CN103421613A - Preparation method for environment-friendly hydraulic oil base oil - Google Patents
Preparation method for environment-friendly hydraulic oil base oil Download PDFInfo
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Abstract
The invention discloses a preparation method for environment-friendly hydraulic oil base oil. The preparation method for the environment-friendly hydraulic oil base oil comprises the steps that (1) raw materials containing grease of plant and animals and heterogeneous alcohol are reacted in a reactor on the condition that supported solid acid is used as a catalyst; (2) a part of materials obtained through the reaction in the step (1) are used as recycle materials to be returned back to the reactor, and the rest of the materials flow into a constant temperature buffer tank, the temperature of the buffer tank is controlled to be the same as the temperature of the reactor, and the pressure of the buffer tank is the normal pressure; (3) gas coming out of the constant temperature buffer tank is condensed and is returned back to the reactor to continue to take part in the reaction; (4) liquid coming out of the constant temperature buffer tank is washed by water, and then reduced pressure distillation is conducted on the liquid, namely, residual heterogeneous alcohol in the product is removed through distillation, and then hydraulic oil base oil long-chain heterogeneous ester is obtained through distillation. The preparation method for the environment-friendly hydraulic oil base oil has high percent conversion and selectivity, obtained hydraulic oil base oil is good in performance, the production process is simple, continuous, controllable, and low in cost, and the preparation method for the environment-friendly hydraulic oil base oil is suitable for industrialized mass production.
Description
Technical field
The present invention relates to the preparation method of hydraulic pressure base oil, particularly a kind of preparation method of take the green hydraulic efficiency oil base oil that animal-plant oil is raw material.
Background technology
Hydraulic efficiency oil is a class of consumption maximum in industrial lubricants, accounts for more than 50%, and it is mainly derived from raw mineral materials.Along with world's crude oil reserve day by day descend and people to the worry of environmental degradation, toxicological harmless, biodegradable, reproducible hydraulic efficiency oil will be the optimal selections of alternative ore base fluid force feed.Animal-plant oil is as a kind of natural raw material, its wide material sources, and annual production is huge; Animal-plant oil has good physico-chemical property: flash-point is high, and viscosity is large, the lubricity excellence, and the element such as sulfur-bearing, nitrogen, do not have viscosity-temperature characteristic preferably, toxicological harmless, and biodegradable, be the raw material of biofuel and biological lubricant uniqueness.
It should be noted that after the animal-plant oil modification as intrinsic its tempting application prospect of power fuel, but that its profit of bringing is affected by raw materials cost is very large, and added value is relatively low, life cycle is very limited.By contrast, animal-plant oil is further prepared to the higher biological lubricant of added value after processing, not only extend the life cycle of animal-plant oil, also can have been retrieved to alleviate the raw material supplying problem to waste lubrication oil, thereby brought higher commercial profit for enterprise.Especially take waste grease as raw material, it will reduce the production cost of biological lubricant base oil more significantly.
The main component of animal-plant oil is triglyceride level, when liquid, the triglyceride level molecule is arranged with irregular form, and along with temperature reduces, the easily crystallization gradually of triglyceride level molecule, form the solid ester of stratiform and separate out, this has obviously reduced the possibility of animal-plant oil as hydraulic efficiency oil.In addition, triglyceride level itself is subject to because containing β-H that free radical is attacked, during the extreme pressure condition, under the catalysis of metal ion, β-H is attacked by free radical easily and oxidizing reaction occurs, and generates macromole and then produces carbon distribution, has limited especially its application in hydraulic efficiency oil.Yet the intrinsic lipid acid of animal-plant oil itself has still represented unique value.How rationally utilizing lipid acid, the hydraulic efficiency oil base oil that animal-plant oil is converted into have higher commercial value, realize higher value application, is problem in the urgent need to address.
Summary of the invention
For the above-mentioned shortcoming and deficiency that overcomes prior art, the object of the present invention is to provide a kind of preparation method of green hydraulic efficiency oil base oil, take animal-plant oil as raw material, production cost is low, and production process is controlled continuously.
