CN110205168A - The formula and preparation process and method for concentration of a kind of dimethyl ether new energy - Google Patents

Abstract

The present invention relates to the formulas and manufacture craft of a kind of dimethyl ether new energy, it include dimethyl ether production removing process, washing process technique and dehydration three parts in manufacture craft, finally obtain dimethyl ether new energy, it can be used for refining fuel, total oxide content can be lower than 100mg/kg, and wherein methanol content is lower than 30 mg/kg.Again because processing step is simple, efficient, cost is relatively low, is conducive to promotion and application.

Description

The formula and preparation process and method for concentration of a kind of dimethyl ether new energy

Technical field

The present invention relates to the technical field of new energy, the formula and its preparation work of specifically a kind of dimethyl ether new energy Skill and method for concentration, more particularly to a kind of alkene preparing dimethy ether formula and its preparation process and method for concentration.

Background technique

It is huge that China's oil resource wretched insufficiency relies on import volume.Although using coal based synthetic gas as synthetic oil, liquefaction Technology is mature, but coal brings negative effect to cause Heavy environmental pollution and at low cost as fossil fuel, but by pollution sources Without saving grace.Reaction production polymethoxy dimethyl ether produced by petrochemical industry conversion oxide alkene and methanol-to-olefins refines skill Art is the novel environment friendly fuel that reduction energy consumption generally acknowledged in the world reduces flue gas emission.Cetane number is up to (80-100CN) low temperature Good fluidity, can improve gasoline and many problems of diesel combustion bring, most important reduction motor vehicle exhaust emission, which is used in It does not need to be transformed using to vehicle engine system on automobile.Show that polymethoxy dimethyl ether exists by test and application study It burns in automobile, carbon dioxide in flue gas discharge amount can reduce 80-90%, and 50-70%, while thermal efficiency ratio bavin can drop in Nox compound Oil and gasoline distinguish high 10-20%, are the new energies highly applied and promoted.

In the prior art, also there are various trials for the preparation of such new energy, for example report the Chinese Academy of Sciences in CN1923770A Shanxi coalification institute methanol by one-step method produces hydrocarbon products technique, which is vaporized after material benzenemethanol gas is concentrated 3-5 times, HC fuel is converted on zeolite molecular sieve catalyst.It is intermediate product synthesis technology due to thermodynamic (al) limit based on methanol Preparing synthetic gas methanol conversion per pass is 75%, therefore unreacted synthesis gas needs systemic circulation ratio to be back to methanol synthesis reaction Device, the technical application that compressor apparatus investment and operation energy dimethyl ether enriched fuel is significantly greatly increased fail industry since cost is excessively high Change application.Dimethyl ether directly is converted through methanol, intermediate product is methyl ether, is generated without methanol: as patent CN01940934A is developed One-step method from syngas preparing dimethy ether effective catalyst, is being MTG by the product of intermediate of methanol, which is H2/Co molar ratio breaks thermodynamics limitation after requiring 2:1 to 3:1 to increase concentration number.These technologies are in production, it is desirable that high, work Skill is complicated, so that cost increase, therefore unstable product quality is badly in need of wanting a kind of work for making dimethyl ether new energy in the market Process.

Summary of the invention

The purpose of the present invention is to provide a kind of formula of improved dimethyl ether new energy and its preparation process and concentration sides Method, it can overcome the shortcomings of that complex process, conversion ratio are low and at high cost in the prior art.

To achieve the goals above, the technical scheme is that a kind of formula of highly enriched dimethyl ether new energy, special Sign is: formula includes the following ingredient of weight percent: the dimethyl ether of 70-85%, the stearic acid of 8-12%, 5-8% alkyl Violent, 1-2.5% the rare earth lanthanum oxide of three oxidation two of acid, 1-2.5%, the sum of weight percent of above-mentioned each ingredient is 100%.

