CN103709016A - Process and device for refining glycol dimethyl ether by using pervaporation method - Google Patents
Process and device for refining glycol dimethyl ether by using pervaporation method Download PDFInfo
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- CN103709016A CN103709016A CN201310714949.3A CN201310714949A CN103709016A CN 103709016 A CN103709016 A CN 103709016A CN 201310714949 A CN201310714949 A CN 201310714949A CN 103709016 A CN103709016 A CN 103709016A
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- C07C41/01—Preparation of ethers
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Abstract
The invention relates to a process for refining glycol dimethyl ether by using a pervaporation method. The process comprises the following steps: neutralizing Williamson synthesized glycol dimethyl ether mother solution, and then, settling to obtain crude glycol dimethyl ether; separating the crude glycol dimethyl ether through a rectifying tower, discharging a glycol dimethyl ether and water azeotrope from the top of the tower, condensing, and then, collecting the glycol dimethyl ether and water azeotrope into an intermediate tank; discharging part of water and ethylene glycol monomethyl ether from the bottom of the tower; delivering the glycol dimethyl ether and water azeotrope to a preheater, and then, enabling the glycol dimethyl ether and water azeotrope to enter an evaporator, wherein the glycol dimethyl ether and water azeotrope is collected in the intermediate tank; enabling water-contained glycol dimethyl ether to enter a pervaporation membrane separator, wherein the water-contained glycol dimethyl ether is evaporated from the evaporator; condensing penetrating materials through a penetrating liquid condenser, then, enabling the penetrating materials to enter a penetrating liquid tank, further, returning the penetrating liquid to the rectifying tower to carry out recovery treatment, thus obtaining high-purity glycol dimethyl ether at the interception side of the pervaporation membrane separator; and, preheating through the preheater, condensing through a finished product condenser, and then, enabling the high-purity glycol dimethyl ether to enter a product tank. The process is simple in technological process, low in equipment investment as well as high in energy utilization ratio and recovery rate.
Description
Technical field
The technique and the device that the present invention relates to the refining glycol dimethyl ether of a kind of pervaporation method, relate in particular to a kind of glycol dimethyl ether that Williamson synthesis method is prepared and carry out refining technique and device, belongs 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 is as a kind of aprotic polar solvent of excellent property, except as gas absorbent, extraction agent and paint remover, also can be used for electrochemistry, boronation, organic medicine intermediate and the field such as synthesizes.
At present, glycol dimethyl ether suitability for industrialized production mainly adopts Williamson synthesis method, first ethylene glycol monomethyl ether is reacted with basic metal or its oxyhydroxide, make ethylene glycol monomethyl ether alcohol alkali cpd, react and make with methylating reagents such as methyl chloride again, next, in glycol dimethyl ether treating process, traditional dewatering process is to adopt the dehydration of siccative Calcium Chloride Powder Anhydrous, consumption approximately 10%, can make the moisture content in glycol dimethyl ether be down to below 1%, and then by rectifying, slough foreshot and get product.Its weak point is that glycol dimethyl ether dehydration adopts the first dry method of rectifying again, complex process, energy consumption is large, and in the time of Calcium Chloride Powder Anhydrous water suction, also adsorb a certain amount of glycol dimethyl ether and form jelly, reclaim more difficult, the contaminate environment of abandoning, and caused the yield of glycol dimethyl ether 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 adopting at present, process for refining to its product improves, need to reduce reagent consumption, improve the content of purity, reduction moisture and the impurity of glycol dinitrate ether product, and can improve product yield.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:
A technique for the refining glycol dimethyl ether of pervaporation method, comprises the steps:
S1: the glycol dimethyl ether acid neutralization that Williamson synthesis method is produced, remove sediment, obtain glycol dimethyl ether crude product;
S2: glycol dimethyl ether crude product is sent into rectifying tower and carry out separation, tower top material obtains light constituent after condensation, the heavy constituent at the bottom of tower is back in the building-up reactions of glycol dimethyl ether;
S3: by after the resulting light constituent heating of step S2, send into Pervaporation membrane separator with vapor form, hold back 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: first utilize the mode of rectifying to get rid of the ethylene glycol monomethyl ether that unreacted completes, can also make a part of water 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.Having overcome first with medicament in traditional technology dewaters, with rectifying, consumes the problem large, product water content is high except the medicament of heavy constituent again.