Purpose of the present invention is by the following technical programs:
A kind of preparation method of green hydraulic efficiency oil base oil comprises the following steps:
(1) will contain raw material and the isomery alcohol of animal-plant oil even by 1:4～1:10 mixed in molar ratio, pass in reactor, controlling temperature of reactor and be 135～200 ℃, pressure is 0.3～0.7MPa, under the effect of load-type solid acid catalyst, animal-plant oil (main component is triglyceride level) reacts with isomery alcohol; Reaction times is more than 4 hours; Contain the isomery alcohol that has neither part nor lot in reaction, animal-plant oil, reaction product long-chain isomery ester, the by-product glycerin that has neither part nor lot in reaction in the material obtained after reaction;
(2) by the material that obtains after step (1) reaction 30～60% in the recycle stock Returning reactor, rest materials flows in the constant temperature surge tank; Control surge tank temperature is identical with temperature of reactor, pressure is normal pressure; Now, in the material in the constant temperature surge tank, the animal-plant oil, reaction product long-chain isomery ester, the by-product glycerin that have neither part nor lot in reaction are liquid state; The amount of recycle stock can be selected according to isomery alcohol carbon chain lengths, and different carbon chain lengths isomery alcohol reacts with triglyceride level, and carbon chain lengths is longer, and the reaction difficulty is larger, and transformation efficiency also descends thereupon;
(3) condensation of gas out by the constant temperature surge tank, sustainable participation reaction in Returning reactor;
(4) by the constant temperature surge tank, liquid out washes with water, removes by-product glycerin, then carries out the underpressure distillation processing: first under normal pressure, 150～210 ℃, the isomery alcohol that has neither part nor lot in reaction is removed in distillation; Then at pressure, be distillation under 0.3～0.7kPa, 190～210 ℃, the light constituent obtained is hydraulic efficiency oil base oil long-chain isomery ester, and restructuring is divided into the animal-plant oil that has neither part nor lot in reaction.
The described raw material that contains animal-plant oil is natural animal-plant grease or waste animal and vegetable oil.
Described isomery alcohol is C
8The alcohol that more than there is side chain.
Described load-type solid acid is supported titanium
2/ SO
4 2-Solid acid or loading type ZrO
2/ SO
4 2-Solid acid.
The described reactor of step (1) is the shell and tube packed bed reactor.
Described supported titanium
2/ SO
4 2-The activated alumina that the carrier of solid acid is 3A, 4A, 5A, 13X molecular sieve or Ф 1～5mm.
Described loading type ZrO
2/ SO
4 2-The activated alumina that the carrier of solid acid is 3A, 4A, 5A, 13X molecular sieve or Ф 1～5mm.
Load-type solid acid of the present invention needs to process through heat-activated before use, remove moisture and other organic adsorbentses on catalyst surface, be the 30h left and right work-ing life, should regularly unload and make activation treatment, concrete working method: by 0.5mol/L sulfuric acid dilute solution, flood 24 hours, 500～600 ℃ of lower roasting 6h are reusable.
Triglyceride level in animal-plant oil of the present invention reacts with isomery alcohol, and detailed process is shown below:
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention adopts and to turn esterification process animal-plant oil, waste grease are carried out to modification, and wherein the transformation efficiency of triglyceride level reaches more than 75%, selectivity reaches more than 90%, realizes the efficient catalytic transesterification.
(2) raw material of the present invention is animal-plant oil renewable, biodegradable and that output is huge, or even the waste grease of high acid value.The popularity of raw material and compatibility make the promotion prospect of this technology brighter and clearer.
(3) operational path of the present invention is simple, and the production process serialization is applicable to large-scale industrialization production.The production of existing biological lubricant base oil mostly adopts homogeneous phase or intends homogeneous catalyst catalysis, inevitably has the link of catalyst separating in process, causes production cost to increase; And the present invention adopts load-type solid acid catalyst, reactant after the catalyst surface of flowing through reacts just with catalyst separating, effectively realized separating of catalyzer and reaction mass, process is simple and rapidly.
(4) catalyzer that the present invention adopts is TiO
2/ SO
4 2-, ZrO
2/ SO
4 2-Loaded catalyst, carrier used is that specific surface area is large, aperture is moderate, is insoluble to molecular sieve or the activated alumina of oil and water.TiO
2/ SO
4 2-, ZrO
2/ SO
4 2-For solid super-strong acid, acidity is sulfuric acid more than 100 times.While mixing with carrier, in the situation that high-temperature roasting, TiO
2/ SO
4 2-, ZrO
2/ SO
4 2-Ti in solid acid or Zr easily with carrier in Si or Al form binary oxide Ti-O-Si or Zr-O-Si(or Ti-O-Al, Zr-O-Al), make active ingredient be difficult for loss, SO
4 2-Effectively strengthened the acidity of catalyzer.This catalyzer is compared with heteropolyacid catalyst with homogeneous catalyst, have cheap, catalytic activity is high, separate simply, characteristics such as etching apparatus not.
