CN104327878A - N-alkane and preparation method thereof - Google Patents
N-alkane and preparation method thereof Download PDFInfo
- Publication number
- CN104327878A CN104327878A CN201410534232.5A CN201410534232A CN104327878A CN 104327878 A CN104327878 A CN 104327878A CN 201410534232 A CN201410534232 A CN 201410534232A CN 104327878 A CN104327878 A CN 104327878A
- Authority
- CN
- China
- Prior art keywords
- normal paraffin
- preparation
- hydrogenation catalyst
- porcelain ball
- condition
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to the n-alkane production field, and in particular, relates to n-alkane and a preparation method thereof. The preparation method of the n-alkane comprises the steps: (A) with waste animal and plant grease as raw material, refining, carrying out an esterification reaction with ethanol or methanol to generate fatty acid methyl ester, and then purifying to obtain fatty acid refined methyl ester; (B) taking a metal oxide containing one or more of Ni, Mo, Co, Pd and Cu metal elements to prepare a solid with Al2O3 as a carrier, and roasting to obtain a hydrogenation catalyst for standby application; and (C) under a condition of the hydrogen-to-oil volume ratio of 1000-1100:1, carrying out a hydrogenation reaction on the fatty acid refined methyl ester and hydrogen with the hydrogenation catalyst as a catalyst, and thus obtaining the n-alkane. The preparation method has easily obtained raw materials which are inexhaustible renewable resources in China, and also promotes 'reduction, harmlessness and resource' treatment on Chinese city domestic garbage.
Description
Technical field
The present invention relates to normal paraffin production field, in particular to a kind of normal paraffin and preparation method thereof.
Background technology
In the lipid acid that normal paraffin is mainly derived from organism and paraffin-base petroleum, in petroleum naphtha, content is 55.4%, normal paraffin is used for ethene, oil dope, premium grads whiteruss, the production of softening agent etc., other is also for leather oiling agent, Premium detergents, makeup, fertilizer additive, daily necessities thinner, solvent, farm chemical emulgent, the raw material of medicine and petroprotein and for vaporizer mosquito liquid, aluminium rolling mill compound, diprotic acid, plastic, rubber solvent, textile auxiliary agent base oil, cloth printing ink solvent, electrical discharge machine treated oil, special slushing oil base oil, intermetallic composite coating base oil, metal cleaner, lamp liquid wax, fine perfumery, nylon plastic etc.Normal paraffin is the main raw material producing ethene, and ethene is the flagship product of petrochemical complex, is the core of petrochemical industry, is the basic material of petrochemical industry, and petrochemicals about 75 ﹪ is by ethylene production.Ethene is very fast in China's output increase, current domestic annual capacity has reached about 1,500 ten thousand tons, but the annual equivalent demand of China is 2400-2600 ten thousand tons, comprise the ethene derived product degree of self-sufficiency less than 50 ﹪, reason due to raw material can not meet the demand in derived product market, and China also needs a large amount of ethene of import and ethene derived product every year.
China is alkane production and consumption big country in the world, raw material mainly comes from petroleum naphtha, but at present along with the exhaustion day by day of world's fuel oil, energy starved is in short supply is the realistic problem that current China energy industry faces, and the crude oil of the present import of China is with poor quality oil, mink cell focus is in the majority, following such situation does not still have too large change, impel China's refined oil supply to must pass through technological innovation and carry out industrial upgrading, transition, aromatic hydrocarbons is subtracted on the one hand by pressure, alkene and liquefied gas, the output of the products such as propylene increases production vapour, diesel oil is to ensure Oil Product Market supply, on the one hand improve oil quality by carrying out shortening reformation cracking to the alkane of petroleum naphtha and aromatic hydrocarbons with this again, thus cause petroleum naphtha to supply unavoidable having too many difficulties to cope with and seem more nervous, also cause alkane shortage with the anxiety of petroleum naphtha simultaneously.
Therefore how to find a kind of low cost of normal paraffin, main direction of studying that synthetic route that raw material is easy to get is present this area.
Summary of the invention
The object of the present invention is to provide a kind of normal paraffin and preparation method thereof, to solve the above problems.