The method for preparing dimethyl ether is as follows: a, carrying out dimethyl ether production removing process to raw material first, passes through in removing section Water washing and rectification obtains primary purification olefin stream；B, washing process is carried out, the primary purification olefin stream that previous step is obtained It is washed in washing section by continuous flow upstream, so that removing the organic oxide of azeotropic and remaining in the olefin stream object of primary purification Micro dimethyl ether obtains dimethyl ether and remains product, and gas phase purified olefins logistics, washing section bottom are thus obtained at the top of washing section Obtain washing olefin feed washing water；C, it is carried out dehydrating, the gas phase purified olefins logistics that previous step obtains successively passes through, mistake Condenser and moisture return tank obtain dewatered refining dimethyl ether, and the total oxide content in refining dimethyl ether can be lower than 100mg/kg, wherein methanol content is lower than 30 mg/kg.

Preferably, in a step, removing the reaction kettle in section includes main body and tower reactor reboiler, and main body includes upper, middle and lower Three structures, thick olefin feedstock is from the top feed of substructure, and extraction distillation solvent is from the top feed of central structure, upper Primary purification olefin stream is obtained at the top of portion's structure.

In b step, the water flow temperature of the continuous flow upstream washing of washing section is just flowed into optionally greater than primary purification olefin stream The mass flow ratio of temperature when washing section, adverse current flowing water and primary purification olefin stream is 0.15-2.

Further, in dimethyl ether removing section and washing section, operation absolute pressure can be 1.1-3.5mpa, preferably 1.3- 3.0 mpa, operation temperature be 31-198 DEG C, preferably 38-165 DEG C, reflux ratio 0.3-2.5, preferably 0.5-1.9.

A kind of method for concentration for the refining dimethyl ether that the preparation method of dimethyl ether formula of new energy obtains, it is characterised in that: Steps are as follows: a, refining dimethyl ether be put into supercentrifuge be carried out dehydrating, by high speed 3-5 times repeatedly dehydration so that Dehydration rate reaches 50-60%, and dewatered refining dimethyl ether is put into water-washing cleaning cartridge, is washed repeatedly, obtains concentration and is The dimethyl ether of 25-35%；B, dimethyl ether enters in slurries combination apparatus after the completion of washing, and hexamethylene diamine, alkylamine, thickener is added, with Centrifuge is carried out after slurries chemical combination to be dehydrated 2-3 times；C, the dimethyl ether obtained in b step, which enters in thickener, carries out thickening processing work Then skill carries out being dehydrated air-dried processing, the final high concentration dimethyl ether fuel for obtaining 5 times -10 times or more, wherein organic matter etc. is miscellaneous Matter content is less than or equal to 0.2%, 0.03% or less content after gaseous impurity purification gas.

Compared with the existing technology, technical solution of the present invention further includes many details in addition to the improvement of overall technical architecture The improvement of aspect, specifically, having the advantages that

1, improvement project of the present invention provides a kind of production technology for making dimethyl ether, including dimethyl ether production removing Technique, washing process technique and dehydration three parts, product total oxide content obtained can be lower than 100mg/kg, wherein first Alcohol content is lower than 30 mg/kg, so that the product can be used for dimethyl ether purification fuel, it is also possible to make dimethyl ether dehydrogenated hydrocarbon or light The macromolecular variation of the raw material hydrocarbon of the cracker of hydrocarbon does not influence to convert under the conditions of oxygen-containing, and by-product is the propane object of 1-1.5% Stream material；

2, in technical solution of the present invention, processing step is reasonable, makes full use of the product of each section, therefore high conversion rate, section The about cost of raw material；

3, invention enhances the concentrations of dimethyl ether thickens and air-dries processing by being further dehydrated, pass through above-mentioned step Suddenly highly enriched dimethyl ether stream product is completed, cycles of concentration reaches 5-10 times and refines rank up to solid when being concentrated；

4, the present invention is for simple production process, and product quality is high, high production efficiency, easy to spread and application.

Specific embodiment

Technical solution of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.