(5) the present invention be take waste grease as raw material, realizes turning waste into wealth, and effectively reduces production cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The preparation method of the green hydraulic efficiency oil base oil of the present embodiment comprises the following steps:
(1) by load TiO
2/ SO
4 2-Solid acid catalyst is filled in the reactor tubulation, jatropha curcas oil and primary isoamyl alcohol is pressed to the 1:5 mixed in molar ratio even, passes in reactor, and controlling temperature of reactor and be 135 ℃, pressure is 0.3MPa, at load TiO
2/ SO
4 2-Under the effect of solid acid catalyst, jatropha curcas oil reacts with primary isoamyl alcohol; Reaction times is more than 4 hours; Contain the isomery alcohol that has neither part nor lot in reaction, jatropha curcas oil, reaction product long-chain isomery ester, the by-product glycerin that has neither part nor lot on a small quantity reaction in the material obtained after reaction; The load TiO of the present embodiment
2/ SO
4 2-The activated alumina that the carrier of solid acid is Ф 2～3mm.
(2) by the material that obtains after step (1) reaction 45% in the recycle stock Returning reactor, rest materials flows in the constant temperature surge tank; Control surge tank temperature is identical with temperature of reactor, pressure is normal pressure; Now, in the material in the constant temperature surge tank, have neither part nor lot in the primary isoamyl alcohol gasification of reaction, the jatropha curcas oil, reaction product long-chain isomery ester, the by-product glycerin that have neither part nor lot in reaction are liquid state.
(3) condensation of gas out by the constant temperature surge tank, sustainable participation reaction in Returning reactor.
(4) the equal-volume water washing three times for liquid out by the constant temperature surge tank, remove by-product glycerin, then carries out the underpressure distillation processing: first under normal pressure, 150 ℃ distillation remove product in residual primary isoamyl alcohol; Then at pressure, be distillation under 0.3kPa, 190 ℃, light constituent is hydraulic efficiency oil base oil (jatropha curcas oil isomery ester), and restructuring is divided into a small amount of unreacted jatropha curcas oil.
In the present embodiment, the transformation efficiency of triglyceride level is 78%, and selectivity is 95%.
The jatropha curcas oil isomery ester that the present embodiment obtains and the partial properties of jatropha curcas oil are as table 1.
The partial properties of table 1 jatropha curcas oil isomery ester and jatropha curcas oil
| Character | Jatropha curcas oil | Jatropha curcas oil isomery ester |
| Kinematic viscosity (40 ℃, cSt) | 47.48 | 7.8 |
| Kinematic viscosity (100 ℃, cSt) | 9.02 | 2.1 |
| Viscosity index | 174 | 48 |
| Pour point (℃) | 30 | -25 |
Embodiment 2
(1) by load ZrO
2/ SO
4 2-Solid acid catalyst is filled in the reactor tubulation, sewer oil and isooctyl alcohol is pressed to the 1:8 mixed in molar ratio even, passes in reactor, and controlling temperature of reactor and be 200 ℃, pressure is 0.7MPa, at load ZrO
2/ SO
4 2-Under the effect of solid acid catalyst, sewer oil reacts with isooctyl alcohol; Reaction times is more than 6 hours; Contain the isooctyl alcohol that has neither part nor lot in reaction, the sewer oil that has neither part nor lot on a small quantity reaction, reaction product long-chain isomery ester, by-product glycerin in the material obtained after reaction; The load ZrO of the present embodiment
2/ SO
4 2-The carrier of solid acid is the 13X molecular sieve.
(2) by the material that obtains after step (1) reaction 60% in the recycle stock Returning reactor, rest materials flows in the constant temperature surge tank; Control surge tank temperature is identical with temperature of reactor, pressure is normal pressure; Now, in the material in the constant temperature surge tank, have neither part nor lot in the isooctyl alcohol gasification of reaction, the sewer oil, reaction product long-chain isomery ester, the by-product glycerin that have neither part nor lot in reaction are liquid state;
(3) condensation of gas out by the constant temperature surge tank, sustainable participation reaction in Returning reactor;
(4) the equal-volume water washing three times for liquid out by the constant temperature surge tank, remove by-product glycerin, then carries out the underpressure distillation processing: first under normal pressure, 210 ℃ distillation remove product in residual isooctyl alcohol; Then at pressure, be distillation under 0.7kPa, 210 ℃, light constituent is hydraulic efficiency oil base oil long-chain isomery ester (sewer oil isomery ester), and restructuring is divided into a small amount of unreacted sewer oil.
