The method for preparing n-decane by liquid wax
The present invention relates to the preparation method of n-decane, particularly is the preparation method of raw material with liquid wax.
N-decane requires the purity height as the solvent of polypropylene catalyst.Useful alpha-methyl styrene method of hydrotreating makes, owing to be to adopt pressurization catalytic reaction to produce, therefore investment is big, the cost height, and the product component complexity that this method obtains is difficult to separate, so the quality of n-decane product also is difficult for guaranteeing.
The method that the purpose of this invention is to provide the higher n-decane product of a kind of purity of cheapness.
The method for preparing n-decane that the present invention proposes, raw material adopts liquid wax, and it is that a kind of normal paraffin that contains is main, mainly by C
8~C
15The hydrocarbon mixture that normal paraffin is formed, generally it contains C
10Normal paraffin (3~5) wt%.Raw material is through taking off heavy wax, taking off light wax, n-decane rectifying and absorption process and obtain the n-decane product.Can also obtain simultaneously aluminum foil rolling oil and saponification liquor wax product.
In taking off heavy wax operation, the tower top temperature of taking off heavy wax tower is that 200~210 ℃ of tower still temperature are 240~245 ℃, theoretical plate number 15-25, take off in the light wax operation, the tower top temperature of taking off light wax tower is 160~170 ℃, tower still temperature is 210~220 ℃, theoretical plate number 28-40, in the n-decane rectification working process, the rectifying tower tower top temperature is 170~180 ℃, tower still temperature is 185.2~185.5 ℃, theoretical plate number 35-50, take off heavy wax, the equipment that takes off light wax, n-decane rectification working process is packing tower or tray column, (0.1-0.15MPa) operation under normal pressure.The service temperature of adsorption tanks is 150~190 ℃, and pressure is 0.3~0.5MPa, and air speed is 0.5~1NM
3/ M
3Sorbent material.The used sorbent material of adsorption tanks is molecular sieve, silica gel or carclazyte.Contain C in the raw material
10The high more separation acquisition n-decane product that helps more of normal paraffin amount.
Of the present invention with C
6~C
15Normal paraffin is in master's the liquid wax, wherein C
10Normal paraffin also can obtain highly purified n-decane product in the time of can be less than 2wt%, considers economically rationally and can guarantee the quality of this product, makes its purity more than 98.6wt%, requires C in the raw material
10Normal paraffin 〉=2wt%, C
9, C
10, C
11In isoparaffin<2wt%, aromatic hydrocarbons<1wt%, alkene<1000wt%, sulfide<30ppm.The service temperature of each operation is regulated in the said temperature scope according to the component of raw material and the change of component of Ge Ta charging.
Because the raw material that the present invention adopts is the product in the petroleum refining process, raw material sources are abundant.Main rectifying and the adsorptive separation technology process of adopting, therefore little than the method investment of hydrogenation reaction, Production Flow Chart is simple, processing ease, production cost is low, and obtains the higher n-decane product of purity easily.
Accompanying drawing is a general flow chart of the present invention.
As shown in drawings, heavy wax tower 2 is taken off in liquid wax 1 adding that raw material forms as mentioned above, and tower reactor material 4 is C12~C
15Cut, tower reactor material 4 obtain low-sulfur, low fragrant aluminum foil rolling oil 14 after sending into adsorption tanks 11 desulfurization, decolouring, and cat head material material 3 behind condenser 17 is sent into and taken off light wax tower 5, and tower reactor material 7 is mainly C11~C
13Cut, tower reactor material 7 are sent into adsorption tanks 12 and obtain saponification liquor wax 15 after the decolouring desulfurization, and the cat head material that takes off light wax tower 5 is mainly C8 to C10Cut, the material 6 behind condenser 18 enters n-decane rectifying column 8, and cat head material 9 is mainly C8、C
9Cut can be made fuel oil, and tower reactor material 10 obtains n-decane product 16 behind the deolefination in the adsorption tanks 13.
The n-decane product that adopts the inventive method to produce, through applying unit analytical test result: density 0.730, bromine number 0.03 gram bromine/100 grams, residue 0.002%, moisture content 80ppm, boiling range: 172.5 ℃ of initial boiling points, do 174.6 ℃, n-decane purity 98.61wt% meets Yanshan Petrochemical Co.'s company standard. Its cost only has 1/2 of imported product price.