The present invention provides a kind of formula of highly enriched dimethyl ether new energy, difference with the prior art is: formula Include the following ingredient of weight percent: the dimethyl ether of 70-85%, the stearic acid of 8-12%, the alkyl acid of 5-8%, 1-2.5% three Two violent, 1-2.5% rare earth lanthanum oxides are aoxidized, the sum of weight percent of above-mentioned each ingredient is 100%.

In one embodiment, formula includes the following ingredient of weight percent: 80% dimethyl ether, 10% stearic acid, 6% alkyl acid, 2% three oxidations are two violent, 2% rare earth lanthanum oxide, the sum of weight percent of above-mentioned each ingredient is 100%.

The preparation method of a kind of dimethyl ether formula of new energy of the present invention, it is characterised in that: prepare the side of dimethyl ether Method is as follows: a, carrying out dimethyl ether production removing process to raw material first, passes through water washing and rectification in removing section and obtain primary purification alkene Hydrocarbon stream；B, washing process is carried out, the primary purification olefin stream that previous step is obtained passes through continuous flow upstream water in washing section It washes, so that the organic oxide of removing azeotropic and remaining micro dimethyl ether obtain more than dimethyl ether in the olefin stream object of primary purification Product is stayed, gas phase purified olefins logistics is thus obtained at the top of washing section, washing section bottom obtains washing olefin feed washing water； C, it is carried out dehydrating, the gas phase purified olefins logistics that previous step obtains successively passes through, and crosses condenser and moisture return tank, obtains Dewatered refining dimethyl ether, the total oxide content in refining dimethyl ether can be lower than 100mg/kg, and wherein methanol content is lower than 30 mg/kg.Here logistics refers to mixed material, and mixed material here includes fixed, liquids and gases mixtures.

Further, in a step, removing the reaction kettle in section includes main body and tower reactor reboiler, and main body includes upper, middle and lower Three structures, thick olefin feedstock is from the top feed of substructure, and extraction distillation solvent is from the top feed of central structure, upper Primary purification olefin stream is obtained at the top of portion's structure.

In a step, mass content >=85% of organic oxygen-containing compound in extraction distillation solvent, organic oxygen-containing here It closes object and is selected from one of methanol, ethyl alcohol, isopropanol, acetone or a variety of mixtures, organic oxygen-containing compound in extractant stream Mass flow ratio with raw material is 0.5-8.

In b step, the water flow temperature of the continuous flow upstream washing of washing section is just flowed into optionally greater than primary purification olefin stream The mass flow ratio of temperature when washing section, adverse current flowing water and primary purification olefin stream is 0.15-2.

In above-mentioned dimethyl ether removing section and washing section, operation absolute pressure can be 1.1-3.5mpa, preferably 1.3-3.0 Mpa, operation temperature be 31-198 DEG C, preferably 38-165 DEG C, reflux ratio 0.3-2.5, preferably 0.5-1.9.

Specifically, the present invention discloses the dimethyl ether of a kind of propane, acetone, methanol from comprising alkene in feed stream Refining dimethyl ether material is produced, the washed aqueous solution of organic oxide in dimethyl ether and solvent are carried out rectifying extraction by work in-process Including organic oxides such as alkene loaded article, propane, acetone, methanol in alkene organic oxide.It washed, separated, only Change, dehydration etc. carries out processing in kettle after techniques, obtain refining dimethyl ether reaction combustion with techniques such as purifying, gasification, catalyst conversions Expect, between the impurity contents such as organic matter 0.-0.2%, 0.03% or less content ensures that dimethyl ether refines after gaseous impurity purification gas Fuel purity simultaneously obtains the high concentration dimethyl ether fuel with 5 times -10 times or more under the conditions of high concentration concentration, through test test two Above is applicable to refine the application of fuel in 70-75% for methyl ether recovery ratio.

In the preparation method embodiment of a specific dimethyl ether formula of new energy, include the following steps: the technique Including dimethyl ether production removing process, washing process technique and dehydration three parts.