Provide a kind of preparation method of normal paraffin in an embodiment of the present invention, comprise the steps:
(A) take waste animal and vegetable oil as raw material, through refining, generates fatty acid methyl ester with ethanol or methyl alcohol generation esterification, fatty acid methyl ester obtained after purification step the smart methyl esters of lipid acid;
(B) by the metal oxide containing one or more in Ni, Mo, Co, Pd and Cu metallic element with Al
2o
3for carrier prepares decorating film, described decorating film roasting 8-10h under the condition of 430-450 DEG C is obtained hydrogenation catalyst for subsequent use;
(C) by described lipid acid essence methyl esters and hydrogen under hydrogen to oil volume ratio is the condition of 1000-1100:1, with described hydrogenation catalyst for catalyzer carries out hydrogenation reaction, reaction pressure is 2-2.5MPa, temperature of reaction controls at 280-360 DEG C, lipid acid essence methyl esters and the total mass of hydrogen and the mass ratio of hydrogenation catalyst are 1-1.2:1, namely obtain normal paraffin after reacting 60-70min.
The preparation method of the normal paraffin that the embodiment of the present invention provides, compared with the preparation method of normal paraffin of the prior art, its with waste animal and vegetable oil (sewer oil) for raw material, turned waste into wealth, by by sewer oil lactate synthesis fatty acid methyl ester, then fatty acid methyl ester carries out catalytic hydrogenation reaction generation normal paraffin, this preparation method's raw material is easy to get, the inexhaustible renewable resource of China, but also facilitate " the minimizing of China's domestic waste, innoxious, resource utilization " process, construct the Mode of Circular of sustainable development, environmental protection purifying contaminated thing, therefore the method how utilizing waste animal and vegetable oil (sewer oil) to produce normal paraffin of the present invention, to alleviating the in short supply of petroleum alkane, reduce the consumption of petroleum-based energy, create good Social benefit and economic benefit and have very important function and significance.
Preferably, the purity of described hydrogen reaches more than 99.9%, and use the high hydrogen of purity to be conducive to the carrying out reacted, improve transformation efficiency and yield, the selectivity of hydrogenation catalyst reaction reaches 100%, and the yield of product normal paraffin is 99.5-99.8%.
Preferably, in described step (B), preparing described hydrogenation catalyst is with Al by the metallic compound containing Ni, Mo, Co
2o
3for carrier prepares roasting gained after decorating film, wherein said Ni, Mo, Co metallic element and Al
2o
3the mass ratio of carrier is 26-29:16-18:2-3:56.
Preferably, described Ni, Mo, Co metallic element and Al
2o
3the mass ratio of carrier is 26-27:16-17:2-2.5:56.
With the catalyzer that this three kinds of elements are prepared, catalytic activity is good, when carrying out catalyzed reaction, the selectivity of reaction can be made to reach 100%, product yield reaches 99.8%, and the shape of described catalyzer is preferably solid strip, size is preferably Φ 0.2cm × 3cm, therefore the catalyzer making strip is not easy to block reactor, and void ratio is beneficial to more greatly running through of raw material between such catalyzer, also have its length had better not be oversize otherwise be easy to rupture, wherein adding Co metallic element in activeconstituents can when hydrogenation reaction, control reaction and not easily isomerization occurs.
Preferably, between described step (B) and described step (C), comprise the steps:
Described hydrogenation catalyst is filled in fixed-bed reactor and forms beds and carry out prevulcanized, by the H of hydrogen and vulcanizing agent
2/ vulcanizing agent volume ratio controls under the condition of 1000-1100:1, and pressure-controlling is at 2-2.2MPa, and the air speed of described vulcanizing agent is 0.5-0.6h
-1, temperature is sulfuration 2-3h under the condition of 170-180 DEG C, is warming up to sulfuration 8-10h under the condition of 230-240 DEG C, is then warming up to sulfuration 8-10h under the condition of 320-330 DEG C, namely completes prevulcanized;
When carrying out hydrogenation reaction in described step (C), reaction conditions is: hydrogen to oil volume ratio is 1000-1100:1, and the inlet temperature of described fixed-bed reactor controls at 280-290 DEG C, and temperature out controls at 350-360 DEG C, and air speed is 1.0-1.2h
-1, reaction pressure is 2-2.5MPa.Because fixed-bed reactor productivity ratio is larger, and can continuous seepage be realized, therefore the reaction of the further shortening generation normal paraffin of biofuel is carried out in fixed-bed reactor, and in order to make the activity of catalyzer greatly improve, needed to carry out segmentation prevulcanized to catalyzer before catalyzer carries out catalyzed reaction, vulcanizing agent generally selects Methyl disulfide.
