CN105670782A - Oil extraction process - Google Patents
Oil extraction process Download PDFInfo
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- CN105670782A CN105670782A CN201610066705.2A CN201610066705A CN105670782A CN 105670782 A CN105670782 A CN 105670782A CN 201610066705 A CN201610066705 A CN 201610066705A CN 105670782 A CN105670782 A CN 105670782A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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Abstract
The invention relates to an oil extraction process. According to the process, a nitrogen gas-stripping technique is applied to the desolution process of oilseed meal, a gas membrane separation technique is used for a recovery process of an organic solvent in noncondensable gas, accordingly, energy consumption and generation of organic wastewater are substantially reduced in the extraction process, the process and the operation are greatly simplified, and the operation cost during production is effectively reduced on the basis that the yield of crude oil is guaranteed by controlling the process condition. By comparison with a traditional process adopting a rice bran crude oil extraction device, the energy-saving rate of the novel extraction process can reach 45%, and the yield of organic wastewater in a water knockout drum part is remarkably reduced.
Description
Technical field
The invention belongs to oils and fats separation technology field, relate to a kind of grease lixiviating process and the oil extraction device based on this technique.
Background technology
Vegetable oil lipoprotein is requisite nutraceutical in current people life, and the data according to Zhong Shang industrial research institute data base show, within 2014, Chinese refined edible vegetable oil yield reaches 65,340,000 tons, increases by 5% than the same period in 2013, increases by 67% than 2010 years. This item data embodies Vegetable oil lipoprotein and has very large market in China. In numerous oil crop, soybean oil becomes topmost product on edible vegetable oil market with its abundant raw material quantity delivered, similar product also has palm-kernel oil and Testa oryzae oil etc., extraction process for this kind of oil plant, the extracting method that expansion extraction technique is acknowledged as efficiency height, profit margin is high, is suitable for large production.
Traditional expansion extraction technique, at oil plant after extrusion pretreatment, enter leaching section, oils and fats extract after produce containing miscella, the solvent-laden oil plant dregs of rice all adopt reduction vaporization, the technique of steam stripping carries out solvent separation, the fixed gas that mixed vapour produces after condensation is by after organic solvent (paraffin oil, vegetable oil) convective mass transfer, tail gas empties, condensed lime set goes water knockout drum to reclaim organic solvent after turnout is managed, and organic wastewater then discharges after treatment. Under the background of domestic, the competition in the international market being growing more intense now, how to reduce the energy expenditure of this process, reduce the generation of waste water, thus effectively reducing cost to become the key factor determining that can grease production enterprise well develop. And how can reduce the energy expenditure of leaching process while ensureing crude oil yield, reduce the discharge capacity of waste water, and to reduce operating cost be then that those skilled in the art thirst for solving always and fail the difficult problem succeeded so far.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, a kind of grease lixiviating process is provided, nitrogen air stripping technology is applied to the desolvation process of the solvent-laden oil plant dregs of rice by this technique, the removal process being used in fixed gas by gas membrane Seperation Technology organic solvent, thus the generation of the energy expenditure being greatly reduced in extract technology and organic wastewater, and ensureing the basis of crude oil yield effectively reduces the operating cost of its production.Present invention also offers a kind of oil extraction device based on above-mentioned grease lixiviating process, this device can realize the operation of said method preferably.
For this, the invention provides a kind of grease lixiviating process, comprising:
Process A, carries out leaching process to oil plant material base in the presence of solvent, it is thus achieved that miscella and the solvent-laden oil plant dregs of rice;
Process B, is evaporated miscella processing, it is thus achieved that crude oil and evaporation solvent vapo(u)r;
The solvent-laden oil plant dregs of rice are steamed de-process by process C, it is thus achieved that the thick oil plant dregs of rice and steaming desolventizing vapour mixture;
Wherein, the de-process of described steaming is undertaken by passing into nitrogen to precipitation layer.
According to the present invention, the intake of described nitrogen is 23-27m3The solvent-laden oil plant dregs of rice of/ton. The intake of preferred described nitrogen is 23-24.5m3The solvent-laden oil plant dregs of rice of/ton. It is preferred that the intake of described nitrogen is 24.5m3The solvent-laden oil plant dregs of rice of/ton. The intake of the nitrogen in the process C of the present invention is the gas-liquid phase equilibrium relation according to nitrogen and normal hexane solvent and lot of experiments is determined; The amount requiring the nitrogen passed in this process just can meet the solvent removal in the solvent-laden oil plant dregs of rice; If the intake of nitrogen is excessive, for instance more than 27m3The solvent-laden oil plant dregs of rice of/ton, can cause nitrogen circulation process operation cost to improve, and if the intake of nitrogen is too low, for instance lower than 23m3The solvent-laden oil plant dregs of rice of/ton, then can cause solvent removal in the solvent-laden oil plant dregs of rice not thorough.
In some preferred specific embodiments of the present invention, for instance in process C, the treating capacity of the solvent-laden oil plant dregs of rice is 8.17 ton hour, then the intake of nitrogen is about 200m3/ hour.
According to the present invention, described steaming takes off the operation temperature of process and is 50-55 DEG C. Preferred described steaming takes off the operation temperature of process and is 50-53 DEG C. It is preferred that it is 53 DEG C that described steaming takes off the operation temperature of process. The present inventor finds through experimental study, in the process C of the present invention steam the de-operation temperature processed select the temperature range more slightly higher than the temperature (about 50 DEG C) of the solvent-laden oil plant dregs of rice obtained after leaching process can be implemented in energy loss relatively low when carry out precipitation operation; If temperature selects relatively low, for instance lower than 50 DEG C, can lose the portion of energy in the solvent-laden oil plant dregs of rice; If selecting temperature too high, for instance higher than 53 DEG C, then process heat exchange engineering cost can be caused to raise.