The dimethyl ether removing processing completes dimethyl ether removing section in the dimethyl ether removing stage and is divided into upper part, middle part With lower part, include the following steps.Top feed of the raw material including alkene and dimethyl ether from lower part, extraction, distillation solvent object The top feed of part in stream, reflux purified olefins logistics are obtained through extracting rectifying at the top of upper part from the top feed on top To primary purification olefin stream, lower section bottom obtains the material comprising dimethyl ether and extraction distillation solvent, material a part It is recycled through tower reactor reboiler, rest part is sent to next section, i.e., feeding alkylene oxide olefin hydrocarbon apparatus, which is used as, reacted Journey raw material.

It completes, includes the following steps in the washing process section.Primary purification olefin stream from washing section bottom feed, water Stream section top feed obtains gas phase purified olefins logistics through continuous flow upstream washing at the top of washing section, and washing section bottom is washed Wash olefin feed washing water.

The dehydration is completed in moisture return tank, is included the following steps.Gas phase purified olefins logistics passes sequentially through The return tank of top of tower, condenser and water, purified olefins logistics after being dehydrated after being dehydrated pass through reflux alkene booster pump After pressurization, it is partly refluxed to the top of part in dimethyl ether removing section, remaining divides water to return as the extraction of purified olefins new product stream Flow pot bottom discharge.

It is wherein at least combined with dimethyl ether removing section and washing section according to the present invention, according to the operation mode, in dimethyl ether It removes section and passes through the effect of the water washing and rectification of organic oxide or its aqueous solution, the separation of removing moisture content and dimethyl ether material.Thus Dimethyl ether removing section bottom obtains the logistics comprising dimethyl ether and organic oxide, is washed by continuous flow upstream from first in washing section The organic oxide and remaining micro dimethyl ether that azeotropic is removed in the olefin stream object of one-step refining obtain dimethyl ether and remain product, Thoroughly the diformazan ether product in removing raw material, preferably purification institute's feed stream, after thus being refined at the top of washing section Gas phase dimethyl ether logistics product, to prevent primary purification dimethyl ether logistics from condensing in washing section, the water flow temperature for washing Preferably less than primary purification olefin stream water is not able to guarantee that technique is completed using the technique into Duan Wendu is washed.

It leaves in the logistics of the gas-phase olefin at the top of washing section containing the water vapour at balance with liquid water through top of tower After condensation, free water is precipitated, divides the method for removing the part water in water return tank that can directly adopt gravitational settling or by poly- Knot device is dehydrated.

To reduce the content of organics in primary purification olefin stream as possible, to reduce the water flow dosage extraction for washing The feed entrance point of distillation solvent is taken to be located at the 3-5 block theoretical plate of dimethyl ether removing section.

According to technique of the present invention can be used single column operated wherein washing section be located at dimethyl ether removing section above.Institute The washing water logistics stated directly flow to dimethyl ether from washing section bottom and take off section upper top.

Or liquid bath and riser: the primary purification alkene object are set between the dimethyl ether removing section and washing section Stream enters riser by riser and enters washing bottom, and water flow and primary purification olefin stream carry out continuous inverse in washing section Flowing water is washed, the washing water logistics that washing section bottom obtains outer top for draining into part in dimethyl ether removing section after being collected by hydrops slot Portion.

In the preparation method embodiment of another dimethyl ether formula of new energy, due to the separation mass-transfer efficiency of extracting rectifying Turn low and to reach required separating effect.The present invention needs certain theoretical plate block number.This means that knockout tower needs are higher Packed height or the actual number of plates, built for safety and equipment in industrial application and easy for installation need to reduce knockout tower Highly, double tower operation can be used in the present invention at this time.

Wherein dimethyl ether removing section is arranged in the second tower, what water flow was arranged in that washing section bottom in the first tower obtains washes It washs water logistics and is able to outlet.