Preferably, the heat-up rate carrying out fixed-bed reactor during hydrogenation catalyst presulfurizing carries out according to 10-12 DEG C/h, during prevulcanized, fixed-bed reactor need to heat up gradually according to certain amplitude, present regular slow intensification to make the prevulcanized milder of catalyzer and effectively, the activity of catalyzer can not be had influence on because of significantly temperature fluctuation.
Preferably, described hydrogenation catalyst is filled in beds described in step that fixed-bed reactor form beds and be positioned at the middle and lower part of described fixed-bed reactor, the top and the bottom of described beds load the porcelain ball packing layer of 50-60cm height respectively, to ensure the smooth stable and homogeneity of beds, make raw material uniformly by beds, channel and Biased flow phenomenon can not be there is.
Preferably, in described step (B), be arranged in the diameter 18-19mm of described porcelain ball packing layer according to porcelain ball on described beds top, 12-13mm, 6-7mm and 3-4mm fills from top to bottom successively, be arranged in the diameter 18-19mm of described porcelain ball packing layer according to porcelain ball of described beds bottom, 12-13mm, 6-7mm and 3-4mm fills from top to bottom successively, the porcelain ball that diameter is larger is placed on the direct impact withstood on from beds position farthest to catalyzer when most external can well resist charging, then successively according to the trend that the diameter of porcelain ball reduces gradually, near beds, for help raw material by during beds evenly be distributed on beds, wherein the porcelain ball of 3-4mm directly contacts with catalyzer and prevents catalyzer from revealing.
Preferably, diameter is the packing height of the porcelain ball of 18-19mm is 10-15cm, diameter is the packing height of the porcelain ball of 12-13mm is 10-15cm, diameter is the packing height of the porcelain ball of 6-7mm is 10-15cm, because the porcelain ball of often kind of diameter has different purposes, therefore each porcelain ball preferably all ensures certain packing height.
Preferably, 10-12 temperature measuring equipment is equidistantly provided with successively from bottom to top in described fixed-bed reactor, high temperature high voltage resistant thermopair preferably selected by temperature measuring equipment, namely facilitates that cost is low can also meet thermometric requirement, controls respectively to the temperature of beds and each responding layer.
The normal paraffin that the preparation method that the embodiment of the present invention additionally provides a kind of normal paraffin obtains, its performance perameter is as follows: the purity of normal paraffin is more than 98%, and bromine number is at below 0.8gBr/100g, and purity height impurity is little, only containing a small amount of aromatic hydrocarbons.
Embodiment
Below by specific embodiment son and the present invention is described in further detail.
Embodiment 1
The preparation method of normal paraffin is as follows:
(A) take waste animal and vegetable oil as raw material, through refining, generates fatty acid methyl ester with ethanol or methyl alcohol generation esterification, fatty acid methyl ester obtained after purification step the smart methyl esters of lipid acid;
(B) by containing the metal oxide nickel in Ni metallic element with Al
2o
3for carrier prepares decorating film, decorating film roasting 8h under the condition of 430 DEG C is obtained hydrogenation catalyst for subsequent use;
(C) by lipid acid essence methyl esters and hydrogen under hydrogen to oil volume ratio is the condition of 1000:1, be that catalyzer carries out hydrogenation reaction with hydrogenation catalyst, reaction pressure is 2MPa, temperature of reaction controls at 280 DEG C, lipid acid essence methyl esters and the total mass of hydrogen and the mass ratio of hydrogenation catalyst are 1:1, namely obtain normal paraffin after reaction 60min, reaction preference reaches 100%, and the yield of product normal paraffin is 99.5%.