In some embodiments of the invention, described steaming takes off the operation pressure of process is 0.05-0.07MPa. It is 0.05MPa that preferred described steaming takes off the operation pressure of process. The de-operation pressure processed that steams in the process C of the present invention is that the gas-liquid phase equilibrium relation according to the nitrogen passed into and normal hexane solvent, the de-operation temperature processed of steaming and lot of experiments are determined; This process requiring, realizing precipitation under about 53 DEG C of conditions operates the modest pressure condition that need to provide; If pressure selects too high, for instance higher than 0.07Mpa, can cause that solvent-laden oil plant dregs of rice solvent removal machine is not thorough, if pressure selects too low, for instance lower than 0.05Mpa, then cause unnecessary energy consumption to increase.
According to the present invention, described technique also includes the process D of solvent recovery: by evaporation solvent vapo(u)r produced in process B, produced steaming carries out condensation process, gas-liquid separation process and gaseous jet simulation after desolventizing vapour mixture converges and process with process C, it is thus achieved that recycling design and containing residual molten recovery nitrogen and be circulated utilization respectively.
In the present invention, described gaseous jet simulation processes and is at least the process of one-level gaseous jet simulation;The gaseous jet simulation that preferred described gaseous jet simulation processes more than for two-stage processes; It is preferred that described gaseous jet simulation processes as two-stage gas membrane separation.
According to the present invention, in process A, oil plant material base is carried out leaching process and includes oil plant material base is carried out multi-stage counter current extraction.
In some embodiments of the invention, in process A, the operation temperature that described leaching processes is 48-53 DEG C. The operation temperature that preferred described leaching processes is 53 DEG C.
In other embodiments of the present invention, the operation pressure that described leaching processes is normal pressure.
In the other embodiment of the present invention, the consumption of the solvent for leaching process is about 0.9-1 ton/ton oil plant material base. Such as, in leaching processing procedure, the inlet amount of oil plant material base is 7.60 ton hour, then the consumption of the solvent for leaching process is about 6.84-7.60 ton hour.
In the present invention, the solvent for leaching process includes fresh solvent and/or recycling design.
In the present invention, it is preferable that described fresh solvent is 6# solvent. No. 6 solvents are common industrial light solvent, and outward appearance is colourless transparent liquid, are the mixture of various lower paraffin hydrocarbon, and wherein normal hexane (boiling point 68.7 DEG C) is main component. 6# solvent product fraction scope relatively industrial hexane width, has the character that industrial hexane is similar. Can be miscible with the most liquid fats except Oleum Ricini, solubilized lower fatty acid.
According to the present invention some preferred embodiment, oil plant material base is carried out the process of pretreatment by described method before being additionally included in process A. Accordingly, in process A, carry out leaching process to through pretreated oil plant material base.
According to the present invention, in process B, miscella is evaporated process and includes miscella carries out the Ith grade of evaporation process, the IIth grade of evaporation process and stripping process successively.
In some specific embodiments of the present invention, miscella is evaporated process and includes:
Step L, carries out the Ith grade of evaporation process and obtains the Ith grade of evaporation oil and the Ith grade of evaporation solvent vapo(u)r miscella;
Step M, carries out the IIth grade of evaporation process and obtains the IIth grade of evaporation oil and the IIth grade of evaporation solvent vapo(u)r the Ith grade of evaporation oil;
Step N, evaporates oil and carries out stripping process acquisition crude oil the IIth grade.
Preferably, by separating device after the material stream heat exchange of the crude oil material stream obtained in step N and the Ith grade of evaporation oil. It is further preferable that by material stream heat exchange oily to the crude oil material stream that obtains in step N and the Ith grade of evaporation and after cooling separating device.
Residual molten amount < 0.3wt% in above-mentioned steps N, in described crude oil.
Term of the present invention " grease lixiviating process " can be understood as a kind of oil extraction method, referring to a kind of method applying nitrogen air stripping technology and gas membrane Seperation Technology optimization Vegetable oil lipoprotein extract technology, the method is also referred to as a kind of Novel low-consumption grease lixiviating process.
Present invention also offers a kind of oil extraction device, it includes loop type extractor and the evaporation process unit being connected with loop type extractor respectively and steams de-processing unit, and the de-processing unit of wherein said steaming includes the evapo-separated machine being connected with loop type extractor and the nitrogen gas generator from nitrogen to evapo-separated machine and the aerator that feed. The bottom of described evapo-separated machine is provided with air cooling equipment, for making the temperature of the defat oil plant dregs of rice be down to room temperature.
According to the present invention, described device also includes solvent recovery unit, it includes the IIth gas mixer, the IIth condenser, the IIIth gas mixer, the IIIth condenser, the Ith gas-liquid separator, gas compressor, filter, film separation unit, the IIth vapour liquid separator and water knockout drum successively by Flow of Goods and Materials direction, wherein, the charging aperture of the IIth gas mixer is connected with evapo-separated machine top by the Ith vacuum pump;The solvent of evaporation process unit goes out steam port and is connected via the charging aperture of the Ith gas mixer and the IIth heat exchanger and the IIth gas mixer.
In some embodiments of the invention, described solvent recovery unit also includes for making the concentration of the membrane separation assemblies in film separation unit return the closed circuit of the IIIth condenser mutually, and described closed circuit includes the IVth gas mixer, the IIth vacuum pump, the IIIth gas mixer and the IIIth condenser successively by Flow of Goods and Materials direction.
In other embodiments of the present invention, described solvent recovery unit also includes the pipeline for the solvent delivery the Ith gas-liquid separator and the IIth gas-liquid separator separates obtained to water knockout drum.