Wherein the lower part of dimethyl ether removing section and middle part are set up separately and set in the second tower, dimethyl ether removes the upper part of section It is arranged in the first tower with washing section, washing section is located at the top on dimethyl ether removing section top, and de- in washing section and dimethyl ether Except hydrops slot and riser is set between section top, wherein leaving the primary purification olefinic fuel of atop part in dimethyl ether removing section Logistics enters the bottom of washing section by riser, the washing water logistics outlet that washing section bottom is collected by hydrops slot, and It is added in the middle part of the second tower dimethyl ether removing section after liquid phase olefin logistics liquid phase booster pump pressurization between section between one tower tower reactor section The top divided.The washing water flow object is mixed with the water flow of removing to be discharged as outlet water logistics.Here double water tower structures It is the prior art, does not just repeat no more its specific structure and principle here.

The extraction distillation solvent logistics is organic oxygen-containing compound, and logistics or its aqueous solution logistics, extracting rectifying are molten Organic oxygen-containing compound in agent logistics is selected from one of methanol, ethyl alcohol, isopropanol, acetone or a variety of mixtures, preferably The organic oxygen-containing compound is methanol or acetone, the application in the form of organic oxygen-containing compound aqueous solution.The aqueous solution has Mass content >=85% of machine oxygenatedchemicals, preferably at least 93%.The aqueous solution logistics of the organic oxygen-containing compound can pass through Aqueous solution logistics is mixed to get in organic oxygen-containing compound, logistics and part or all of outlet washing water logistics.

The outlet washing water stream portions enter dimethyl ether after all mixing with extraction distillation solvent logistics and remove section The top of middle part or the washing water stream portions all take off after solvent stream mixes into dimethyl ether with extraction smart flow Enter dimethyl ether after partly or entirely mixing with distillation solvent logistics except the water flow at the top of part in section, or removing and removes section The top of the part at middle part becomes refining dimethyl ether.

The feed stream comprising oxygen organic and dimethyl ether does not require olefin(e) centent substantially, and wherein May include the diformazan ether content of relatively wide range, i.e., the method for the present invention to the diformazan ether content adaptability of feed stream very By force, such as: the mass fraction of the dimethyl ether in the feed stream of the content comprising each species of oxygen organic and dimethyl ether is 1-60% is preferably 2-45%.

Feed stream in principle including oxygen organic and dimethyl ether can come from any suitable oxygenate conversion Process, as long as wherein olefin-containing and dimethyl ether can be generated in reaction effluent segmentation subtractive process so as to pass through diformazan Ether removes the related logistics being further processed.Such as the feed stream comprising alkene and dimethyl ether can come from oxygen-containing chemical combination Object olefin hydrocarbon may also contain other components, such as carbon in the case in addition to alkene and dimethyl ether in the feed stream Four component of three components, propylene component and carbon etc..

It, can be according in the determination of this field routine operation and each lever piece of selection according to the present invention during whole operation Operating pressure, operation temperature and reflux ratio are general, remove in section and washing section in the dimethyl ether, and operation absolute pressure can be 1.1-3.5mpa, preferably 1.3-3.0mpa, operation temperature is 31-198 DEG C, preferably 38-165 DEG C, reflux ratio 0.3-2.5, excellent Select 0.5-1.9.In preferred operating pressure and operating temperature range, overhead condenser can use cooling water as cold source.Tower Reboiler can be by using low-pressure steam as heat source, so as to optimize the public work grade of operating system in kettle.

The number of theoretical plate of the dimethyl ether removing section is 10-26 block, and excellent is 12-20 block theoretical tray: the washing section Theoretical cam curve is the preferred 3-4 theoretical tray of 2-6 block.

