CN103709016B - A kind of pervaporation method refines technique and the device of glycol dimethyl ether - Google Patents
A kind of pervaporation method refines technique and the device of glycol dimethyl ether Download PDFInfo
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- CN103709016B CN103709016B CN201310714949.3A CN201310714949A CN103709016B CN 103709016 B CN103709016 B CN 103709016B CN 201310714949 A CN201310714949 A CN 201310714949A CN 103709016 B CN103709016 B CN 103709016B
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- dimethyl ether
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
Abstract
The present invention relates to the technique that a kind of pervaporation method refines glycol dimethyl ether, step is as follows: Williamson synthesizing glycol dme mother liquor obtains glycol dimethyl ether crude product after Neutralization settlement, thick glycol dimethyl ether is separated through rectifying tower, the azeotrope of glycol dimethyl ether-water is discharged by tower top and be collected in tundish after condensation, part water and ethylene glycol monomethyl ether are discharged by the bottom of tower, be collected in the azeotrope of the glycol dimethyl ether-water of tundish by being delivered to preheater, enter vaporizer again, the moisture glycol dimethyl ether steamed from vaporizer enters Pervaporation membrane separator, infiltration material by penetrating fluid condenser condenses laggard enter penetrating fluid tank, penetrating fluid returns further to rectifying tower and recycles, Pervaporation membrane separator retains side and obtains high purity glycol dimethyl ether, after preheater and finished product condenser condenses, products pot is entered after elder generation.Present invention process process is simple, and facility investment is few, and capacity usage ratio is high, and the rate of recovery is high.
Description
Technical field
The present invention relates to technique and device that a kind of pervaporation method refines glycol dimethyl ether, particularly relate to technique and device that a kind of glycol dimethyl ether prepared Williamson synthesis method refines, belong to infiltrating and vaporizing membrane Application Areas.
Background technology
Glycol dimethyl ether is colourless liquid, has ether smell, stable in properties, can with the multiple immiscible organic solvents such as water and ethanol, ether, chloroform.Glycol dimethyl ether, as a kind of aprotic polar solvent of excellent property, except being used as gas absorbent, extraction agent and paint remover, also can be used for the fields such as electrochemistry, boronation, the synthesis of organic medicinal intermediate.
At present, glycol dimethyl ether suitability for industrialized production mainly adopts Williamson synthesis method, first ethylene glycol monomethyl ether and basic metal or its oxyhydroxide are reacted, make ethylene glycol monomethyl ether alcohol alkali cpd, react obtained with the methylating reagent such as methyl chloride again, next, in glycol dimethyl ether treating process, traditional dewatering process adopts the dehydration of siccative Calcium Chloride Powder Anhydrous, consumption about 10%, the moisture content in glycol dimethyl ether can be made to be down to less than 1%, and then to slough foreshot by rectifying and get product.Its weak point is the method that glycol dimethyl ether dehydration adopts first dry rectifying again, complex process, energy consumption is large, and while Calcium Chloride Powder Anhydrous water suction, also adsorb a certain amount of glycol dimethyl ether formation jelly, reclaim more difficult, the then contaminate environment of abandoning, and the yield that result also in glycol dimethyl ether is low.
Summary of the invention
The technical problem that the present invention mainly solves is: for the technique of the Williamson method synthesizing glycol dme extensively adopted at present, the process for refining of its product is improved, need the purity reducing reagent consumption, improve glycol dinitrate ether product, the content reducing moisture and impurity, and can product yield be improved.It is simple that the method has technological process, and facility investment is few, and capacity usage ratio is high, the feature that the rate of recovery is high.
Concrete technical scheme is as follows:
Pervaporation method refines a technique for glycol dimethyl ether, comprises the steps:
S1: the glycol dimethyl ether acid neutralization that Williamson synthesis method is produced, removing sediment, obtains glycol dimethyl ether crude product;
S2: glycol dimethyl ether crude product is sent into rectifying tower and is separated, tower top material obtains light constituent after condensation, and the heavy constituent at the bottom of tower is back in the building-up reactions of glycol dimethyl ether;
S3: after the light constituent heating obtained by step S2, send into seepage slope membrane separation apparatus in vapour form, retain side material and obtain glycol dinitrate ether product after condensation, per-meate side material obtains penetrating fluid after condensation.
The principle of this operational path is: the ethylene glycol monomethyl ether first utilizing the mode of rectifying to get rid of unreacted to complete, a part of water can also be made to be removed as the heavy constituent of rectifying tower simultaneously, water-content in tower top material is reduced, now, by infiltration evaporation technique, tower top material is dewatered again, so just can realize water content in glycol dinitrate ether product and be down to low-down degree.Overcome first with medicament in traditional technology to dewater, again by medicament consume greatly, the product water content high problem of rectifying except heavy constituent.