According to some embodiments of the present invention, described film separation unit includes at least one gaseous jet simulation assembly. Preferred described film separation unit includes the gaseous jet simulation assembly of more than two series connection. It is preferred that described film separation unit includes the gaseous jet simulation assembly of two series connection. In the present invention, it is preferable that described gaseous jet simulation assembly is rolled film device; Preferred membrane material is polydimethylsiloxane (PDMS) film; Preferred membrane area is 30-40m2/ ton crude oil; It is preferred that membrane area is 30-34m2/ ton crude oil; The membrane area being more highly preferred to is 34m2/ ton crude oil; Preferred membrane permeation lateral pressure is less than 1kPa.
The present inventor studies discovery, and in gaseous jet simulation processing procedure, membrane permeation lateral pressure is less than 1kPa, and membrane separating effect is better; The present inventor have selected commercially available PDMS film as membrane material through lot of experiments; Through a large amount of optimization Test, the PDMS material that thickness is 30 μm is carried on the backing material that thickness is 100 μm and is made for gas separation membrane.
The present inventor further study show that, although operation temperature rising can make membrane flux rise, but the higher meeting of temperature makes film generation swelling, reduces the life-span of film. Inventor determines the membrane flux under moderate membrance separation temperature and relevant temperature based on the studies above result by lot of experiments, and determines preferred membrane area in conjunction with the residual molten amount in the solvent-laden oil plant dregs of rice. Such as, 35 DEG C and membrane permeation lateral pressure less than 1kPa when, the flux of normal hexane is 2-2.2m by the PDMS film of the present invention3/(m2H atm), membrane area is then 30-40m2/ ton crude oil; Preferred membrane area is 34m2/ ton crude oil; In this process, the membrane area used is less than setting, for instance 30m2/ ton crude oil, or the hypertonia of membrane permeation side, for instance more than 1kPa, the treating capacity and the separating effect that are all likely to result in film decline.
According to certain embodiments of the present invention, in solvent recovery unit, described filter is filled by hydrophilic filler, primarily serves the purpose of a small amount of moisture of removing and solid impurity.
According to certain embodiments of the present invention, described evaporation process unit is connected with loop type extractor by pump, and it includes the Ith grade of vaporizer, the Ith heat exchanger, the IIth grade of vaporizer and stripper successively according to Flow of Goods and Materials direction. Preferred described evaporation process unit also includes the Ith condenser being connected via the Ith heat exchanger with stripper.
In the present invention, the IIth gas mixer, the IIth condenser, the IIIth gas mixer and the IIIth condenser constitute the condenser system of solvent recovery unit.
In the present invention, solvent recovery unit, and the circulation line that the organic solvent that this unit reclaims is sent back to infuser constitutes the solvent circulation of apparatus of the present invention.
In apparatus of the present invention, solvent recovery unit, and the circulation line that the nitrogen that this unit reclaims is sent back to evapo-separated machine constitutes the nitrogen circulating system of apparatus of the present invention.
The present invention still further provides a kind of said apparatus and prepares the application in crude oil in oil extraction method.
Term of the present invention " evaporation process miscella concentration " refers to the oil content in the miscella that evaporation process obtains, and represents with percentage by weight.
Term of the present invention " residual molten amount " refers to the content of the volatile ingredient of residual, represents with percentage by weight.
" residual molten " of the present invention word refers to the volatile ingredient of residual.
Term of the present invention " steams desolventizing vapour mixture " and refers to and steams the gaseous mixture that desolventizing steam, nitrogen and a small amount of steam are formed.
Term of the present invention " gassing process " refers to that gas-liquid separation processes.
Term of the present invention " oil content " refers to the amount of oils and fats contained in miscella or evaporation miscella or crude oil.
Heretofore described term " the concentration phase of membrane separation assemblies " refers to the high concentration solvent steam (being also known as concentration tail gas in the present invention) that the membrane permeation side of membrane separation assemblies obtains.
The organic solvent containing a small amount of organic wastewater that the solvent recovery unit that refers to heretofore described term " thick recycling design " reclaims, this thick recycling design separates, through water knockout drum, the recycling design obtained after a small amount of organic wastewater can send infuser recycling back to.
Term of the present invention " PSA nitrogen generator " is also known as varying-voltage adsorption nitrogen machine (PressureSwingAdsorption), and the principle of PSA is to utilize molecular sieve that admixture of gas is separated by the difference of gas with various molecule " absorption " performance; PSA nitrogen generator is with air for raw material, utilizes the solid absorbent of a kind of high-effect, high selection to the performance of nitrogen and the selective absorption of oxygen the nitrogen in air and oxygen separating out, thus preparing the device of nitrogen.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is described in further detail:
Fig. 1 is the flow chart of grease lixiviating process of the present invention.
Fig. 2 is the flow chart of traditional Rice bran crude oil extract technology.