The mass flow of organic oxygen-containing compound and the feed stream for including alkene and dimethyl ether in the extractant stream Than being preferably 0.7-6 for 0.5-8: the flowing water and the mass flow ratio of olefin-containing and the raw material of dimethyl ether are preferably for 0.15-2 0.25-1。

In view of the dimethyl ether of removing can continue on for conversion process of oxocompound, organic oxygen-containing compound or its is water-soluble Liquid can be conversion process of oxocompound raw material.To make extraction distillation solvent be easier to obtain, and it is obtained in this way Solution comprising dimethyl ether and organic oxygen-containing compound can directly return to conversion process of oxocompound, and the reaction was continued, so as to Significantly to save operating cost, the higher feed stock conversion of conversion process of oxocompound may be implemented.

In a laboratory experiment result, by the thick alkene of raw material, that is, petrochemical industry alkene, propane, acetone and methanol etc. are organic Oxide, after being separated by liquid cleaner, the thick alkene of 15.6g, oxidation of organic compounds, hard is added in laboratory in 180ml reaction kettle Resin acid 1.5g, alkyl acid 1g carry out catalysis reaction, and loaded article is methanol 10g, while adding catalyst rare earth lanthanum oxide, thickener three It aoxidizes two violent 0.5g to replace under conditions of 1.0mpa in kettle air 3 times, so that residual air capacity in kettle is lower than 0.1%, boost again To 2.0mpa, quiet 30min is leaked hunting for reaction kettle after ensuring that device is air tight, empties gas reactor, carries out heating heating reaction 80-100 DEG C 500 revs/min of mixing speed, reaction pressure 1.0mpa, reaction time 2h, reaction result thickens 5 times or more dimethyl ether Obtain dimethyl ether material: 13.2g.

In another experimental result, by the thick alkene of raw material, that is, petrochemical industry alkene, the organic oxidations such as propane, acetone and methanol Object, 15.6 thick alkene organic oxidation materials are added in laboratory in 180ml reaction kettle after being separated by liquid cleaner, add simultaneously 1.5g stearic acid < thickener > alkyl acid 1g carries out catalysis reaction, and loaded article is methanol 10g, while the oxidation of thickener three two is violent 0.5g, replacing under conditions of 1.0mpa makes for air 3 times organic oxide that purification reaction gas purifying organic gas be discharged in kettle, Residual air capacity boosts to 2.0mpa again lower than 0.1% and stands 30min, and leaking hunting for reaction kettle ensures the air tight heel row of device 80-100 DEG C 500 revs/min of mixing speed of reaction of empty gas reactor heating heating, reaction pressurization 1.0Mpa reaction time 2h, reaction 7 times of thickening or more, which obtains dimethyl ether material 14.1g reaction while adding rare earth catalyst lanthana 2g, does not participate in reaction.

The method for concentration for the refining dimethyl ether that a kind of preparation method of dimethyl ether formula of new energy of the invention obtains, it is special Sign is: steps are as follows: a, refining dimethyl ether being put into supercentrifuge is carried out dehydrating, by high speed 3-5 times repeatedly So that dehydration rate reaches 50-60%, dewatered refining dimethyl ether is put into water-washing cleaning cartridge, is washed repeatedly, obtained for dehydration Concentration is the dimethyl ether of 25-35%；B, dimethyl ether enters in slurries combination apparatus after the completion of washing, and hexamethylene diamine, alkylamine, increasing is added It thick dose, is dehydrated 2-3 times with carrying out centrifuge after slurries chemical combination；C, the dimethyl ether obtained in b step, which enters in thickener, to be increased Then thick treatment process carries out being dehydrated air-dried processing, the final high concentration dimethyl ether fuel for obtaining 5 times -10 times or more, wherein having The impurity contents such as machine object are less than or equal to 0.2%, 0.03% or less content after gaseous impurity purification gas.