In step S1, that the glycol dimethyl ether mother liquor that need to produce Williamson synthesis method first carries out neutralizing treatment, owing to containing the complete basic metal of unreacted or its oxyhydroxide in mother liquor, after it is carried out to neutralizing treatment, the equipment in follow-up technique of can guaranteeing is not subject to the corrosion of alkali, simultaneously yet preliminary some solid residues in separating reaction material; Can adopt conventional Neutralization settlement still, under constantly stirring, add hydrochloric acid soln, regulate left and right, pH to 7～8.
In step S2, the thick glycol dimethyl ether obtaining carries out rectifying separation in rectifying tower, for example, at the bottom of the heavy constituent impurity (: ethylene glycol monomethyl ether and a part of water) in thick glycol dimethyl ether can enter tower; Light constituent, comprises glycol dimethyl ether, a part of water, unreacted methyl chloride completely, and some other small molecules amount 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 has been realized the removing of ethylene glycol monomethyl ether, and has obtained preliminary separation, has removed some impurity in material, has alleviated the burden of follow-up separation process.As improvement, in this step, the heavy constituent obtaining 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 again infiltration evaporation separation circuit, find can improve infiltration evaporation membrane separation efficiency like this, can make the moisture content in product decline further.Through lot of experiments, find preferably to heat in the following way in step S3: the glycol dimethyl ether steam of first light constituent and infiltration evaporation separator being held back to side carries out heat exchange, also can suitably heat, and elevates the temperature to 40～100 ℃; Then, material after heating is further heated to 80～150 ℃ in vaporizer, the advantage of such improved procedure is: by carrying out heat exchange with product, saved energy, waste heat is fully utilized, another benefit is the mass transfer force that has improved infiltration evaporation process, can improve better the purity of product.
Due in step S2, when ethylene glycol monomethyl ether is carried out rectifying and removed, also taken away portion of water simultaneously, the load reduction that this just makes infiltrating and vaporizing membrane, makes the water content of the finished product lower, and step S2 and S3 have played synergistic action effect.
In step S3, the selection of infiltrating and vaporizing membrane also through lot of experiments grope 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, while carrying out separation for such system, need to select most suitable infiltrating and vaporizing membrane so that product obtains preferably separatedly, make the purity of product, flux all better.If the separation factor of film is low, can cause moisture in product, small molecular weight impurity etc. can not be completely separated with glycol dimethyl ether, if it is improper that mould material is selected, can cause water can see through rete, and small molecular weight impurity is stayed and is held back side, although moisture content declines, other impurity but fails to obtain effective separation.The type selecting of infiltrating and vaporizing membrane is preferably: molecular screen membrane, soft silica film, chitosan film, PVA film or sodium alginate film; Molecular screen membrane more preferably.
The gauge pressure that working pressure in infiltration evaporation step is preferably held back side is 0～1MPa, and the absolute pressure of per-meate side is 10～10000Pa.More preferably, the gauge pressure of holding back side is 0.1～0.8 MPa, and the absolute pressure of per-meate side is 100～1500Pa.Be mainly because if pressure reduction is too small, cause water not see through rete completely, if pressure reduction is excessive, can cause facility investment large, running cost is 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 has been to provide the device of the refining glycol dimethyl ether of a kind of pervaporation method, comprise rectifying tower, infiltration evaporation membrane separation apparatus, Neutralization settlement still is connected in 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 infiltration evaporation membrane separation apparatus; The side of holding back of infiltration evaporation membrane separation apparatus is connected in products pot by product condenser, and the per-meate side of infiltration evaporation membrane separation apparatus 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 infiltration evaporation membrane separation apparatus by force (forcing) pump, preheater, vaporizer successively.
As the improvement of this device, infiltration flow container is connected in the opening for feed of rectifying tower; Infiltration evaporation membrane separation apparatus is held back between the export pipeline of side and the inlet ductwork of vaporizer and is connected by heat exchange mode.
beneficial effect
Compare with the process for refining of traditional Williamson method glycol dimethyl ether, method tool of the present invention has the following advantages:
1. before rectifying, do not need 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 further utilizes as reaction raw materials, has improved ethylene glycol monomethyl ether transformation efficiency;
3. traditional technology adopts desiccant dehydration, and glycol dimethyl ether loss is large, and present method adopts the first rectifying mode of infiltration evaporation again, has effectively overcome the shortcoming of reagent dewatering type, and simple to operate, the rate of recovery is high;
4. the present invention utilizes product heat to carry out preheating to the moisture glycol dimethyl ether entering before vaporizer, has improved system self-energy utilization ratio, has further reduced 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, alleviated the step of infiltration evaporation technique simultaneously, realized synergy;
6. the present invention returns penetrating fluid to rectifying tower recycling, 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, the 2nd, and rectifying tower, the 3rd, overhead condenser, the 4th, tundish, the 5th, force (forcing) pump, the 6th, preheater, the 7th, vaporizer, the 8th, infiltration evaporation membrane separation apparatus, the 9th, penetrating fluid condenser, the 10th, vacuum pump, the 11st, infiltration flow container, the 12nd, product condenser, the 13rd, products pot.