In figure, the implication of accompanying drawing labelling is as follows: 1 oil plant material base; 1 ' Testa oryzae charging; 2 solvents; 2 ' 6# solvents; 3 crude oils; The 4 raw steam being passed directly into; 5 air; 5 ' steam (include the raw steam being passed directly into and the steam passed in chuck); The 6 thick oil plant dregs of rice; 6 ' brown shorts the dregs of rice; 7 reclaim nitrogen; 8 organic wastewaters; 9 recycling design; 10 paraffin oil; The 11 raw steam being passed directly into; 12 tail gas (without solvent); 13 circulation paraffin oil (feeding absorption tower 61); Solvent vapo(u)r (feeding the IIIth condenser 46) in 14 tail gas reclaimed; 21 infusers; 22 pumps; 23 the Ith grades of vaporizers; 24 the Ith heat exchangers; 25 the IIth grades of vaporizers; 26 strippers; 27 the Ith condensers; 31 evapo-separated machines; 32 aerators; 33 nitrogen gas generators; ; 41 the Ith gas mixers; 42 the Ith vacuum pumps; 43 the IIth gas mixers; 44 the IIth condensers; 45 the IIIth gas mixers; 46 the IIIth condensers; 46 ' the IIIth heat exchangers; 47 the Ith gas-liquid separators; 48 gas compressors; 49 filters; 50 the Ith gaseous jet simulation assemblies; 51 the IIth gaseous jet simulation assemblies; 52 the IIth gas-liquid separators; 53 water knockout drums; 54 the IIth heat exchangers; 54 ' the Ith preheaters; 55 the IVth gas mixers; 56 the IIth vacuum pumps; 57 pipelines; 58 the IIIth gas-liquid separators; 61 absorption towers; 62 the IVth heat exchangers; 63 the IIth preheaters; 64 Analytic Towers; 65 the IVth condensers.
Detailed description of the invention
For making the present invention easier to understand, describing the present invention in detail below in conjunction with drawings and Examples, these embodiments only play illustrative effect, it is not limited to the range of application of the present invention, NM specific experiment method in the following example, generally conventionally experimental technique carries out.
Fig. 1 is the flow chart of grease lixiviating process of the present invention.It will be seen from figure 1 that the device based on the grease lixiviating process of the present invention includes loop type extractor 21 and the evaporation process unit being connected with loop type extractor 21 and steams de-processing unit.
The de-processing unit of described steaming includes the evapo-separated machine 31 being connected with loop type extractor 21 and the PSA nitrogen generator 33 from nitrogen to evapo-separated machine 31 and the aerator 32 that feed; The bottom of described evapo-separated machine 31 is provided with air cooling equipment (not shown), for making the temperature of the defat oil plant dregs of rice be down to room temperature.
Described evaporation process unit is connected with loop type extractor 21 by pump 22, and it includes the Ith grade of vaporizer the 23, the Ith heat exchanger 24, the IIth grade of vaporizer 25 and stripper 26 successively according to Flow of Goods and Materials direction. Preferred described evaporation process unit also includes the Ith condenser 27 being connected via the Ith heat exchanger 24 with stripper 26.
Described device also includes solvent recovery unit, and it includes the IIth gas mixer the 43, the IIth condenser the 44, the IIIth gas mixer the 45, the IIIth condenser the 46, the Ith gas-liquid separator 47, gas compressor 48, filter the 49, the Ith gaseous jet simulation assembly the 50, the IIth gaseous jet simulation assembly the 51, the IIth gas-liquid separator 52 and water knockout drum 53 successively by Flow of Goods and Materials direction; Wherein, the charging aperture of the IIth gas mixer 43 is connected with evapo-separated machine 31 by the Ith vacuum pump 42; The solvent vapo(u)r outlet of evaporation process unit is connected with the charging aperture of the IIth gas mixer 43 with the IIth heat exchanger 54 via the Ith gas mixer 41. Wherein, the Ith gaseous jet simulation assembly 50 and the IIth gaseous jet simulation assembly 51 constitute secondary membrane separative element.
In certain embodiments, described solvent recovery unit also includes for making the concentration of film separation unit (the Ith gaseous jet simulation assembly 50 and the IIth gaseous jet simulation assembly 51) return the closed circuit of the IIIth condenser 46 mutually, and this closed circuit includes the IVth gas mixer the 55, the IIth vacuum pump the 56, the IIIth gas mixer 45 and the IIIth condenser 46 successively by Flow of Goods and Materials direction.
In further embodiments, described solvent recovery unit also includes for the pipeline 57 by the solvent delivery bottom the Ith gas-liquid separator 47 and the IIth gas-liquid separator 52 to water knockout drum 53.
In certain embodiments, in solvent recovery unit, described filter 49 is filled by hydrophilic filler, primarily serves the purpose of a small amount of moisture of removing and solid impurity.
In further embodiments, described film separation unit includes the gaseous jet simulation assembly (including the Ith gaseous jet simulation assembly 50 and the IIth gaseous jet simulation assembly 51 successively by Flow of Goods and Materials direction) of two series connection, the preferred rolled film device of described gaseous jet simulation assembly, membrane material is preferably polydimethylsiloxane (PDMS) film (PDMS layer thickness about 30 μm, supporting layer thickness about 100 μm), membrane area is preferably 30-40m2/ ton crude oil; It is preferred that membrane area is 34m2/ ton crude oil; Membrane permeation lateral pressure is less than 1kPa.
In the flow process of above-mentioned grease lixiviating process, the IIth gas mixer the 43, the IIth condenser the 44, the IIIth gas mixer 45 and the IIIth condenser 46 constitute the condenser system of solvent recovery unit.
In the flow process of above-mentioned grease lixiviating process, solvent recovery unit, and the circulation line (not shown) for the organic solvent that this unit reclaims is sent back to infuser 21 constitutes the solvent circulation of apparatus of the present invention.
In the flow process of above-mentioned grease lixiviating process, solvent recovery unit, and the circulation line (not shown) for the nitrogen that this unit reclaims is sent back to evapo-separated machine 31 constitutes the nitrogen circulating system of apparatus of the present invention.
According to certain specific embodiments of the invention, adopt grease lixiviating process device as shown in Figure 1 to carry out oil extraction and prepare crude oil, including procedure below:
(1) in loop type extractor 21, feed solvent and oil plant material base 1, and in atmospheric conditions, oil plant material base 1 is carried out leaching process, for instance obtained miscella and the solvent-laden oil plant dregs of rice by multi-stage counter current extraction;
The operation temperature that leaching in this process processes is 48-53 DEG C, it is preferred to 53 DEG C; Consumption for leaching the solvent of process is about 0.9-1 ton/ton oil plant material base.