Dimethyl ether thickening in the case of carry out being dehydrated air-dried processing, use porous air-dry machine simultaneously with 50-70 DEG C of temperature into Row air-dries processing, and three oxidation two of addition is violent and rare earth lanthanum oxide does catalysis speed-raising, and the molding concentration time herein is 20- 40min。

In one embodiment, since the present invention has purification petrifaction ethylene, propylene, the olefin feedstock production new energy of dimethyl ether Source acts on us for more preferable performance dimethyl ether fuel and develops a kind of highly enriched dimethyl ether process, complete by following steps At highly enriched dimethyl ether stream product, cycles of concentration reaches 5-10 times and refines rank up to solid when being concentrated.Tower reactor reboiler into It (can be produced by conveying dedicated pipeline by refining dimethyl ether after number of theoretical plate Optimization Theory number when entering latter end technique Line) be sent into supercentrifuge be dehydrated standard centrifuge, dehydration rate inversion set cooperation under carry out the dehydration of dimethyl ether purified product, High speed takes off 3-5 dehydration rate 50-60% repeatedly, and residue has oxygen compound to go successively to reboiler progress circular flow to guarantee into This.Dewatered refining dimethyl ether enters liquid cleaner under the anti-static precautions of force (forcing) pump, is purifying liquid dimethyl ether Device repeatedly water purification or washing 30min.

Starch that enter slurries combination apparatus (dedicated from slurrying there are about the dimethyl ether of 30% concentration after the completion of the technique of water-washing cleaning cartridge Liquefy clutch) hexamethylene diamine 1g, stearic acid 1.5g, alkyl acid 1g is added to carry out 2-3 operation of centrifuge dehydration after slurries chemical combination Time 20-40min or so is rear to carry out thickening treatment process into thickener.

Thickener is quickly stirred 500-1000 revs/min of bracelet per minute by fire resisting electric furnace at a warm condition, is being thickened Dehydration is carried out under machine effect and 5-7 times of cycles of concentration of decolorization dimethyl ether or more and is lost flowability, and the processing time is according to object Material water content and dimethyl ether content of organics be measured total concentration amount carry out thickening processing time be less than or equal to 60mim.

The air-dried processing of second dehydration is carried out in dimethyl ether thickening uses porous air-dry machine simultaneously to protect 50-70 DEG C Shi Jinhang air-dries three oxidation two of processing addition suddenly and rare earth lanthanum oxide does catalysis speed-raising and molding concentration 20-40min or so It completes.Simultaneously be equipped with air compressor carry out dehydration and drying processing so that dimethyl ether further solidify and is concentrated and meanwhile make material divide It dissipates.

It is high that secondary treatment that is highly enriched while carrying out surplus material carries out reverse osmosis equipment processing to remaining waste water when necessary Concentration dimethyl ether can pack after air-drying processing, and material reprocess and is repeated several times until residue after waste water is handled Without dimethyl ether raw material for extremely in material.Containing organic compound during processing can processing waste water in distress generate, so Have to enter into electrolytic cell carry out electrolysis processing repeatedly 3-5 times can qualified discharge.Used various equipment are existing in the present invention Have technology, nor the present invention needs project to be protected, therefore, for above equipment repeat no more its specific working principle and Structure.

The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that Present invention specific implementation is confined to these above-mentioned explanations.For those of ordinary skill in the art to which the present invention belongs, Without departing from the inventive concept of the premise, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to the present invention Protection scope.

Claims (9)

1. a kind of formula of highly enriched dimethyl ether new energy, it is characterised in that: the formula ingredient following comprising weight percent: The dimethyl ether of 70-85%, the stearic acid of 8-12%, the alkyl acid of 5-8%, 1-2.5% violent, 1-2.5% the rare-earth oxidations of three oxidation two Lanthanum, the sum of weight percent of above-mentioned each ingredient are 100%.

2. a kind of highly enriched dimethyl ether formula of new energy according to claim 1, it is characterised in that: formula includes weight hundred Point than following ingredient: 80% dimethyl ether, 10% stearic acid, 6% alkyl acid, 2% three oxidations are two violent, 2% rare-earth oxidation Lanthanum, the sum of weight percent of above-mentioned each ingredient are 100%.

