CN1017146B - Synthesizing process of isooctyl ester nitrate - Google Patents
Synthesizing process of isooctyl ester nitrateInfo
- Publication number
- CN1017146B CN1017146B CN 87105712 CN87105712A CN1017146B CN 1017146 B CN1017146 B CN 1017146B CN 87105712 CN87105712 CN 87105712 CN 87105712 A CN87105712 A CN 87105712A CN 1017146 B CN1017146 B CN 1017146B
- Authority
- CN
- China
- Prior art keywords
- reaction
- reactor
- nitric
- isooctyl ester
- ester nitrate
- Prior art date
- 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.)
- Expired
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Abstract
The present invention relates to a technology for synthesizing isooctyl ester nitrate, which adopts the mixture ratio of nitro-sulfur mixed acid. Thus, nitration reaction is carried out at normal temperature, the product has the advantages of high yield, high purity and low cost. The synthesizing technology is suitable for a kettle-type reactor, an overflow-type reactor and an injection-type reactor, and has the advantages of simple technology, easy industrialization and convenient popularization. When added in diesel oil, the product has obvious effect of increasing the cetane number of the diesel oil.
Description
Isooctyl ester nitrate synthesis technique of the present invention belongs to the nitric ether synthesis technique, and isooctyl ester nitrate is a kind of good cetane number improver.
Nitric ether generally adopts the nitrated classical way of alcohol, i.e. mixed acid process under temperature-10 ℃～10 ℃ condition, slowly joins alcohol in the well-beaten nitration mixture, and after reaction finished, reactant injected the frozen water layering.To wash in the ester layer.For anti-oxidation branched chain reaction, select under the low temperature (10 ℃) synthetic, but in industrial realization cold operation difficulty, temperature is crossed low or the nitration mixture proportioning is selected improperly, and then the productive rate of nitric ether is low.U.S. Pat 2,768,964(56) the i.e. nitration mixture of the suitable proportioning of adding in reactor of continuous nitrification method that a kind of azeotropic that reduces pressure down steams ester and water is proposed, add nitric acid and alcohol continuously, and the nitric ether of generation and the continuous azeotropic of water are steamed, this method is used for synthetic lower boiling nitric ether productive rate preferably, but has only productive rate about 50% for high boiling nitric ether; With the rising of boiling point, temperature of reaction also raises, and side reaction hold to take place, and makes that the nitric ether productive rate is low, purity is low.
The objective of the invention is to propose a kind of in industrial easy enforcement, reaction at normal temperatures can obtain the synthesis technique of productive rate height, isooctyl ester nitrate that purity is high.
Design of the present invention achieves the above object by selecting suitable nitration mixture proportioning and nitrated temperature.Improper when the nitration mixture proportioning, or temperature selects improperly, purely can produce the side reaction of oxidation side chain when nitrated, reduces productive rate and purity, even reaction can not control, and produces violent the decomposition and material spray.Sometimes almost all be the side reaction of oxidation side chain, ester content only 1.7%.As select suitable nitration mixture proportioning and suitable temperature condition, product purity reaches more than 98%.But when temperature rose to 40 ℃, product purity reduced to 90%.
The synthetic technological condition of isooctyl ester nitrate of the present invention makes isooctyl alcohol not produce the side reaction of oxidation side chain, obtains productive rate height, isooctyl ester nitrate that purity is high, and the effect of the diesel cetane-number that is significantly improved in testing of engine.
Implementing the present invention carries out in tank reactor or overflow type reactor.Reactor is stainless steel and makes, and except that with the chuck cooling, the internal cooling pipe is housed still.
The effective icy salt solution cooling of the chuck of tank reactor and internal cooling.Lake sulphur nitration mixture concentration proportioning: nitric acid 15～33%, sulfuric acid 58～70%, water 5～15%.Wherein nitric acid dosage is than the nitrated required chemical equivalent excessive 0～13% of alcohol.After nitration mixture added reactor, alcohol added reactor from header tank.In half an hour, add.Temperature can be kept 0～40 ℃ in the reactor, adds the material back and continues to stir 5～30 minutes.Product leaves standstill the back and divides the disacidify layer, washes, alkali cleaning, is washed to pH=7, vacuum-drying product again.
Overflow reactor is a straight pipe type, and chuck and internal cooling pipe use the icy salt solution cooling.The alcohol charging is entered by reactor lower part, and nitration mixture enters from 1/3 of reaction mass height.Constantly stir 0.5～10 minute duration of contact during reaction.Keep material constant by upflow tube, effusive material leaves standstill the back at separator and divides the disacidify layer, washes, alkali cleaning, is washed to pH=7, vacuum-drying product again.
Another characteristics of the present invention are that reactor can have two kinds of glass and stainless steels by pressing empty jet nitrator (1) and cooling tube (6) to form.Cooling tube uses the icy salt solution cooling.Its structure such as Fig. 2.This kind technology is with certain pressure (0.2～1kg/cm
2) air be pressed in the jet nitrator, this moment, high velocity air formed outer mixing jetting with alcohol, formed interior mixing jetting with nitration mixture.Under action of high-speed airflow, alcohol, acid further mix through spraying larynx (9) to expansion segment, are emulsified into uniform emulsion at last, emulsion enters in the cooling tube (6), still keep the gas emulsus, so reactant mixes sufficient reacting, rapid, safety at short notice.
