CN101462920A - Method for preparing n-hexadecane under normal atmosphere - Google Patents
Method for preparing n-hexadecane under normal atmosphere Download PDFInfo
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- CN101462920A CN101462920A CN 200710151075 CN200710151075A CN101462920A CN 101462920 A CN101462920 A CN 101462920A CN 200710151075 CN200710151075 CN 200710151075 CN 200710151075 A CN200710151075 A CN 200710151075A CN 101462920 A CN101462920 A CN 101462920A
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- hexadecane
- preparing
- haloalkane
- under normal
- normal atmosphere
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Abstract
The invention belongs to a method for preparing hexadecane under ordinary pressure in the field of chemical agent, which comprises the steps: (1) glacial acetic acid is put into a reaction kettle and is sequentially added with zinc dust and haloalkane with the same level; (2) hydrochloric acid is dripped into the mixed solution, and the whole dripping process lasts for 22-26h and is kept to be in a circumfluence state; after the dripping process, the obtained mixed solution is maintained for 5-6h at the temperature of 100-110 DEG C, and the crude product of cetane liquid on the upper layer of the reaction mixture is separated; (3) the crude product of the cetane liquid is washed by sulphuric acid repeatedly, and then colorless or pale yellow cetane liquid is obtained and is washed to be neutral; (4) the obtained cetane liquid is dried by anhydrous magnesium sulfate, and after dryer is filtered out, the filtrate is distilled; finally, the finished product of the hexadecane is prepared. The method is a one-step synthesis mode of using hydrogen atom for deacidizing haloalkane, and utilizes sulphuric acid to replace aether to remove unsaturated hydrocarbon and alcohols, so as to have low fatalness, high safety factor and lowered cost.
Description
Technical field
The invention belongs to the chemical reagent field, relate to the method that a kind of hydrogen atom reduction bromoalkane prepares the method, particularly a kind of preparing n-hexadecane under normal atmosphere of even normal paraffin.
Background technology
One of normal paraffin is as one of key ingredient of environmental protection liquid fuel composition, and component of diesel oil at low-temperature improving agent, just be used widely.Simultaneously, the normal paraffin monomer also has crucial function in the analysis field such as organism in geology, crude oil and Atmospheric particulates.But owing to differ in the source of normal paraffin, cause the composition difference of its all kinds of normal paraffins, thereby make product on forming, have in various degree difference, thereby also need some special normal paraffin monomer adjustment prescriptions so that its quality can access maximum the assurance.Through the data at home and abroad investigation, concluding the method for getting up to be used to prepare normal paraffin has following several:
1. take the plain wax fractionation process of molecular sieve or urea to prepare the mixture of normal paraffin, and then carry out segmentation subzero fractionation normal paraffin monomer methods, typical process has the molex technology of VOP company, and the independently developed IUDW technology of China;
2. take Woertz prepared in reaction symmetry even normal paraffin.
3. adopt the idoalkane method of reducing.
In above three kinds of methods, first method processing condition more complicated is had relatively high expectations to some equipment, material, and scale of investment is bigger, only is suitable for extensive petrochemical industry production; Second method is to adopt sodium Metal 99.5 to link symmetrical haloalkane as reactant, and operational danger is bigger, and safety coefficient is lower; The third method is that the idoalkane reactant self exists great volatility, and the resultant crude product needs ether to extract repeatedly, and the cycle is longer, and cost is higher.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, provide that a kind of method is easy, raw material is easy to get, the method for the with short production cycle and preparing n-hexadecane under normal atmosphere that purity is higher.
The present invention realizes that the technical scheme of purpose is:
A kind of method of preparing n-hexadecane under normal atmosphere, the step of its preparation method is:
(1). earlier glacial acetic acid is placed in the reactor, adds zinc powder and same level haloalkane successively under stirring, mixture is warming up to 75～85 ℃;
(2). splash into the hydrochloric acid in the reactor high level tank, this moment, mixture temperature rose rapidly, and occurred with refluxing, whole dropping process 22～26 hours, and keep the backflow shape; Drip the back and kept again 5～6 hours at 100～110 ℃, with the mixture precipitation sinking, the n-Hexadecane liquid crude product of aspect on the separate reacted mixture;
(3). n-Hexadecane liquid crude product is adopted the sulfuric acid repetitive scrubbing, obtain colourless or pale yellow n-Hexadecane liquid, extremely neutral with the washing of 10% sodium hydroxide again;
(4). use anhydrous magnesium sulfate drying, distill filtrate after filtering out siccative, promptly obtain the n-hexadecane finished product.
