acid, then circularly utilizing the waste acid, finally selecting a normal reaction temperature of between 8 DEG C below zero and 40 DEG C in order to the safety and the control of the purity and the yield of energy consumption and the like, and utilizing the proportion of acid mixing to control reaction rate to achieve optimum process conditions such as continuous recycling of the waste acid, continuous feeding nitrification and the like. The technology overcomes the disadvantages of unsteady quality of products, large potential safety hazard, high energy consumption and material consumption and the like, improves the yield, ensures that the quality of the products entirely and steadily reaches that of high-class products, and greatly improves the utilization efficiency of equipment.
Description
Technical field
The invention belongs to the technical field of the organic nitric acid lipoid substance of preparation, be specifically related to a kind of organic nitric acid lipid normal-temperature continuous production technology for cetane number improver.
Background technology
Method with solvent extraction and hydrogenation can improve diesel-fuel cetane number, but costly, and is uneconomical economically, and it is low to produce the cetane number improver cost, technology is simple, and can improve cetane value effectively, so cetane number improver just more and more is subject to people's attention.Isooctyl ester nitrate is received diesel cetane-number improver, especially mixes use, can improve cetane value widely with 2-methyl-2-nitro propyl group nitric ether.
The method of producing isooctyl ester nitrate generally all adopts mixed acid process, promptly at normal temperature or be lower than under the condition of normal temperature isooctyl alcohol is added in the nitration mixture of being made up of nitric acid and sulfuric acid, under the refrigerating brine cooling conditions, make reactive system keep the layering in the frozen water of reinjecting of low temperature, reactant, the ester layer is washed.Generation for anti-oxidation side reaction, must carry out at low temperatures, to stably continue to keep cold operation that refrigerant must be arranged, and this plant investment is bigger, and it is also bigger to consume energy, simultaneously, in the sepn process of ester and water, adopt component distillation, this method is used for synthetic lower boiling nitric ether higher yields, and (101～103 ℃/1333Pa) productivity ratio is lower, only has about 50% for the high boiling point isooctyl ester nitrate.
" synthesizing of diesel cetane-number improver (I)-isooctyl ester nitrate " (Hu Yingxi, Lv Jiuzhuo, Liu Xia, Chen Chiyang " petrochemical complex Journal of Chinese Universities " the 4th phase in 1997) discloses a kind of hexadecyl improving agent lab scale synthetic method, and the disclosed content of the document is quoted at this as prior art.
The industrial manufacture process of prior art cetane number improver (isooctyl ester nitrate) has two kinds, a kind of is high temperature gap method, temperature of reaction is controlled at 60～80 ℃, reacts under the effect of catalyzer with ammonium nitrate or nitric acid and isooctyl alcohol, and spent acid can not recycle, raw material consumption is big, yield is low, and unstable product quality, and temperature is crossed to hang down and do not reacted, temperature is high slightly emits still easily, even blasts.Another kind is a low temperature process, and temperature of reaction is reacted under the effect of catalyzer with concentrated nitric acid and isooctyl alcohol at-10～0 ℃, and production process must strict control low temperature, needs freezingly, and power consumption is high, and spent acid can not recycle, and raw material consumption is big, and the production safety coefficient is little.
Summary of the invention
The present invention is directed to the deficiency that exists in the hexadecyl improving agent, a kind of normal-temperature continuous production technology for cetane number improver is provided, this technology has the yield height, constant product quality, and the advantage that the utilising efficiency of equipment is high has solved the problems of the prior art.
A kind of normal-temperature continuous production technology for cetane number improver, adopt nitric acid and isooctyl alcohol under the effect of catalyzer, to react, it is characterized in that, comprise the steps: that nitration mixture adding speed is 160 ~ 250 liters/hour, isooctyl alcohol adding speed is 50 ~ 100 liters/hour, in nitrating pot, feed intake continuously, the reaction product overflow is to quantizer, carrying out organic phase separates with spent acid, organic phase goes washing refining, nitration mixture still preparation nitration mixture is got back in acid mutually, carries out nitration reaction after the nitration mixture analysis is qualified and feeds intake, and realizes continuous cyclic production;
Described nitration mixture is the mixture of the vitriol oil and concentrated nitric acid, and wherein the content of concentrated nitric acid is 5～20%, and catalyzer is the vitriol oil; Temperature of reaction is-8～40 ℃.
Compared with prior art, beneficial effect of the present invention is: 1) power consumption reduces, and spent acid can recycle; 2) raw material consumption is few; 3) yield height, constant product quality; 4) the utilising efficiency height of equipment.