Preferably, oil plant material base carried out pretreatment before process leaching processes to obtain through pretreated oil plant material base. Accordingly, when leaching processes, in loop type extractor 21, feed solvent and the oil plant material base 1 through pretreatment, and in atmospheric conditions, the oil plant material base 1 through pretreatment is carried out leaching process.
In certain embodiments, the solvent for leaching process includes fresh solvent 2 and/or recycling design 9.
(2) utilizing evaporation process unit to be evaporated miscella processing acquisition crude oil and evaporation solvent vapo(u)r, it comprises the following steps:
The miscella obtained in loop type extractor 21 is fed the Ith grade of vaporizer 23 and carries out the Ith grade of evaporation process by () employing pump 22, is obtained the Ith grade of evaporation process miscella from the bottom of the Ith grade of vaporizer 23 via the Ith heat exchanger 24 and the IIth grade of vaporizer 25 of entrance after crude oil 3 heat exchange of stripper 26; And the obtain the Ith grade of evaporation solvent vapo(u)r discharge from the Ith grade of vaporizer top laggard enter the Ith gas mixer 41.
In this step, the operation temperature of the Ith grade of evaporation process is about 52-54 DEG C. The preferably operation temperature of the Ith grade of evaporation process about 53 DEG C. Operation pressure is about 0.05-0.06MPa. Preferred operations pressure is about 0.05MPa. Oil content > 60wt% in the Ith grade of evaporation miscella obtained after process.
() utilizes the IIth grade of vaporizer 25 that the Ith grade of evaporation process miscella is carried out the IIth grade of evaporation process, is obtained the IIth grade of evaporation process miscella and enters stripper 26 from the bottom of the IIth grade of vaporizer 25; And the obtain the IIth grade of evaporation solvent vapo(u)r discharge from the IIth grade of vaporizer top laggard enter the Ith gas mixer 41.
In this step, the operation temperature of the IIth grade of evaporation process is about 115-120 DEG C. The preferably operation temperature of the IIth grade of evaporation process about 120 DEG C. The operation pressure of the IIth grade of evaporation process is about 0.05-0.06MPa. Preferably the operation pressure of the IIth grade of evaporation process is about 0.05MPa. The oil content > 95wt% of the IIth grade of evaporation process miscella obtained after process.
() is passed directly into raw steam 4 to stripper 26 tower reactor, utilize stripper 26 that the IIth grade of evaporation process miscella is carried out stripping process, the crude oil 3 obtained discharge from the bottom of stripper 26 after through by the Ith heat exchanger 24 and from separating device after lowering the temperature then through the Ith condenser 27 after the Ith grade of evaporation process miscella heat exchange bottom the Ith grade of vaporizer 23; The fixed gas at stripper 26 top enters the Ith gas mixer 41.
The operating condition of this step is: the raw steam pressure being passed directly into is 0.15-0.2MPa, it is preferred to 0.18MPa; Quantity of steam is about 0.038-0.05 ton/ton crude oil, it is preferred to 0.04 ton/ton crude oil; Tower top operation temperature is about 120-125 DEG C, it is preferred to 120 DEG C; Tower reactor operation temperature is about 123-127 DEG C, it is preferred to 125 DEG C; Operation pressure is about 0.05-0.06MPa, it is preferred to 0.05MPa.
(3) utilize the de-processing unit of steaming that the solvent-laden oil plant dregs of rice from loop type extractor 21 steam de-process, comprise the following steps;
() opens nitrogen gas generator 33 and aerator 32, air 5 is fed nitrogen gas generator 33, and the nitrogen produced by nitrogen gas generator 33 by aerator 32 feeds the precipitation oxidant layer (not shown) of evapo-separated machine 31, the intake of described nitrogen is 23-27m3The solvent-laden oil plant dregs of rice of/ton. The intake of preferred described nitrogen is 24.5m3The solvent-laden oil plant dregs of rice of/ton.
() is with 23-27m3The amount of the solvent-laden oil plant dregs of rice of/ton, it is preferable that with 24.5m3The amount of the solvent-laden oil plant dregs of rice of/ton passes into nitrogen to the precipitation layer of evapo-separated machine 31, it is 50-55 DEG C in operation temperature, when operation pressure is 0.05-0.07MPa, the solvent-laden oil plant dregs of rice from loop type extractor 21 are steamed de-process, the thick oil plant dregs of rice obtained discharge bottom evapo-separated machine 31 laggard enter cooling layer with cold air (not shown) cool down, the oil plant dregs of rice 6 after cooling input storage tank (not shown) store; The fixed gas (namely steaming desolventizing vapour mixture) at the top of evapo-separated machine 31 then enters solvent recovery unit by vacuum pump 42 and the IIth gas mixer 42.