Embodiment 2
The preparation method of normal paraffin is as follows:
(A) take waste animal and vegetable oil as raw material, through refining, generates fatty acid methyl ester with ethanol or methyl alcohol generation esterification, fatty acid methyl ester obtained after purification step the smart methyl esters of lipid acid;
(B) by containing metal oxide nickel, cobalt oxide and the molybdenum oxide in Ni, Mo, Co metallic element with Al
2o
3for carrier prepares decorating film, decorating film roasting 10h under the condition of 450 DEG C is obtained hydrogenation catalyst for subsequent use, wherein Ni, Mo, Co metallic element and Al
2o
3the mass ratio of carrier is 26:16:2:56;
(C) hydrogenation catalyst fills in fixed-bed reactor and forms beds and carry out prevulcanized, by the H of hydrogen and vulcanizing agent
2/ vulcanizing agent volume ratio controls under the condition of 1000:1, and pressure-controlling is at 2MPa, and the air speed of vulcanizing agent is 0.5h
-1, fixed-bed reactor heat up with the speed of 10-12 DEG C/h, are sulfuration 2h under the condition of 170 DEG C in temperature, are warming up to sulfuration 8h under the condition of 230 DEG C, are then warming up to sulfuration 8h under the condition of 320 DEG C, namely complete prevulcanized;
(D) by lipid acid essence methyl esters and hydrogen under hydrogen to oil volume ratio is the condition of 1000:1, be that catalyzer carries out hydrogenation reaction and obtains normal paraffin with hydrogenation catalyst, the inlet temperature of fixed-bed reactor controls at 280 DEG C, and temperature out controls at 350 DEG C, and air speed is 1.0h
-1, reaction pressure is 2MPa, and reaction preference reaches 100%, and the yield of product normal paraffin is 99.8%.
Embodiment 3
The preparation method of normal paraffin is as follows:
(A) take waste animal and vegetable oil as raw material, through refining, generates fatty acid methyl ester with ethanol or methyl alcohol generation esterification, fatty acid methyl ester obtained after purification step the smart methyl esters of lipid acid;
(B) by containing metal oxide nickel, cobalt oxide, cupric oxide and the molybdenum oxide in Ni, Mo, Co, Pd metallic element with Al
2o
3for carrier prepares decorating film, decorating film roasting 10h under the condition of 440 DEG C is obtained hydrogenation catalyst for subsequent use, wherein Ni, Mo, Co, Pd metallic element and Al
2o
3the mass ratio of carrier is 29:18:3:2:56;
(C) middle and lower part that hydrogenation catalyst fills in fixed-bed reactor forms beds, the top and the bottom of beds load the porcelain ball packing layer of 50cm height respectively, the porcelain ball packing layer being arranged in beds top is filled from top to bottom successively according to diameter 18-19mm, 12-13mm, 6-7mm and 3-4mm of porcelain ball, and the described porcelain ball packing layer being arranged in beds bottom is filled from top to bottom successively according to diameter 18-19mm, 12-13mm, 6-7mm and 3-4mm of porcelain ball;
(D) catalyzer is carried out prevulcanized, by the H of hydrogen and vulcanizing agent
2/ vulcanizing agent volume ratio controls under the condition of 1100:1, and pressure-controlling is at 2.2MPa, and the air speed of vulcanizing agent is 0.6h
-1, fixed-bed reactor heat up with the speed of 10-12 DEG C/h, are sulfuration 3h under the condition of 180 DEG C in temperature, are warming up to sulfuration 10h under the condition of 240 DEG C, are then warming up to sulfuration 10h under the condition of 330 DEG C, namely complete prevulcanized;
(E) by lipid acid essence methyl esters and hydrogen under hydrogen to oil volume ratio is the condition of 1100:1, be that catalyzer carries out hydrogenation reaction and obtains normal paraffin with hydrogenation catalyst, the inlet temperature of fixed-bed reactor controls at 290 DEG C, and temperature out controls at 360 DEG C, and air speed is 1.2h
-1, reaction pressure is 2.5MPa, and reaction preference reaches 100%, and the yield of product normal paraffin is 99.6%.