In step S1, need the glycol dimethyl ether mother liquor to Williamson synthesis method is produced first to carry out neutralizing treatment, owing to containing the complete basic metal of unreacted or its oxyhydroxide in mother liquor, after neutralizing treatment is carried out to it, can ensure that in follow-up technique, equipment is not subject to the corrosion of alkali, simultaneously also can some solid residues preliminarily in separating reaction material; Conventional Neutralization settlement still can be adopted, under constantly stirring, add hydrochloric acid soln, about regulating pH to 7 ~ 8.
In step s 2, the thick glycol dimethyl ether obtained carries out rectifying separation in rectifying tower, and the heavy constituent impurity (such as: the water of ethylene glycol monomethyl ether and a part) in thick glycol dimethyl ether can enter at the bottom of tower; Light constituent, comprise glycol dimethyl ether, a part of water, unreacted methyl chloride completely, and some other small-molecular-weight impurity can enter to tower top, if when rectifying is abundant, tower top glycol dimethyl ether and water can form azeotrope.In this step, thick glycol dimethyl ether achieves removing ethylene glycol monomethyl ether, obtains preliminary separation, eliminates some impurity in material, alleviates the burden of follow-up separation process.As improvement, in this step, the heavy constituent obtained at the bottom of tower is back in Williamson reaction as raw material, raw material is utilized fully, and can change molecular balance, improves the transformation efficiency of ethylene glycol monomethyl ether, improves the yield of integrated artistic.
In step s3, after preferably will heating up to light constituent, carry out infiltration evaporation separation circuit again, find can improve infiltration evaporation membrane separation efficiency like this, the moisture content in product can be made to decline further.Through lot of experiments, find to heat preferably by such as under type in step s3: the glycol dimethyl ether steam first light constituent and infiltration evaporation separator being retained side carries out heat exchange, also can suitably heat, and elevates the temperature to 40 ~ 100 DEG C; Then, material after heating is heated to 80 ~ 150 DEG C further in vaporizer, the advantage of such improved procedure is: by carrying out heat exchange with product, save energy, waste heat is fully utilized, another benefit is the mass transfer force that improve infiltration evaporation process, can improve the purity of product better.
Due in step s 2, carry out while rectifying removes to ethylene glycol monomethyl ether, also taken away portion of water, this just makes the load of infiltrating and vaporizing membrane reduce, and make the water content of the finished product lower, step S2 and S3 serves synergistic action effect simultaneously.
In step s3, the selection of infiltrating and vaporizing membrane has also been through that lot of experiments gropes to obtain, owing to entering into the system to be separated of infiltration evaporation film device, include glycol dimethyl ether, water, some small molecular weight impurities, when such system is separated, need to select most suitable infiltrating and vaporizing membrane to be separated preferably to make product, make the purity of product, flux all better.If the separation factor of film is low, the moisture in product, small molecular weight impurity etc. can be caused not to be separated with glycol dimethyl ether completely, if it is improper that mould material is selected, can cause water can through rete, and small molecular weight impurity is stayed and is retained side, although moisture content declines, other impurity but fails effectively to be separated.The type selecting of infiltrating and vaporizing membrane is preferably: molecular screen membrane, soft silica film, chitosan film, PVA film or sodium alginate film; More preferably molecular screen membrane.
The gauge pressure that working pressure in infiltration evaporation step preferably retains side is 0 ~ 1MPa, and the absolute pressure of per-meate side is 10 ~ 10000Pa.More preferably, the gauge pressure retaining side is 0.1 ~ 0.8 MPa, and the absolute pressure of per-meate side is 100 ~ 1500Pa.Mainly because if pressure reduction is too small, then cause water can not completely through rete, if pressure reduction is excessive, then facility investment can be caused large, and running cost be high.
Infiltration evaporation membrane element can be combined by 1 ~ 100 infiltration vaporization membrane module series, parallel or series-parallel connection mode.
Another object of the present invention there is provided the device that a kind of pervaporation method refines glycol dimethyl ether, comprise rectifying tower, Pervaporation membrane separator, Neutralization settlement still is connected to the opening for feed of rectifying tower, the tower top discharge port of rectifying tower is connected with tundish by overhead condenser, and the outlet of tundish is connected with Pervaporation membrane separator; The side that retains of Pervaporation membrane separator is connected to products pot by product condenser, and the per-meate side of Pervaporation membrane separator is connected with infiltration flow container by penetrating fluid condenser, and penetrating fluid condenser is also connected with vacuum pump.
As the improvement of this device, the outlet of tundish is connected with Pervaporation membrane separator by force (forcing) pump, preheater, vaporizer successively.