Embodiment
Embodiment
On the production technique basis of former high temperature gap method, improve, use the vitriol oil instead and make catalyzer, with the different vitriol oils, concentrated nitric acid, the proportioning of water, control different temperature of reaction, the realization serialization is produced, after spent acid comes back to the complex acid post and carries out nitration mixture according to the content of acid, and recycle, nitration mixture is controlled at dense nitre content 5～20%, the vitriol oil is controlled at 60～80%, last purity for safety and energy consumption, normal-temperature reaction temperature-8～40 ℃ is selected in the control of yield etc., utilize the nitration mixture proportioning, controls reaction speed reaches the continuous reuse of spent acid, the nitrated optimum process condition that waits of continuous dosing, changed unstable product quality, potential safety hazard is big, shortcomings such as energy consumption material consumption height, realized that yield brings up to 99.5% from 85%, quality product is all stable to reach premium grads, and has improved the utilising efficiency of equipment greatly.
Claims (1)
1. normal-temperature continuous production technology for cetane number improver, adopt nitric acid and isooctyl alcohol under the effect of catalyzer, to react, it is characterized in that, comprise the steps: that nitration mixture adding speed is 160 ~ 250 liters/hour, isooctyl alcohol adding speed is 50 ~ 100 liters/hour, in nitrating pot, feed intake continuously, the reaction product overflow is to quantizer, carrying out organic phase separates with spent acid, organic phase goes washing refining, nitration mixture still preparation nitration mixture is got back in acid mutually, carries out nitration reaction after the nitration mixture analysis is qualified and feeds intake, and realizes continuous cyclic production;
Described nitration mixture is the mixture of the vitriol oil and concentrated nitric acid, and wherein the content of concentrated nitric acid is 5～20%, and catalyzer is the vitriol oil; Temperature of reaction is-8～40 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810138578A CN101633620A (en) | 2008-07-25 | 2008-07-25 | Normal-temperature continuous production technology for cetane number improver |
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| CN200810138578A CN101633620A (en) | 2008-07-25 | 2008-07-25 | Normal-temperature continuous production technology for cetane number improver |
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| CN101633620A true CN101633620A (en) | 2010-01-27 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911194A (en) * | 2013-01-04 | 2014-07-09 | 高剑峰 | Composite type diesel fuel cetane number improver and production process thereof |
| CN103980125A (en) * | 2014-05-13 | 2014-08-13 | 常州大学 | Synthetic method of isooctyl nitrate |
| CN106220508A (en) * | 2016-07-06 | 2016-12-14 | 北京兴有化工有限责任公司 | Reduce the acidity of cetane number improver and remove organic and inorganic impurity method |
| CN107935857A (en) * | 2017-12-11 | 2018-04-20 | 中国科学院大连化学物理研究所 | A kind of production method of isooctyl ester nitrate |
| CN108203383A (en) * | 2016-12-19 | 2018-06-26 | 付海明 | cetane number improver and preparation method thereof |
| JP2022538771A (en) * | 2019-07-02 | 2022-09-06 | アシムケム ラボラトリーズ （ティエンジン） カンパニー リミテッド | Continuous synthesis method and apparatus for cyclopropane-based compound |
-
2008
- 2008-07-25 CN CN200810138578A patent/CN101633620A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911194A (en) * | 2013-01-04 | 2014-07-09 | 高剑峰 | Composite type diesel fuel cetane number improver and production process thereof |
| CN103911194B (en) * | 2013-01-04 | 2016-04-20 | 高剑峰 | composite diesel cetane number improver and production technique thereof |
| CN103980125A (en) * | 2014-05-13 | 2014-08-13 | 常州大学 | Synthetic method of isooctyl nitrate |
| CN106220508A (en) * | 2016-07-06 | 2016-12-14 | 北京兴有化工有限责任公司 | Reduce the acidity of cetane number improver and remove organic and inorganic impurity method |
| CN106220508B (en) * | 2016-07-06 | 2018-07-31 | 北京兴有化工有限责任公司 | It reduces the acidity of cetane number improver and removes organic and inorganic impurity method |
| CN108203383A (en) * | 2016-12-19 | 2018-06-26 | 付海明 | cetane number improver and preparation method thereof |
| CN108203383B (en) * | 2016-12-19 | 2020-10-16 | 付海明 | Cetane number improver and preparation method thereof |
| CN107935857A (en) * | 2017-12-11 | 2018-04-20 | 中国科学院大连化学物理研究所 | A kind of production method of isooctyl ester nitrate |
| JP2022538771A (en) * | 2019-07-02 | 2022-09-06 | アシムケム ラボラトリーズ （ティエンジン） カンパニー リミテッド | Continuous synthesis method and apparatus for cyclopropane-based compound |
| US11993552B2 (en) | 2019-07-02 | 2024-05-28 | Asymchem Laboratories (Tianjin) Co., Ltd. | Method and device for continuously synthesizing cyclopropane compounds |
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Application publication date: 20100127 |