Embodiment 4
The preparation method of normal paraffin is as follows:
(A) take waste animal and vegetable oil as raw material, through refining, generates fatty acid methyl ester with ethanol or methyl alcohol generation esterification, fatty acid methyl ester obtained after purification step the smart methyl esters of lipid acid;
(B) by containing metal oxide nickel, cobalt oxide and the molybdenum oxide in Ni, Mo, Co metallic element with Al
2o
3for carrier prepares decorating film, decorating film roasting 10h under the condition of 450 DEG C is obtained hydrogenation catalyst for subsequent use, wherein Ni, Mo, Co metallic element and Al
2o
3the mass ratio of carrier is 27:17:2.5:56;
(C) middle and lower part that hydrogenation catalyst fills in fixed-bed reactor forms beds, the top and the bottom of beds load the porcelain ball packing layer of 60cm height respectively, be arranged in the diameter 18-19mm of porcelain ball packing layer according to porcelain ball on beds top, 12-13mm, 6-7mm and 3-4mm fills from top to bottom successively, be arranged in the diameter 18-19mm of described porcelain ball packing layer according to porcelain ball of beds bottom, 12-13mm, 6-7mm and 3-4mm fills from top to bottom successively, wherein diameter is the packing height of the porcelain ball of 18-19mm is 10-15cm, diameter is the packing height of the porcelain ball of 12-13mm is 10-15cm, diameter is the packing height of the porcelain ball of 6-7mm is 10-15cm,
(D) catalyzer is carried out prevulcanized, by the H of hydrogen and vulcanizing agent
2/ vulcanizing agent volume ratio controls under the condition of 1100:1, and pressure-controlling is at 2.2MPa, and the air speed of vulcanizing agent is 0.6h
-1, fixed-bed reactor heat up with the speed of 10-12 DEG C/h, are sulfuration 3h under the condition of 180 DEG C in temperature, are warming up to sulfuration 10h under the condition of 240 DEG C, are then warming up to sulfuration 10h under the condition of 330 DEG C, namely complete prevulcanized;
(E) by lipid acid essence methyl esters and hydrogen under hydrogen to oil volume ratio is the condition of 1100:1, be that catalyzer carries out hydrogenation reaction and obtains normal paraffin with hydrogenation catalyst, the inlet temperature of fixed-bed reactor controls at 290 DEG C, and temperature out controls at 360 DEG C, and air speed is 1.1h
-1, reaction pressure is 2.4MPa, and reaction preference reaches 100%, and the yield of product normal paraffin is 99.8%.
Experimental example 1
By the reaction product normal paraffin of embodiment 1-4, key lab of bounties biomass fine chemistry industry Beijing of censorship Beijing Institute of Petrochemical Technology is detected, and the specific performance index of product is as shown in table 1 below:
The performance index parameter of table 1 normal paraffin
As can be seen from Table 1, the normal paraffin that the embodiment of the present invention is prepared meets the top grade product standard of country completely, inclusion-free, purity is high, and preparation method's sewer oil of the present invention is as raw material, to alleviate petroleum alkane in short supply, the consumption that reduces petroleum-based energy, create good Social benefit and economic benefit and have very important function and significance.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for normal paraffin, is characterized in that, comprises the steps:
(A) take waste animal and vegetable oil as raw material, through refining, generates fatty acid methyl ester with ethanol or methyl alcohol generation esterification, fatty acid methyl ester obtained after purification step the smart methyl esters of lipid acid;
(B) by the metal oxide containing one or more in Ni, Mo, Co, Pd and Cu metallic element with Al
2o
3for carrier prepares decorating film, described decorating film roasting 8-10h under the condition of 430-450 DEG C is obtained hydrogenation catalyst for subsequent use;
(C) by described lipid acid essence methyl esters and hydrogen under hydrogen to oil volume ratio is the condition of 1000-1100:1, with described hydrogenation catalyst for catalyzer carries out hydrogenation reaction, reaction pressure is 2-2.5MPa, temperature of reaction controls at 280-360 DEG C, lipid acid essence methyl esters and the total mass of hydrogen and the mass ratio of hydrogenation catalyst are 1-1.2:1, namely obtain normal paraffin after reacting 60-70min.
2. the preparation method of a kind of normal paraffin according to claim 1, is characterized in that, in described step (B), preparing described hydrogenation catalyst is with Al by the metal oxide containing Ni, Mo, Co
2o
3for carrier prepares roasting gained after decorating film, wherein said Ni, Mo, Co metallic element and Al
2o
3the mass ratio of carrier is 26-29:16-18:2-3:56.
3. the preparation method of a kind of normal paraffin according to claim 2, is characterized in that, described Ni, Mo, Co metallic element and Al
2o
3the mass ratio of carrier is 26-27:16-17:2-2.5:56.