As the improvement of this device, infiltration flow container is connected to the opening for feed of rectifying tower; Pervaporation membrane separator is retained between the export pipeline of side and the inlet ductwork of vaporizer and is connected by heat exchange mode.
beneficial effect
Compared with the process for refining of traditional Williamson method glycol dimethyl ether, method tool of the present invention has the following advantages:
1. do not need before rectifying just to steam, greatly reduce energy consumption;
2. the ethylene glycol monomethyl ether of discharging at the bottom of rectifying tower turns back to retort and utilizes further as reaction raw materials, improves ethylene glycol monomethyl ether transformation efficiency;
3. traditional technology adopts desiccant dehydration, and glycol dimethyl ether loss is large, and present method adopts the mode of first rectifying infiltration evaporation again, and effectively overcome the shortcoming of reagent dewatering type, simple to operate, the rate of recovery is high;
4. the present invention utilizes product heat to carry out preheating to entering the moisture glycol dimethyl ether before vaporizer, improves system self-energy utilization ratio, reduce further production energy consumption;
5. the present invention utilizes rectification step will remove ethylene glycol monomethyl ether and part water to realize a step and complete, alleviate the step of infiltration evaporation technique simultaneously, achieve synergy;
6. penetrating fluid returns to rectifying tower recycling by the present invention, substantially realizes glycol dimethyl ether free of losses.
7. glycol dimethyl ether process for refining provided by the invention, the water content in glycol dimethyl ether is little, can be reduced to 0.005 (w/w) in optimum embodiment.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Wherein 1 is Neutralization settlement still, and 2 is rectifying tower, and 3 is overhead condensers, and 4 is tundish, and 5 is force (forcing) pumps, 6 is preheaters, and 7 is vaporizers, and 8 is Pervaporation membrane separator, and 9 is penetrating fluid condensers, 10 is vacuum pumps, and 11 is infiltration flow containers, and 12 is product condensers, and 13 is products pots.
Embodiment
The refining plant structure that following examples adopt as shown in Figure 1, comprise rectifying tower 2, Pervaporation membrane separator 8, Neutralization settlement still 1 is connected to the opening for feed of rectifying tower 2, the tower top discharge port of rectifying tower 2 is connected with tundish 4 by overhead condenser 3, and the outlet of tundish 4 is connected with Pervaporation membrane separator 8 by force (forcing) pump 5, preheater 6, vaporizer 7 successively; The side that retains of Pervaporation membrane separator 8 is connected to products pot 13 by product condenser 12, the per-meate side of Pervaporation membrane separator 13 is connected with infiltration flow container 11 by penetrating fluid condenser 9, penetrating fluid condenser 9 is also connected with vacuum pump 10, and infiltration flow container 11 is connected to the opening for feed of rectifying tower 2; Pervaporation membrane separator is retained the export pipeline of side and is connected by heat exchange mode with between the inlet ductwork of vaporizer 7.
embodiment 1
Hydrochloric acid soln is added neutral to material liquid pH in the glycol dimethyl ether mother liquor that Williamson synthesis method is produced, completely to be precipitated, extract supernatant liquor to be separated to rectifying tower 2, the light constituent of tower top is collected in tundish by being discharged by tower top after condensation, wherein be mainly the azeotrope of glycol dimethyl ether-water, also comprise some other small molecular weight impurity; Ethylene glycol monomethyl ether in system and part water are discharged by the bottom of tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and utilizes further as raw material.
Controlling flow is that the light constituent being collected in tundish is transported to preheater 5 by 3000kg/h, by product steam, 75 DEG C are preheated to this feed liquid, then vaporizer 7 is entered, feed liquid is heated to 138 DEG C and enters in vapour form and carry out dehydration by the Pervaporation membrane separator 8 that 10 NaA molecular sieve membrane membrane modules are in series and be separated, total membrane area 200m
2.Film retain side gauge pressure 0.5MPa, per-meate side absolute pressure 500Pa.Water in feed liquid through infiltrating and vaporizing membrane through penetrating fluid condenser 9 condensation laggard enter penetrating fluid tank 11, penetrating fluid water content is 95.05%, and penetrating fluid returns further to rectifying tower and recycles; Feed liquid water content drops to 0.12% (w/w) by membrane sepn concentrate, enters products pot 13 again after flowing through preheater 5 pairs of feed liquid preheatings through product condenser 12 condensation.The content of glycol dimethyl ether is 99.5%, the yield comparatively traditional method raising about 5 ~ 7% of ethylene glycol monomethyl ether.
embodiment 2
Hydrochloric acid soln is added neutral to material liquid pH in the glycol dimethyl ether mother liquor that Williamson synthesis method is produced, completely to be precipitated, extract supernatant liquor to be separated to rectifying tower 2, the light constituent of tower top is collected in tundish by being discharged by tower top after condensation, wherein be mainly the azeotrope of glycol dimethyl ether-water, also comprise some other small molecular weight impurity; Ethylene glycol monomethyl ether in system and part water are discharged by the bottom of tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and utilizes further as raw material.