Embodiment 1:
As shown in table 1, raw material is C
8~C
15Normal paraffin is main liquid wax, and wherein: n-decane is 1.95wt%.C
9, C
10, C
11In isoparaffin<2wt%, alkene<1.5wt%, aromatic hydrocarbons<1wt%, sulfide<30ppm.Obtain product n-decane (purity is 98.62wt%), aluminum foil rolling oil and saponification liquor wax.
Embodiment 2:
As shown in table 2, raw material is C
8~C
15Normal paraffin is main liquid wax, and wherein: n-decane is 5.0wt%.Obtain product n-decane (purity 98.63wt%), aluminum foil rolling oil and saponification liquor wax.
Embodiment 3:
As shown in table 3, raw material is C
8~C
15Normal paraffin is main liquid wax, and wherein: n-decane is 9.6wt%, obtains product n-decane (purity is 98.99wt%), aluminum foil rolling oil and saponification liquor wax.
Table 1.
| One, takes off heavy wax tower |
Two, take off light wax tower |
Three, n-decane rectifying tower |
| The thing stream number |
1 |
3 |
4 |
6 |
7 |
9 |
10 |
| The logistics title |
Charging |
Cat head |
The tower still |
Cat head |
The tower still |
Cat head |
The tower still |
| Temperature (℃) |
180 |
63.2 |
244.1 |
51.9 |
217.5 |
50.5 |
185.2 |
| Pressure (MPa) |
0.120 |
0.100 |
0.126 |
0.100 |
0.125 |
0.100 |
0.125 |
| Weight fraction |
C8+C9 |
0.0030 |
0.0049 |
0 |
0.1332 |
0 |
0.9945 |
0.0120 |
| C10 |
0.0200 |
0.0324 |
0 |
0.8651 |
0.0009 |
0.0055 |
0.9862 |
| C11 |
0.2550 |
0.4121 |
0.0010 |
0.0017 |
0.4277 |
0 |
0.0018 |
| ≥C12 |
0.7220 |
0.5506 |
0.9990 |
0 |
0.5714 |
0 |
0 |
| Reflux ratio |
1.0 |
25.89 |
7.54 |
| Stage number |
18 |
35 |
45 |
Table 2.
| One, takes off heavy wax tower |
Two, take off light wax tower |
Three, n-decane rectifying tower |
| The thing stream number |
1 |
3 |
4 |
6 |
7 |
9 |
10 |
| The logistics title |
Charging |
Cat head |
The tower still |
Cat head |
The tower still |
Cat head |
The tower still |
| Temperature (℃) |
180 |
80.3 |
243.5 |
53.3 |
217.3 |
50.5 |
185.2 |
| Pressure (MPa) |
0.120 |
0.100 |
0.126 |
0.100 |
0.125 |
0.100 |
0.125 |
| Weight fraction |
C8+C9 |
0.0050 |
0.0080 |
0 |
0.0884 |
0 |
0.9945 |
0.0125 |
| C10 |
0.0520 |
0.0831 |
0 |
0.9105 |
0.0009 |
0.0055 |
0.9863 |
| C11 |
0.2500 |
0.3988 |
0.0010 |
0.0011 |
0.4083 |
0 |
0.0012 |
| ≥C12 |
0.6930 |
0.5101 |
0.9990 |
0 |
0.5608 |
0 |
0 |
| Reflux ratio |
1.0 |
14.04 |
11.63 |
| Stage number |
16 |
33 |
40 |
Table 3.
| One, takes off heavy wax tower |
Two, take off light wax tower |
Three, n-decane rectifying tower |
| The thing stream number |
1 |
3 |
4 |
6 |
7 |
9 |
10 |
| The logistics title |
Charging |
Cat head |
The tower still |
Cat head |
The tower still |
Cat head |
The tower still |
| Temperature (℃) |
180 |
77.2 |
243.3 |
54.3 |
216.8 |
50.5 |
185.3 |
| Pressure (MPa) |
0.120 |
0.100 |
0.126 |
0.100 |
0.125 |
0.100 |
0.125 |
| Weight fraction |
C8+C9 |
0.0060 |
0.0090 |
0 |
0.0579 |
0 |
0.9945 |
0.0090 |
| C10 |
0.0980 |
0.1464 |
0 |
0.9410 |
0.0009 |
0.0055 |
0.9899 |
| C11 |
0.2610 |
0.3895 |
0.0010 |
0.0011 |
0.4607 |
0 |
0.0011 |
| ≥C12 |
0.6350 |
0.4551 |
0.9990 |
0 |
0.5384 |
0 |
0 |
| Reflux ratio |
1.0 |
9.219 |
18.19 |
| Stage number |
20 |
30 |
32 |