4. the preparation method of a kind of normal paraffin according to claim 1, is characterized in that, between described step (B) and described step (C), comprises the steps:
Described hydrogenation catalyst is filled in fixed-bed reactor and forms beds and carry out prevulcanized, by the H of hydrogen and vulcanizing agent
2/ vulcanizing agent volume ratio controls under the condition of 1000-1100:1, and pressure-controlling is at 2-2.2MPa, and the air speed of described vulcanizing agent is 0.5-0.6h
-1, temperature is sulfuration 2-3h under the condition of 170-180 DEG C, is warming up to sulfuration 8-10h under the condition of 230-240 DEG C, is then warming up to sulfuration 8-10h under the condition of 320-330 DEG C, namely completes prevulcanized;
When carrying out hydrogenation reaction in described step (C), reaction conditions is: hydrogen to oil volume ratio is 1000-1100:1, and the inlet temperature of described fixed-bed reactor controls at 280-290 DEG C, and temperature out controls at 350-360 DEG C, and air speed is 1.0-1.2h
-1, reaction pressure is 2-2.5MPa.
5. the preparation method of a kind of normal paraffin according to claim 4, is characterized in that, the heat-up rate carrying out fixed-bed reactor during hydrogenation catalyst presulfurizing carries out according to 10-12 DEG C/h.
6. the preparation method of a kind of normal paraffin according to claim 4, it is characterized in that, described hydrogenation catalyst is filled in beds described in step that fixed-bed reactor form beds and be positioned at the middle and lower part of described fixed-bed reactor, the top and the bottom of described beds load the porcelain ball packing layer of 50-60cm height respectively.
7. the preparation method of a kind of normal paraffin according to claim 6, it is characterized in that, in described step (B), the described porcelain ball packing layer being arranged in described beds top is filled from top to bottom successively according to diameter 18-19mm, 12-13mm, 6-7mm and 3-4mm of porcelain ball, and the described porcelain ball packing layer being arranged in described beds bottom is filled from top to bottom successively according to diameter 18-19mm, 12-13mm, 6-7mm and 3-4mm of porcelain ball.
8. the preparation method of a kind of normal paraffin according to claim 7, it is characterized in that, diameter is the packing height of the porcelain ball of 18-19mm is 10-15cm, and diameter is the packing height of the porcelain ball of 12-13mm is 10-15cm, and diameter is the packing height of the porcelain ball of 6-7mm is 10-15cm.
9. the normal paraffin that the preparation method of the normal paraffin described in any one of claim 1-8 obtains.
10. normal paraffin according to claim 9, is characterized in that, its performance perameter is as follows: the purity of normal paraffin is more than 98%, and bromine number is at below 0.8gBr/100g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410534232.5A CN104327878A (en) | 2014-10-11 | 2014-10-11 | N-alkane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410534232.5A CN104327878A (en) | 2014-10-11 | 2014-10-11 | N-alkane and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104327878A true CN104327878A (en) | 2015-02-04 |
Family
ID=52402692
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410534232.5A Pending CN104327878A (en) | 2014-10-11 | 2014-10-11 | N-alkane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104327878A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126812A (en) * | 2018-09-17 | 2019-01-04 | 龙岩卓越新能源股份有限公司 | Utilize the method for long-chain natural plants wax in production of biodiesel |
| CN109126813A (en) * | 2018-09-17 | 2019-01-04 | 龙岩卓越新能源股份有限公司 | Utilize the method for waste animal and plant fat production atoleine |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462915A (en) * | 2007-12-20 | 2009-06-24 | 中国石油化工股份有限公司 | Preparation of C6-C12 alkane |
| CN101787303A (en) * | 2010-03-12 | 2010-07-28 | 江苏卡特新能源有限公司 | Method for preparing alkane from acidized oil |
| CN103130602A (en) * | 2011-11-24 | 2013-06-05 | 中国石油化工股份有限公司 | Method for producing low-carbon olefin from animal and plant oil and waste animal and plant oil |
| CN103130601A (en) * | 2011-11-24 | 2013-06-05 | 中国石油化工股份有限公司 | Method for producing low-carbon olefin from animal and plant oil and waste animal and plant oil |
| CN103666519A (en) * | 2012-09-04 | 2014-03-26 | 中国石油天然气股份有限公司 | Method for preparing alkanes by hydrodeoxygenation of non-edible animal and vegetable oil |