Embodiment
The refining plant structure that following examples adopt as shown in Figure 1, comprise rectifying tower 2, infiltration evaporation membrane separation apparatus 8, Neutralization settlement still 1 is connected in 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 infiltration evaporation membrane separation apparatus 8 by force (forcing) pump 5, preheater 6, vaporizer 7 successively; The side of holding back of infiltration evaporation membrane separation apparatus 8 is connected in products pot 13 by product condenser 12, the per-meate side of infiltration evaporation membrane separation apparatus 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 in the opening for feed of rectifying tower 2; Infiltration evaporation membrane separation apparatus is held back between the export pipeline of side and the inlet ductwork of vaporizer 7 and is connected by heat exchange mode.
embodiment 1
In the glycol dimethyl ether mother liquor of producing to Williamson synthesis method, add hydrochloric acid soln neutral to material liquid pH, treat that precipitation completely, extract supernatant liquor to rectifying tower 2 and carry out separation, the light constituent of tower top is by being discharged and be collected in tundish after condensation by tower top, 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 at the bottom of by tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and further utilizes as raw material.
Controlling flow is that 3000kg/h is transported to preheater 5 by the light constituent that is collected in tundish, by product steam, this feed liquid is preheated to 75 ℃, then enter vaporizer 7, feed liquid be heated to 138 ℃ with vapor form enter into by 10 NaA molecular screen membrane membrane module infiltration evaporation membrane separation apparatuss 8 in series, dewatered separated, total membrane area 200m
2.Film hold back side gauge pressure 0.5MPa, per-meate side absolute pressure 500Pa.Water in feed liquid sees through infiltrating and vaporizing membrane and enters to permeate flow container 11 through 9 condensations of penetrating fluid condenser are laggard, and penetrating fluid water content is 95.05%, and penetrating fluid further returns to rectifying tower and recycles; Feed liquid water content drops to 0.12% (w/w) by membrane sepn concentrate, after the 5 pairs of feed liquid preheatings of preheater of flowing through, enters products pot 13 again through 12 condensations of product condenser.The content of glycol dimethyl ether is 99.5%, and the yield of ethylene glycol monomethyl ether improves approximately 5～7% compared with traditional method.
embodiment 2
In the glycol dimethyl ether mother liquor of producing to Williamson synthesis method, add hydrochloric acid soln neutral to material liquid pH, treat that precipitation completely, extract supernatant liquor to rectifying tower 2 and carry out separation, the light constituent of tower top is by being discharged and be collected in tundish after condensation by tower top, 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 at the bottom of by tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and further utilizes as raw material.
Controlling flow is that 3000kg/h is transported to preheater 5 by the light constituent that is collected in tundish, by product steam, this feed liquid is preheated to 40 ℃, then enter vaporizer 7, feed liquid be heated to 80 ℃ with vapor form enter into by 20 NaA molecular screen membrane membrane module infiltration evaporation membrane separation apparatuss 8 in series, dewatered separated, total membrane area 300m
2.Film hold back side gauge pressure 0.8 MPa, per-meate side absolute pressure 100 Pa.Water in feed liquid sees through infiltrating and vaporizing membrane and enters to permeate flow container 11 through 9 condensations of penetrating fluid condenser are laggard, and penetrating fluid water content is 97.05%, and penetrating fluid further returns to rectifying tower and recycles; Feed liquid water content drops to 0.08% (w/w) by membrane sepn concentrate, after the 5 pairs of feed liquid preheatings of preheater of flowing through, enters products pot 13 again through 12 condensations of product condenser.The content of glycol dimethyl ether is 99.8%, and the yield of ethylene glycol monomethyl ether improves approximately 4～6% compared with traditional method.
embodiment 3
In the glycol dimethyl ether mother liquor of producing to Williamson synthesis method, add hydrochloric acid soln neutral to material liquid pH, treat that precipitation completely, extract supernatant liquor to rectifying tower 2 and carry out separation, the light constituent of tower top is by being discharged and be collected in tundish after condensation by tower top, 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 at the bottom of by tower, and ethylene glycol monomethyl ether returns to glycol dimethyl ether reactor and further utilizes as raw material.