And described same level haloalkane is a bromohexadecane.
And the part by weight of described glacial acetic acid, zinc powder and same level haloalkane is 31.4:10.7:10.
And described hydrochloric acid is concentration 36～38%, in hydrogenchloride 1015mol.
Advantage of the present invention and positively effect are:
1. raw material of the present invention is easy to get, and the present invention adopts industrial chemicals commonly used such as the competent bromohexadecane in market, zinc powder, glacial acetic acid, hydrochloric acid.
2. the inventive method is easy, and all in normal pressure, 18～110 ℃ of operations down, existence conditions all can reach whole process.
3. the present invention is the one-step synthesis mode that adopts hydrogen atom reduction haloalkane, and substitutes ether to remove unsaturated hydrocarbons and alcohols thing with sulfuric acid, and dangerous low, the safety coefficient height has reduced cost.
Embodiment
Below in conjunction with embodiment, the present invention is further described; Following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
A kind of method of preparing n-hexadecane under normal atmosphere, the step of its preparation method is:
(1). earlier 96kg glacial acetic acid (1600mol) is placed in the reactor, add 32.7kg zinc powder (5000mol) and 30.54kg bromohexadecane (1000mol) successively under stirring, and mixing is warming up to 80 ℃;
(2). splash into the hydrochloric acid (36～38%, in hydrogenchloride 1015mol) in the high level tank, this moment, mixture temperature rose rapidly, and occurred with refluxing; About 25 hours of whole process dripping hydrochloric acid 100kg, and keep the backflow shape, add the back and kept again 6 hours at 110 ℃, with the mixture precipitation sinking, isolate the n-Hexadecane liquid crude product that is raised to the reaction mixture surface;
(3). this n-Hexadecane liquid crude product adopts the sulfuric acid repetitive scrubbing, and each 2000ml obtains colourless or pale yellow liquid, and is extremely neutral with the washing of 10% sodium hydroxide again;
(4). behind anhydrous magnesium sulfate drying, filter out siccative, 287 ℃ of cuts are collected in distillation, output 19kg (be theory 80%), the stratographic analysis gradient can reach 96～98%.
Claims (4)
1. the method for a preparing n-hexadecane under normal atmosphere, it is characterized in that: the step of its preparation method is:
(1). earlier glacial acetic acid is placed in the reactor, adds zinc powder and same level haloalkane successively under stirring, mixture is warming up to 75～85 ℃;
(2). splash into the hydrochloric acid in the reactor high level tank, this moment, mixture temperature rose rapidly, and occurred with refluxing, whole dropping process 22～26 hours, and keep the backflow shape; Drip the back and kept again 5～6 hours at 100～110 ℃, with the mixture precipitation sinking, the n-Hexadecane liquid crude product of aspect on the separate reacted mixture;
(3). n-Hexadecane liquid crude product is adopted the sulfuric acid repetitive scrubbing, obtain colourless or pale yellow n-Hexadecane liquid, extremely neutral with the washing of 10% sodium hydroxide again;
(4). use anhydrous magnesium sulfate drying, distill filtrate after filtering out siccative, promptly obtain the n-hexadecane finished product.
2. the method for a kind of preparing n-hexadecane under normal atmosphere according to claim 1, it is characterized in that: described same level haloalkane is a bromohexadecane.
3. the method for a kind of preparing n-hexadecane under normal atmosphere according to claim 1, it is characterized in that: the part by weight of described glacial acetic acid, zinc powder and same level haloalkane is 31.4:10.7:10.
4. the method for a kind of preparing n-hexadecane under normal atmosphere according to claim 1, it is characterized in that: described hydrochloric acid is concentration 36～38%, in hydrogenchloride 1015mol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710151075 CN101462920A (en) | 2007-12-17 | 2007-12-17 | Method for preparing n-hexadecane under normal atmosphere |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710151075 CN101462920A (en) | 2007-12-17 | 2007-12-17 | Method for preparing n-hexadecane under normal atmosphere |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101462920A true CN101462920A (en) | 2009-06-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710151075 Pending CN101462920A (en) | 2007-12-17 | 2007-12-17 | Method for preparing n-hexadecane under normal atmosphere |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101462920A (en) |
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2007
- 2007-12-17 CN CN 200710151075 patent/CN101462920A/en active Pending
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| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Open date: 20090624 |