(4) the produced desolventizing vapour mixture that steams carries out solvent recovery process with process (3) to evaporation solvent vapo(u)r produced in process (2) to utilize solvent recovery unit, including:
The solvent vapo(u)r at the Ith grade of vaporizer 23 in process (2), the IIth grade of vaporizer 25 and stripper 26 top is fed after the Ith gas mixer 41 mixing after the IIth heat exchanger 54 recovers energy with recycling design 9 heat exchange by (), enters back into the IIth gas mixer 42 steaming desolventizing vapour mixture produced with process (3) and mixes;
The mixed solvent steam that () the IIth gas mixer 43 obtains enters the IIth condenser 44 and is cooled to 35-37 DEG C, it is preferably cooled to 35 DEG C, fixed gas enters after the IIIth gas mixer 45 mixes with the concentration tail gas from gas membrane separation unit and enters the IIIth condenser 46, fixed gas in IIIth condenser 46 tail gas after the Ith gas-liquid separator 47 gassing processes is fed entrance the Ith gaseous jet simulation assembly 50 after filter 49 removes a small amount of granule foreign and moisture and carries out the Ith membrane separation by gas compressor 48, tail gas after membrane separation is again introduced into the IIth gaseous jet simulation assembly 51 and carries out the IIth membrane separation, gaseous jet simulation assembly all adopts rolled film device, membrane material is PDMS film, membrane area is needed to be about 30-40m2/ ton crude oil, it is preferred to 34m2/ ton crude oil. Membrane permeation lateral pressure is less than 1kPa. The high concentration solvent steam (i.e. concentration tail gas) that the membrane permeation side of final secondary membrane separation assembly obtains loops back the IIIth condenser 46 condense through the IIth vacuum pump 56 and the IIIth gas mixer 45 after all entering the IVth gas mixer 55 mixing; And the gas of the film retentate side of secondary membrane separation assembly is after the IIth gas-liquid separator 52 carries out gas-liquid separation, the nitrogen 7 obtained utilizes as the air stripping nitrogen circulation of evapo-separated machine 31, and the thick recycling design obtained 57 is delivered to water knockout drum 53 by the road, and in water knockout drum 53, carry out turnout reason further, isolated a small amount of organic wastewater 8 to discharge from water knockout drum 53, and the recycling design 9 obtained is recycled with entrance infuser 21 after the evaporation solvent vapo(u)r heat exchange of the Ith gas mixer 41 via the IIth heat exchanger 54.
In this step, the IIth condenser 44 in the condenser system of solvent recovery unit and the liquid phase entrance water knockout drum 53 after the Ith gas-liquid separator 47 of lime set produced by the IIIth condenser 46 carry out turnout reason, recovery organic solvent.
In aforesaid operations process, there is certain loss in solvent circulation, nitrogen circulating system, for solvent loss, adopts solvent tank feed profile to solve, and nitrogen losses adopts PSA nitrogen generator 33 to supplement a certain amount of nitrogen and solves.
Nitrogen air stripping technology is applied to the desolvation process of the solvent-laden oil plant dregs of rice by grease lixiviating process provided by the present invention, the removal process being used in fixed gas by gas membrane Seperation Technology organic solvent, thus the generation of the energy expenditure being greatly reduced in extract technology and organic wastewater, enormously simplify technique and operation simultaneously, the basis ensureing crude oil yield by controlling process conditions to achieve effectively reduces the operating cost of its production, solves those skilled in the art and thirst for solving and a unsolved difficult problem so far always. With production capacity be 1.33 ton hour Testa oryzae oil traditional Rice bran crude oil extract technology compared with, the novel extract technology of the present invention relatively traditional handicraft overall energy-saving rate reaches 45%, and is remarkably decreased in the discharge capacity of water knockout drum part organic wastewater.
Embodiment
Example 1:
(1) by Testa oryzae (RB) (7.6 ton hour after extrusion pretreatment, water content 8%, temperature 40 DEG C) 1 and solvent 2 (fresh solvent, 6# solvent) feed loop type extractor 21, under normal pressure and 53 DEG C of conditions, carry out multi-stage counter current extraction extract oils and fats, it is thus achieved that miscella and solvent-laden rice bran meal; The consumption being used for leaching the solvent of process in this process is 7.1 ton hour (namely the consumption of the solvent for leaching process is about 0.93 ton/ton oil plant material base).
(2) utilizing evaporation process unit to be evaporated miscella processing acquisition crude oil and evaporation solvent, it comprises the following steps:
The miscella (oil content is about 20wt%-25wt%) obtained in loop type extractor 21 is fed the Ith grade of vaporizer 23 and carries out the Ith grade of evaporation process by () employing pump 22, is obtained the Ith grade of evaporation process miscella from the bottom of the Ith grade of vaporizer 23 via the Ith heat exchanger 24 and the IIth grade of vaporizer 25 of entrance after the crude oil material stream heat exchange of stripper 26; And the obtain the Ith grade of evaporation solvent vapo(u)r discharge from the Ith grade of vaporizer top laggard enter the Ith gas mixer 41.
In this step, the operation temperature of the Ith grade of evaporation process about 53 DEG C, operation pressure is about 0.05MPa, the Ith grade of evaporation process miscella concentration > 60wt% of the discharging obtained after process.
() utilizes the IIth grade of vaporizer 25 that the Ith grade of evaporation process miscella is carried out the IIth grade of evaporation process, is obtained the IIth grade of evaporation process miscella and enters stripper 26 from the bottom of the IIth grade of vaporizer 25; And the obtain the IIth grade of evaporation solvent discharge from the IIth grade of vaporizer top laggard enter the Ith gas mixer 41.
In this step, the operation temperature of the IIth grade of evaporation process about 120 DEG C, operation pressure is about 0.05MPa, the IIth grade of evaporation process miscella concentration > 95wt% of discharging obtained after process.
() is passed directly into raw steam 4 to stripper 26 tower reactor, utilize stripper 26 that the IIth grade of evaporation process miscella is carried out stripping process, the finished product crude oil 3 obtained discharge from the bottom of stripper 26 after through squeezing into crude oil tank by the Ith heat exchanger 24 and from separating device after being cooled to room temperature then through the Ith condenser 27 after the Ith grade of evaporation process miscella heat exchange bottom the Ith grade of vaporizer 23;The fixed gas at stripper 26 top enters the Ith gas mixer 41.