Controlling flow is that 3000kg/h is transported to preheater 5 by the light constituent that is collected in tundish, by product steam, this feed liquid is preheated to 80 ℃, then enter vaporizer 7, feed liquid be heated to 138 ℃ with vapor form enter into by 60 NaA molecular screen membrane membrane module infiltration evaporation membrane separation apparatuss 8 in series, dewatered separated, total membrane area 200m
2.Film hold back side gauge pressure 0.5MPa, per-meate side absolute pressure 1000Pa.Water in feed liquid sees through infiltrating and vaporizing membrane and enters to permeate flow container 11 through 9 condensations of penetrating fluid condenser are laggard, and penetrating fluid water content is 90.63%, and penetrating fluid further returns to rectifying tower and recycles; Feed liquid water content drops to 0.005% (w/w) by membrane sepn concentrate, after the 5 pairs of feed liquid preheatings of preheater of flowing through, enters products pot 13 again through 12 condensations of product condenser.The content of glycol dimethyl ether is 99.9%, and the yield of ethylene glycol monomethyl ether improves approximately 8～10% compared with traditional method.
Claims (9)
1. a technique for the refining glycol dimethyl ether of pervaporation method, is characterized in that, comprises the steps:
S1: the glycol dimethyl ether acid neutralization that Williamson synthesis method is produced, remove sediment, obtain glycol dimethyl ether crude product;
S2: glycol dimethyl ether crude product is sent into rectifying tower and carry out separation, tower top material obtains light constituent after condensation, the heavy constituent at the bottom of tower is back in the building-up reactions of glycol dimethyl ether;
S3: by after the resulting light constituent heating of step S2, send into Pervaporation membrane separator with vapor form, hold back side material and obtain glycol dinitrate ether product after condensation, per-meate side material obtains penetrating fluid after condensation.
2. the technique of the refining glycol dimethyl ether of pervaporation method according to claim 1, is characterized in that: the acid in step S1 is hydrochloric acid soln, regulates pH to 7～8.
3. the technique of the refining glycol dimethyl ether of pervaporation method according to claim 1, is characterized in that: in step S3, light constituent first heats or heat exchange is warming up to 40～100 ℃, is more further warming up to 80～150 ℃ in vaporizer.
4. the technique of the refining glycol dimethyl ether of pervaporation method according to claim 1, is characterized in that: in step S3, infiltrating and vaporizing membrane is a kind of in molecular screen membrane, soft silica film, chitosan film, PVA film or sodium alginate film.
5. the technique of the refining glycol dimethyl ether of pervaporation method according to claim 1, is characterized in that: in step S3, the gauge pressure that infiltration evaporation membrane separation apparatus is held back side is 0.1～0.8 MPa, and the absolute pressure of per-meate side is 100～1500Pa.
6. the technique of the refining glycol dimethyl ether of pervaporation method according to claim 1, is characterized in that: infiltration evaporation membrane element is combined by 1～100 infiltration vaporization membrane module series, parallel or series-parallel connection mode.
7. the device of the refining glycol dimethyl ether of a pervaporation method, comprise rectifying tower (2), infiltration evaporation membrane separation apparatus (8), it is characterized in that: Neutralization settlement still (1) is connected in 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 infiltration evaporation membrane separation apparatus (8); The side of holding back of infiltration evaporation membrane separation apparatus (8) is connected in products pot (13) by product condenser (12), the per-meate side of infiltration evaporation membrane separation apparatus (13) is connected with infiltration flow container (11) by penetrating fluid condenser (9), and penetrating fluid condenser (9) is also connected with vacuum pump (10).
8. pervaporation method according to claim 8 is refined the device of glycol dimethyl ether, it is characterized in that, the outlet of tundish (4) is connected with infiltration evaporation membrane separation apparatus (8) by force (forcing) pump (5), preheater (6), vaporizer (7) successively.
9. the device of the refining glycol dimethyl ether of pervaporation method according to claim 8, is characterized in that, infiltration flow container (11) is connected in the opening for feed of rectifying tower (2); Infiltration evaporation membrane separation apparatus is held back between the export pipeline of side and the inlet ductwork of vaporizer (7) and is connected by heat exchange mode.
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