In the present embodiment, the transformation efficiency of triglyceride level is 75.5%, and selectivity is 90%.
The sewer oil isomery ester that the present embodiment obtains and the partial properties of sewer oil are as table 2.
The sewer oil isomery ester that table 2 the present embodiment obtains and the partial properties of sewer oil
| Character | Sewer oil | Sewer oil isomery ester |
| Kinematic viscosity (40 ℃, cSt) | 38.7 | 10.2 |
| Kinematic viscosity (100 ℃, cSt) | 8.5 | 2.8 |
| Viscosity index | 206 | 121 |
| Pour point (℃) | 22 | -18 |
Above-described embodiment is preferably embodiment of the present invention, but embodiments of the present invention are not limited by the examples, as, supported titanium
2/ SO
4 2-The carrier of solid acid, loading type ZrO
2/ SO
4 2-The carrier of solid acid can be the activated alumina of 3A, 4A, 5A, 13X molecular sieve or Ф 1～5mm; Other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify, and all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (7)
1. the preparation method of a green hydraulic efficiency oil base oil, is characterized in that, comprises the following steps:
(1) will contain raw material and the isomery alcohol of animal-plant oil even by 1:4～1:10 mixed in molar ratio, pass in reactor, controlling temperature of reactor and be 135～200 ℃, pressure is 0.3～0.7MPa, and under the effect of load-type solid acid catalyst, animal-plant oil reacts with isomery is pure; Reaction times is more than 4 hours; Contain the isomery alcohol that has neither part nor lot in reaction, animal-plant oil, reaction product long-chain isomery ester, the by-product glycerin that has neither part nor lot in reaction in the material obtained after reaction;
(2) by the material that obtains after step (1) reaction 30～60% in the recycle stock Returning reactor, rest materials flows in the constant temperature surge tank; Control surge tank temperature is identical with temperature of reactor, pressure is normal pressure; Now, in the material in the constant temperature surge tank, have neither part nor lot in the isomery alcohol gasification of reaction, the animal-plant oil, reaction product long-chain isomery ester, the by-product glycerin that have neither part nor lot in reaction are liquid state;
(3) condensation of gas out by the constant temperature surge tank, sustainable participation reaction in Returning reactor;
(4) by the constant temperature surge tank, liquid out washes with water, removes by-product glycerin, then carries out the underpressure distillation processing: first under normal pressure, 150～210 ℃, distillation has neither part nor lot in the isomery alcohol of reaction in removing product; Then at pressure, be distillation under 0.3～0.7kPa, 190～210 ℃, the light constituent obtained is hydraulic efficiency oil base oil long-chain isomery ester, and restructuring is divided into the animal-plant oil that has neither part nor lot in reaction.
2. the preparation method of green hydraulic efficiency oil base oil according to claim 1, is characterized in that, the described raw material that contains animal-plant oil is natural animal-plant grease or waste animal and vegetable oil.
3. the preparation method of green hydraulic efficiency oil base oil according to claim 1, is characterized in that, described isomery alcohol is C
8The alcohol that more than there is side chain.
4. the preparation method of green hydraulic efficiency oil base oil according to claim 1, is characterized in that, described load-type solid acid is supported titanium
2/ SO
4 2-Solid acid-or loading type ZrO
2/ SO
4 2-Solid acid.
5. the preparation method of green hydraulic efficiency oil base oil according to claim 1, is characterized in that, the described reactor of step (1) is the shell and tube packed bed reactor.
6. the preparation method of green hydraulic efficiency oil base oil according to claim 4, is characterized in that, described supported titanium
2/ SO
4 2-The activated alumina that the carrier of solid acid is 3A, 4A, 5A, 13X molecular sieve or Ф 1～5mm.
7. the preparation method of green hydraulic efficiency oil base oil according to claim 4, is characterized in that, described loading type ZrO
2/ SO
4 2-The activated alumina that the carrier of solid acid is 3A, 4A, 5A, 13X molecular sieve or Ф 1～5mm.
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| CN114703006A (en) * | 2022-04-12 | 2022-07-05 | 山东奇士登润滑科技有限公司 | Biodegradable flame-retardant hydraulic oil and preparation method thereof |
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Application publication date: 20131204 |