The operating condition of this step is: the air pressure of the raw steam 4 being passed directly into, at about 0.18MPa, passes into quantity of steam and is about 0.038 ton/ton crude oil; Tower top operation temperature is about 120 DEG C, and tower reactor operation temperature is about 125 DEG C, and operation pressure is about 0.05MPa, volatile component content < 0.3% in tower reactor crude oil.
Finished product crude oil 3 enters and enters the Ith condenser 27 after the Ith heat exchanger 24 (the IIth grade of evaporation feed liquor preheater) and the Ith evaporation process miscella carry out heat exchange and be cooled to room temperature and squeeze into crude oil storage tank.
(3) utilize the de-processing unit of steaming that the solvent-laden rice bran meal from loop type extractor 21 steams de-process, comprise the following steps:
() opens nitrogen gas generator 33 and aerator 32, air 5 is fed nitrogen gas generator 33, and the nitrogen produced by nitrogen gas generator 33 by aerator 32 feeds the precipitation oxidant layer (not shown) of evapo-separated machine 31, the flow that passes into of described nitrogen is about 200m3/h。
() feeds containing solvent rice bran meal to evapo-separated machine 31 with the amount of 8.17 ton hour, and with about 200m3The flow of/h passes into nitrogen to the precipitation layer of evapo-separated machine 31, and (intake of nitrogen is 24.5m3/ ton is containing solvent rice bran meal), it it is 50 DEG C in operation temperature, when operation pressure is 0.05MPa, solvent-laden rice bran meal from loop type extractor 21 is steamed de-process, most solvent is separated with the solid bran dregs of rice, the brown shorts dregs of rice obtained discharge bottom evapo-separated machine 31 laggard enter cooling layer with cold air (not shown) cool down, the rice bran meal 6 after cooling goes storage tank (not shown); The fixed gas (steaming the gaseous mixture of desolventizing steam and nitrogen) at the top of evapo-separated machine 31 then enters solvent recovery unit via vacuum pump 41.
(4) produced steaming after desolventizing vapour mixture converges carries out solvent recovery process with process (3) to evaporation solvent vapo(u)r produced in process (2) to utilize solvent recovery unit, including:
() by the Ith grade of vaporizer 23 in process (2), the IIth grade of vaporizer 25, stripper 26 top organic vapor converge after entrance the Ith gas mixer 41 mixing after the IIth heat exchanger 54 (air preheater) and recycling design 9 heat exchange recover energy, then steam desolventizing vapour mixture produced with process (3) converges entrance the IIth gas mixer 43 and mixes;
The solvent vapo(u)r that () the IIth gas mixer 43 obtains enters the IIth condenser 44 and is cooled to 35 DEG C, fixed gas enters after the IIIth gas mixer 45 mixes with concentration tail gas (the concentration phase from film separation unit) and enters the IIIth condenser 46, fixed gas tail gas after the Ith gas-liquid separator 47 gassing processes is fed entrance the Ith gaseous jet simulation assembly 50 after filter 49 removes a small amount of granule foreign and moisture content and carries out the Ith membrane separation by gas compressor 48, tail gas after the Ith grade of membrane separation is again introduced into the IIth gaseous jet simulation assembly 51 and carries out the IIth grade of membrane separation. in this step, membrane permeation lateral pressure is less than 1kPa, and gaseous jet simulation assembly all adopts rolled film device, and membrane material is PDMS film, it is necessary to membrane area is about 34m2/ ton crude oil. The high concentration solvent steam (solvent strength > 90wt%) that the membrane permeation side of final secondary membrane separation assembly obtains loops back the IIIth condenser 46 cool down through the IIth vacuum pump 56 and the IIIth gas mixer 45 after entering the IVth gas mixer 55 mixing;The nitrogen-rich gas of the film retentate side of the IIth membrane separation assemblies is then after the IIth gas-liquid separator 52 carries out gas-liquid separation, gas phase (nitrogen 7) utilizes as the air stripping nitrogen circulation of evapo-separated machine 31, liquid phase (thick recycling design) 57 is delivered to water knockout drum 53 by the road, and in water knockout drum 53, carry out turnout reason further, isolated a small amount of organic wastewater 8 to discharge from water knockout drum 53, and the recycling design 9 obtained is recycled with entrance infuser 21 after the evaporation solvent vapo(u)r heat exchange of the Ith gas mixer 41 via the IIth heat exchanger 54.
In this step, the IIth condenser 44 in the condenser system of solvent recovery unit and the liquid phase entrance water knockout drum 53 after the Ith gas-liquid separator 47 of lime set produced by the IIIth condenser 46 carry out turnout reason, recovery organic solvent.
In aforesaid operations process, there is certain loss in solvent circulation, nitrogen circulating system, for solvent loss, adopts solvent tank feed profile to solve, and nitrogen losses adopts PSA nitrogen generator 33 to supplement a certain amount of nitrogen and solves.