Another characteristics of the present invention are the preferable processing condition of isooctyl ester nitrate synthesis technique; Nitric-sulfuric acid concentration proportioning: nitric acid 20～25%, sulfuric acid 62～68%, water 7～13%; 10～25 ℃ of temperature of reaction.
The advantage of isooctyl ester nitrate synthesis technique of the present invention is that processing condition are simple, is adapted to various reactors, reaction at normal temperatures, and productive rate height, purity height, cost are low; In industrial easy realization, be convenient to promote the use of.
Accompanying drawing 1 of the present invention is that empty schematic flow sheet: the 1-of injection of a kind of pressure in the isooctyl ester nitrate synthesis technique presses empty jet nitrator, 2-acid jar, 3,5, the 6-cooling tube, 4-alcohol jar, 7-gas-liquid separator, 8-thermostatic bath.
Accompanying drawing 2 is the sectional views of pressing empty jet nitrator: 9-sprays larynx.
Embodiment:
1. in tank reactor, add 1950 parts of nitration mixture, its concentration proportioning: HNO
320%, H
2SO
468%, H
2O12%, the effective icy salt solution cooling of chuck and internal cooling, from header tank isooctyl alcohol is added reactor for 720 parts, adding speed makes temperature of reaction maintain 20～25 ℃ and adds half an hour approximately, continues stirring under this temperature more than half an hour, standing demix then, remove acid solution, the ester layer is washed, alkali cleaning, is washed to pH=7, vacuum-drying again, product purity is 98%, yield 97.5%.
2. process only changes nitration mixture proportioning: HNO with example 1
325%, H
2SO
462%, H
2O13%.Product purity is 97.5%, yield 97.0%.
3. in overflow reactor, with 1950 parts of nitration mixture (proportioning is with example 1) and 720 parts of alcohol at the same time between in enter reactor continuously, under fully stirring, 5 minutes duration of contact are from the material inflow separator of upflow tube outflow, standing demix, divide disacidify liquid, the ester layer is through washing, alkali cleaning, be washed to pH=7, vacuum-drying again, product purity is 97%, yield 96.5%.
4. implement with reference to Fig. 1, at first feed pressurized air to nitrator 1, then at the same time between in 1950 parts of nitration mixture be depressed into nitrator (1) through cooling tube (3) and 720 parts of alcohol through cooling tube (5) spray nitrated, spray into in the icy salt solution round-robin cooling tube (6), about 1.5 minutes residence time, temperature of reaction is controlled at 20～25 ℃, gas emulsions enters gas-liquid separator (7) then, after the gas emptying, reactant flows into separator, carry out aftertreatment, product purity 97.0%, yield 95.0%.
Claims (3)
1, a kind of synthesis technique of isooctyl ester nitrate, this method are with isooctyl alcohol ester and nitration mixture prepared in reaction following formula: compound:
It is characterized in that the nitric-sulfuric acid concentration proportioning in the reactor: nitric acid 15～33%, sulfuric acid 58～70%, water 5～15%; 0～40 ℃ of temperature of reaction.
2, synthesis technique according to claim 1 is characterized in that using one by the reactor of pressing empty jet nitrator (1), cooling tube (6) to form.
3, synthesis technique according to claim 1 is characterized in that the preferred process condition, the nitric-sulfuric acid concentration proportioning: nitric acid 20～25%, sulfuric acid 62～68%, water 7～13%; 10～25 ℃ of temperature of reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87105712 CN1017146B (en) | 1987-08-24 | 1987-08-24 | Synthesizing process of isooctyl ester nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87105712 CN1017146B (en) | 1987-08-24 | 1987-08-24 | Synthesizing process of isooctyl ester nitrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1031525A CN1031525A (en) | 1989-03-08 |
| CN1017146B true CN1017146B (en) | 1992-06-24 |
Family
ID=4815424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87105712 Expired CN1017146B (en) | 1987-08-24 | 1987-08-24 | Synthesizing process of isooctyl ester nitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1017146B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787092B (en) * | 2010-02-10 | 2011-08-03 | 莱芜钢铁集团有限公司 | Amido polyving akohol poly-nitricether as improver of cetane number of diesel oil |
| CN102964255B (en) | 2012-12-04 | 2013-12-25 | 山东力宝得化工股份有限公司 | Safe production method for alkyl nitrate |
| CN104892425A (en) | 2014-03-07 | 2015-09-09 | 康宁股份有限公司 | Continuous synthesis of isooctyl nitrate in flow reactor |
| CN104557556B (en) * | 2015-01-26 | 2017-07-18 | 大连微凯化学有限公司 | A kind of device and process for producing isooctyl ester nitrate |
| RU2640953C2 (en) * | 2016-07-12 | 2018-01-18 | Федеральное Казенное Предприятие "Бийский Олеумный Завод" | Method for obtaining 2-ethylhexylnitrate |
-
1987
- 1987-08-24 CN CN 87105712 patent/CN1017146B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1031525A (en) | 1989-03-08 |
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