Controlling flow is that the light constituent being collected in tundish is transported to preheater 5 by 3000kg/h, by product steam, 40 DEG C are preheated to this feed liquid, then vaporizer 7 is entered, feed liquid is heated to 80 DEG C and enters in vapour form and carry out dehydration by the Pervaporation membrane separator 8 that 20 NaA molecular sieve membrane membrane modules are in series and be separated, total membrane area 300m
2.Film retain side gauge pressure 0.8 MPa, per-meate side absolute pressure 100 Pa.Water in feed liquid through infiltrating and vaporizing membrane through penetrating fluid condenser 9 condensation laggard enter penetrating fluid tank 11, penetrating fluid water content is 97.05%, and penetrating fluid returns further to rectifying tower and recycles; Feed liquid water content drops to 0.08% (w/w) by membrane sepn concentrate, enters products pot 13 again after flowing through preheater 5 pairs of feed liquid preheatings through product condenser 12 condensation.The content of glycol dimethyl ether is 99.8%, the yield comparatively traditional method raising about 4 ~ 6% of ethylene glycol monomethyl ether.
embodiment 3
Hydrochloric acid soln is added neutral to material liquid pH in the glycol dimethyl ether mother liquor that Williamson synthesis method is produced, completely to be precipitated, extract supernatant liquor to be separated to rectifying tower 2, the light constituent of tower top is collected in tundish by being discharged by tower top after condensation, wherein be mainly the azeotrope of glycol dimethyl ether-water, also comprise some other small molecular weight impurity; Ethylene glycol monomethyl ether in system and part water are discharged by the bottom of tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and utilizes further as raw material.
Controlling flow is that the light constituent being collected in tundish is transported to preheater 5 by 3000kg/h, by product steam, 80 DEG C are preheated to this feed liquid, then vaporizer 7 is entered, feed liquid is heated to 138 DEG C and enters in vapour form and carry out dehydration by the Pervaporation membrane separator 8 that 60 NaA molecular sieve membrane membrane modules are in series and be separated, total membrane area 200m
2.Film retain side gauge pressure 0.5MPa, per-meate side absolute pressure 1000Pa.Water in feed liquid through infiltrating and vaporizing membrane through penetrating fluid condenser 9 condensation laggard enter penetrating fluid tank 11, penetrating fluid water content is 90.63%, and penetrating fluid returns further to rectifying tower and recycles; Feed liquid water content drops to 0.005% (w/w) by membrane sepn concentrate, enters products pot 13 again after flowing through preheater 5 pairs of feed liquid preheatings through product condenser 12 condensation.The content of glycol dimethyl ether is 99.9%, the yield comparatively traditional method raising about 8 ~ 10% of ethylene glycol monomethyl ether.
Claims (1)
1. pervaporation method refines a technique for glycol dimethyl ether, it is characterized in that, comprises the steps:
In the glycol dimethyl ether mother liquor that Williamson synthesis method is produced, add hydrochloric acid soln neutral to material liquid pH, completely to be precipitated, extract supernatant liquor and be separated to rectifying tower, the light constituent of tower top is discharged by tower top and be collected in tundish after condensation; Ethylene glycol monomethyl ether in system and part water are discharged by the bottom of tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and utilizes further as raw material; Controlling flow is that the light constituent being collected in tundish is transported to preheater by 3000kg/h, by product steam, 80 DEG C are preheated to this feed liquid, then vaporizer is entered, feed liquid is heated to 138 DEG C and enters in vapour form and carry out dehydration by the Pervaporation membrane separator that 60 NaA molecular sieve membrane membrane modules are in series and be separated, total membrane area 200m
2; Film retain side gauge pressure 0.5MPa, per-meate side absolute pressure 1000Pa; Water in feed liquid through infiltrating and vaporizing membrane through penetrating fluid condenser condenses laggard enter penetrating fluid tank, penetrating fluid water content is 90.63%, and penetrating fluid returns further to rectifying tower and recycles; Feed liquid water content drops to 0.005wt% by membrane sepn concentrate, and flowing through preheater to the content entering products pot glycol dimethyl ether through product condenser condenses again after feed liquid preheating is 99.9%.
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| CN113061079A (en) * | 2021-03-31 | 2021-07-02 | 河南红东方化工股份有限公司 | Ethylene glycol dimethyl ether continuous rectification process |
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Address after: 211806, No. 6, step road, Pukou Economic Development Zone, Nanjing, Jiangsu Patentee after: JIANGSU NINE HEAVEN HIGH-TECH Co.,Ltd. Address before: 211808, No. 1 Hu Dong Road, Pukou Economic Development Zone, Jiangsu, Nanjing Patentee before: JIANGSU NINE HEAVEN HIGH-TECH Co.,Ltd. |