In order to this technique of more specific explanation is compared to the feature of conventional grease extract technology, tradition Testa oryzae oil extract technology flow chart is listed in Fig. 2 and carries out the comparison of two kinds of techniques. Can be seen that, on the one hand, in traditional handicraft (as in figure 2 it is shown, production capacity is 1.33 ton hour), evapo-separated machine 31 is to adopt steam to carry out solvent steaming to take off, and steams and needs in de-process to consume the moisture that substantial amounts of steam is respectively used in stripping separation solvent and the heating, drying dregs of rice; And present invention process evapo-separated machine 31 is to realize solvent with nitrogen as gas stripping gas to separate, it is to avoid the steam consumption in former technique, greatly reduce the energy consumption of 31 evapo-separated machines. On the other hand, in traditional handicraft (such as Fig. 2), the tail gas that Ith gas-liquid separator 47 produces feeds absorption tower 61, absorption tower 61 reclaims the solvent in tail gas using paraffin oil as absorbing medium, and in Analytic Tower 64, strips the solvent in separating paraffin oil by high-temperature steam further; And the tail gas that the Ith gas-liquid separator 47 is produced by present invention process feeds gaseous jet simulation assembly 50 and 51, the separation and recovery of solvent in tail gas is realized, thus reducing the energy consumption of vent gas treatment process when not using absorbing medium (such as paraffin oil), not consuming extra steam. It addition, present invention process is substantially simple than traditional handicraft, easy and simple to handle, and it have been experienced that, present invention process compares traditional handicraft, and steam saving amount, up to 63wt%, saves cooling water inflow up to 26wt%, and overall energy consumption saving rate is up to 45%. Compared to traditional handicraft, present invention process achieves in the operating cost ensureing effectively to reduce on the basis of crude oil yield its production.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment of making, equivalent replace or improvement etc. within the spirit and principles in the present invention, should be included within protection scope of the present invention.
Claims (10)
1. a grease lixiviating process, comprising:
Process A, carries out leaching process to oil plant material base in the presence of solvent, it is thus achieved that miscella and the solvent-laden oil plant dregs of rice;
Process B, is evaporated miscella processing, it is thus achieved that crude oil and evaporation solvent vapo(u)r;
The solvent-laden oil plant dregs of rice are steamed de-process by process C, it is thus achieved that the thick oil plant dregs of rice and steaming desolventizing vapour mixture;
Wherein, the de-process of described steaming is undertaken by passing into nitrogen to precipitation layer.
2. technique according to claim 1, it is characterised in that the intake of described nitrogen is 23-27m3The solvent-laden oil plant dregs of rice of/ton; Preferred described steaming takes off the operation temperature of process and is 50-55 DEG C; It is 0.05-0.07MPa that preferred described steaming takes off the operation pressure of process.
3. technique according to claim 1 and 2, it is characterized in that, also include the process D of solvent recovery: produced steaming carries out condensation process, gas-liquid separation process and gaseous jet simulation after desolventizing vapour mixture converges and process with process C by evaporation solvent vapo(u)r produced in process B, it is thus achieved that recycling design and reclaim nitrogen and be circulated utilization respectively.
4. the technique according to any one in claim 1-3, it is characterised in that in process B, is evaporated process and includes miscella is sequentially carried out the Ith grade of evaporation process, the IIth grade of evaporation process and stripping process miscella.
5. an oil extraction device, it includes loop type extractor and the evaporation process unit being connected with loop type extractor respectively and steams de-processing unit, and the de-processing unit of wherein said steaming includes the evapo-separated machine being connected with loop type extractor and the nitrogen gas generator from nitrogen to evapo-separated machine and the aerator that feed.
6. device according to claim 5, it is characterized in that, described device also includes solvent recovery unit, it includes the IIth gas mixer, the IIth condenser, the IIIth gas mixer, the IIIth condenser, the Ith gas-liquid separator, gas compressor, filter, film separation unit, the IIth vapour liquid separator and water knockout drum successively by Flow of Goods and Materials direction, wherein, the charging aperture of the IIth gas mixer is connected with evapo-separated machine top by the Ith vacuum pump; The solvent vapo(u)r outlet of evaporation process unit is connected via the charging aperture of the Ith gas mixer and the IIth heat exchanger and the IIth gas mixer.
7. device according to claim 6, it is characterized in that, described solvent recovery unit also includes for making the concentration of the membrane separation assemblies in film separation unit return the closed circuit of the IIIth condenser mutually, and described closed circuit includes the IVth gas mixer, the IIth vacuum pump, the IIIth gas mixer and the IIIth condenser successively by Flow of Goods and Materials direction.
8. device according to claim 6, it is characterised in that described solvent recovery unit also includes the pipeline for the solvent delivery the Ith gas-liquid separator and the IIth gas-liquid separator separates obtained to water knockout drum.
9. the device according to any one in claim 6-8, it is characterised in that described film separation unit includes at least one gaseous jet simulation assembly; Preferred described film separation unit includes the gaseous jet simulation assembly of more than two series connection; Preferred described gaseous jet simulation assembly is rolled film device; Preferred membrane material is PDMS film; Preferred membrane area is 30-40m2/ ton crude oil; Preferred membrane permeation lateral pressure is less than 1kPa.
10. the device in claim 5-9 as described in any one prepares the application in crude oil at oil extraction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108539093A (en) * | 2017-03-03 | 2018-09-14 | 住友化学株式会社 | film manufacturing device and film manufacturing method |
| CN111471519A (en) * | 2020-05-14 | 2020-07-31 | 赵汇川 | Device and method for extracting cashew nut shell oil |
| CN113698985A (en) * | 2021-08-27 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Process for removing residual solvent in production process of crude corn oil |
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| CN103614236A (en) * | 2013-12-12 | 2014-03-05 | 酉阳县康友粮油有限公司 | Oil extracting process |
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| CN1090597A (en) * | 1993-02-01 | 1994-08-10 | 食品科学公司 | From cereal materials and cereals base food, leach the equipment and the method for oil |
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| CN108539093A (en) * | 2017-03-03 | 2018-09-14 | 住友化学株式会社 | film manufacturing device and film manufacturing method |
| CN108539093B (en) * | 2017-03-03 | 2022-04-22 | 住友化学株式会社 | Film manufacturing apparatus and film manufacturing method |
| CN111471519A (en) * | 2020-05-14 | 2020-07-31 | 赵汇川 | Device and method for extracting cashew nut shell oil |
| CN113698985A (en) * | 2021-08-27 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Process for removing residual solvent in production process of crude corn oil |
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