3. a kind of preparation method of dimethyl ether formula of new energy according to claim 1, it is characterised in that: prepare dimethyl ether Method it is as follows: a, dimethyl ether carried out to raw material first produce removing process, obtained in removing section by water washing and rectification preliminary smart Olefin stream processed；B, washing process is carried out, the primary purification olefin stream that previous step is obtained passes through continuous inverse in washing section Flowing water is washed, so that the organic oxide of removing azeotropic and remaining micro dimethyl ether obtain diformazan in the olefin stream object of primary purification Ether remains product, and gas phase purified olefins logistics is thus obtained at the top of washing section, and washing section bottom obtains washing olefin feed and washes Wash water；C, it is carried out dehydrating, the gas phase purified olefins logistics that previous step obtains successively passes through, and crosses condenser and moisture reflux Tank obtains dewatered refining dimethyl ether, and the total oxide content in refining dimethyl ether can be lower than 100mg/kg, and wherein methanol contains Amount is lower than 30 mg/kg.

4. a kind of preparation method of dimethyl ether formula of new energy according to claim 3, it is characterised in that: in a step, take off Except the reaction kettle in section includes main body and tower reactor reboiler, main body includes the structure of upper, middle and lower three, and thick olefin feedstock is from lower part The top feed of structure, extraction distillation solvent obtain primary purification from the top feed of central structure at the top of superstructure Olefin stream.

5. a kind of preparation method of dimethyl ether formula of new energy according to claim 4, it is characterised in that: in a step, extraction Take mass content >=85% of organic oxygen-containing compound in distillation solvent, organic oxygen-containing compound here be selected from methanol, ethyl alcohol, One of isopropanol, acetone or a variety of mixtures, the mass flow ratio of organic oxygen-containing compound and raw material in extractant stream For 0.5-8.

6. a kind of preparation method of dimethyl ether formula of new energy according to claim 3, it is characterised in that: in b step, water The water flow temperature of the continuous flow upstream washing of section is washed optionally greater than the temperature at the beginning of primary purification olefin stream when inflow washing section, adverse current The mass flow ratio of flowing water and primary purification olefin stream is 0.15-2.

7. a kind of preparation method of dimethyl ether formula of new energy according to claim 4, it is characterised in that: dimethyl ether removing In section and washing section, operation absolute pressure can be 1.1-3.5mpa, and preferably 1.3-3.0 mpa, operation temperature is 31-198 DEG C, It is preferred that 38-165 DEG C, reflux ratio 0.3-2.5, preferably 0.5-1.9.

8. the concentration for the refining dimethyl ether that a kind of preparation method of dimethyl ether formula of new energy according to claim 3 obtains Method, it is characterised in that: steps are as follows: it a, refining dimethyl ether is put into supercentrifuge is carried out dehydrating, by repeatedly So that dehydration rate reaches 50-60%, dewatered refining dimethyl ether is put into water-washing cleaning cartridge for high speed 3-5 times dehydration, is carried out repeatedly Washing obtains the dimethyl ether that concentration is 25-35%；B, dimethyl ether enters in slurries combination apparatus after the completion of washing, addition hexamethylene diamine, Alkylamine, thickener are dehydrated 2-3 times with carrying out centrifuge after slurries chemical combination；C, the dimethyl ether obtained in b step enters thickener In carry out thickening treatment process, then carry out being dehydrated air-dried processing, the final high concentration dimethyl ether combustion for obtaining 5 times -10 times or more Material, wherein the impurity contents such as organic matter are less than or equal to 0.2%, 0.03% or less content after gaseous impurity purification gas.

9. the concentration for the refining dimethyl ether that a kind of preparation method of dimethyl ether formula of new energy according to claim 8 obtains Method, it is characterised in that: carry out being dehydrated air-dried processing in the case of dimethyl ether thickening, use porous air-dry machine simultaneously with 50-70 DEG C Temperature carry out air-drying processing, and add that three oxidations two are violent and rare earth lanthanum oxide does catalysis and raises speed, molding concentration herein Time is 20-40min.