| CN103725305A (en) * | 2013-12-17 | 2014-04-16 | 中国科学院广州能源研究所 | Method for preparing hydrocarbon liquid fuels from higher fatty acid methyl ester |
| CN104661988A (en) * | 2012-09-20 | 2015-05-27 | 纳幕尔杜邦公司 | Process for making linear long-chain alkanes using renewable feedstocks |
-
2014
- 2014-10-11 CN CN201410534232.5A patent/CN104327878A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462915A (en) * | 2007-12-20 | 2009-06-24 | 中国石油化工股份有限公司 | Preparation of C6-C12 alkane |
| CN101787303A (en) * | 2010-03-12 | 2010-07-28 | 江苏卡特新能源有限公司 | Method for preparing alkane from acidized oil |
| CN103130602A (en) * | 2011-11-24 | 2013-06-05 | 中国石油化工股份有限公司 | Method for producing low-carbon olefin from animal and plant oil and waste animal and plant oil |
| CN103130601A (en) * | 2011-11-24 | 2013-06-05 | 中国石油化工股份有限公司 | Method for producing low-carbon olefin from animal and plant oil and waste animal and plant oil |
| CN103666519A (en) * | 2012-09-04 | 2014-03-26 | 中国石油天然气股份有限公司 | Method for preparing alkanes by hydrodeoxygenation of non-edible animal and vegetable oil |
| CN104661988A (en) * | 2012-09-20 | 2015-05-27 | 纳幕尔杜邦公司 | Process for making linear long-chain alkanes using renewable feedstocks |
| CN103725305A (en) * | 2013-12-17 | 2014-04-16 | 中国科学院广州能源研究所 | Method for preparing hydrocarbon liquid fuels from higher fatty acid methyl ester |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126812A (en) * | 2018-09-17 | 2019-01-04 | 龙岩卓越新能源股份有限公司 | Utilize the method for long-chain natural plants wax in production of biodiesel |
| CN109126813A (en) * | 2018-09-17 | 2019-01-04 | 龙岩卓越新能源股份有限公司 | Utilize the method for waste animal and plant fat production atoleine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100513521C (en) | Preparation method of biological diesel oil | |
| CN101568622B (en) | Converting loads from renewable sources into good-quality diesel fuel bases | |
| KR101301459B1 (en) | Hydrorefining process and hydrorefined oil | |
| CN103801295B (en) | The Catalysts and its preparation method of aviation kerosine prepared by castor oil | |
| JP6226861B2 (en) | Solid acid catalyst, method for producing the same, and method for producing fatty acid alkyl ester using the same | |
| CN107974266B (en) | Method and system for producing aviation fuel components from waste oil | |
| CN101927168B (en) | Nickel-based catalyst for preparing isopropyl alcohol by acetone hydrogenation and application thereof | |
| CN102746871B (en) | From the method for biological oil and fat preparation fuel | |
| CN100590107C (en) | Method for producing mixed butanol and octanol by butanol and octanol residual liquid | |
| CN108504381B (en) | Method for preparing diesel oil with high cetane number by directly hydrogenating animal and vegetable oil | |
| CN107974265B (en) | Method for producing aviation fuel component from waste oil | |
| CN1240811C (en) | Process for hydrogenating oil obtained by fast cracking of bioplasm | |
| CN104327878A (en) | N-alkane and preparation method thereof | |
| CN102250634A (en) | Method for producing renewable gasoline and diesel oil by utilizing vegetable oil | |
| WO2010068203A1 (en) | Even carbon number paraffin composition and method of manufacturing same | |
| CN115725363A (en) | Process for preparing second-generation biodiesel by hydrogenating waste oil | |
| CN104774648B (en) | A kind of heavy benzene hydrogenation refines the method for clean fuel oil | |
| Bala et al. | Nanomaterials based sustainable bioenergy production systems: Current trends and future prospects | |
| CN107673952A (en) | The method that 1,2 propane diols and normal propyl alcohol are prepared using biological glycerol | |
| CN102807900B (en) | High-value utilization method for oxygen-enriched coal tar | |
| CN103687835B (en) | For being the method for propylene glycol by transformation of glycerol | |
| CN109294613A (en) | A kind of method that grease type raw material prepares hydrocarbon fuel | |
| CN102344338A (en) | Process for upgrading heavy benzene hydrogenation | |
| CN102464997B (en) | Hydrogenation method for producing motor fuel from biological grease | |
| KR101330183B1 (en) | Heterogeneous catalyst for preparing bio-diesel and method for preparing bio-diesel using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150204 |
|
| RJ01 | Rejection of invention patent application after publication |