CN210140545U - α -gradient recovery device for ethanol in linolenic acid water washing waste liquid - Google Patents

Abstract

The utility model provides a α -gradient recovery unit of ethanol in linolenic acid washing waste liquid, can handle the washing waste liquid that obtains in α -linolenic acid production in order to obtain qualified raw materials ethanol to can regard as chemical fertilizer to carry out recycle to the active ingredient in the above-mentioned washing waste liquid, reduce the waste liquid discharge in α -linolenic acid production, reduction in production cost, reduction in environmental pollution.

Description

α -gradient recovery device for ethanol in linolenic acid water washing waste liquid

Technical Field

The utility model relates to an ethanol recovery unit, especially α -linolenic acid washing waste liquid in ethanol gradient recovery unit belongs to α -linolenic acid production facility technical field.

Background

In α -linolenic acid production, linseed oil or perilla seed oil is subjected to ethyl esterification, saturated and low-unsaturated fatty acids in α -ethyl linolenate are removed by a urea inclusion process to obtain α -ethyl linolenate with high purity, the process flow of the urea inclusion process comprises the steps of adding ethanol and urea into crude ethyl linolenate, cooling after heating and standing to separate out a urea inclusion compound, adding ethanol and urea again to filtrate after filtration to perform inclusion and purification reactions for multiple times, then washing α -ethyl linolenate ethanol mixed liquor for multiple times, heating and evaporating under reduced pressure to obtain a product after washing, and finally performing molecular distillation to obtain a final product, wherein in a washing link, a large amount of washing waste liquid can be generated, the main components of the washing waste liquid are ethanol, but the washing waste liquid contains a large amount of water, reaction intermediates and unreacted raw materials, the components of the washing waste liquid are unknown, the linolenic acid content in the washing waste liquid is difficult to be separated by a conventional separation method at present, the linolenic acid content in the washing waste liquid is too high for other purposes, even if a rectifying tower is adopted for refining, the technical standard, the waste liquid can be used as an industrial waste liquid for obtaining ammonia nitrogen-ammonia-nitrogen-ammonia-acid waste liquid waste.

Disclosure of Invention

An object of the utility model is to provide an ethanol gradient recovery unit in α -linolenic acid washing waste liquid, can handle the washing waste liquid that obtains in α -linolenic acid production in order to obtain qualified raw materials ethanol to can carry out recycle as the chemical fertilizer to the active ingredient in the above-mentioned washing waste liquid, reduce the waste liquid emission in the α -linolenic acid production, reduction in production cost reduces environmental pollution.

In order to achieve the purpose, the technical scheme includes that the ethanol gradient recovery device in α -linolenic acid washing waste liquid comprises an acid storage tank, an acid preparation distillation kettle, a condenser, a waste liquid storage tank and an ethanol storage tank, the acid preparation distillation kettle comprises a kettle body, a distillation kettle feed inlet, a distillation kettle discharge outlet, a steam jacket, an acid inlet, an acid detection port, a temperature measurement port and an ethanol steam outlet are formed in the kettle body, a stirrer is arranged in the distillation kettle body and connected with an output end of a stirring motor arranged outside the distillation kettle body through a stirring shaft, the acid inlet is connected with a discharge port of the acid storage tank through an anticorrosive metering pump, the temperature measurement port is provided with a thermometer, the distillation kettle discharge outlet is connected with the waste liquid storage tank through a waste liquid discharge valve, a spray head connected with the acid inlet is arranged inside the kettle body, the ethanol steam outlet of the acid preparation distillation kettle is connected with a condensation steam inlet of the condenser, a cooling water inlet and a cooling water outlet are arranged on the condenser, an ethanol storage tank is provided with an ethanol feed inlet, an ethanol storage tank, an ethanol discharge port, an ethanol reflux storage tank, a condensate outlet of the condenser is connected with a condensate return valve, a condensate return pipe, a condensate collection tank.

The utility model has the advantages of the utility model discloses a set up and store up sour jar, join in marriage sour stills, condenser and a plurality of ethanol storage tank, can adopt different temperatures to carry out the raw materials ethanol in the gradient distillation back recovery washing waste liquid after the acid treatment to the washing waste liquid in α -linolenic acid production to produce the ammonia nitrogen fertilizer that can be used to the chemical fertilizer, not only reduced the waste liquid emission in the α -linolenic acid production, but also reduction in production cost, its equipment investment cost is low, and is easy and simple to handle, has very big popularization and utilization and worth.

Drawings

Fig. 1 is a schematic flow chart of an apparatus according to an embodiment of the present invention.

Fig. 2 is a schematic structural diagram of an acid preparation distillation still according to an embodiment of the present invention.

Detailed Description

In order to explain the utility model more fully, the following embodiment examples of the present invention are provided, which are only for the explanation of the present invention and do not limit the scope of the present invention.

The invention is explained in further detail with reference to the drawings, in which: 1. preparing an acid distillation kettle; 2. an acid storage tank; 3. a temperature probe; 4. a condenser; 5. a steam jacket; 6. a discharge hole of the distillation kettle; 7. a feeding hole of the distillation kettle; 8. an acid inlet; 9. acid detecting port; 10. a high-temperature pH on-line monitor; 11. a steam condensate outlet; 12. an anti-corrosion metering pump; 13. a steam inlet; 14. a feed inlet of an ethanol storage tank; 15. a discharging port of the ethanol storage tank; 16. an emptying pipe; 17. a cooling water inlet; 18. a cooling water outlet; 19. a condensing steam inlet; 20. a condensate outlet; 21. a reflux pump; 22. a stirring shaft; 23. a shower head; 24. an acid inlet pipe; 25. an ethanol vapor outlet; 26. a stirrer; 27. a stirring motor; 28. a return port; 29. a first ethanol storage tank; 30. a second ethanol storage tank; 31. a third ethanol storage tank; 32. a first condensing valve; 33. a second condensate valve; 34. a third condensing valve; 35. a first reflux valve; 36. a second reflux valve; 37. a third reflux valve; 38. a waste liquid storage tank; 39. a waste liquid pump; 40. discharging branch pipes; 41. a sampling valve; 42. and a waste liquid discharge valve.

As shown in the figure, the ethanol gradient recovery device in α -linolenic acid washing waste liquid comprises an acid storage tank 2, an acid preparation distillation still 1, a condenser 4 and an ethanol storage tank, wherein the ethanol storage tank is provided with an ethanol storage tank feed inlet 14, an emptying pipe 16, an ethanol storage tank discharge port 15 and a reflux port 28, the acid preparation distillation still comprises a still body, the still body is provided with a distillation still feed inlet 7, a distillation still discharge port 6, a steam jacket 5, an acid inlet 8, an acid measurement port 9 and an ethanol steam outlet 25, the distillation still body is provided with a temperature probe 3 and a stirrer 26, the stirrer is connected with an output end of a stirring motor 27 arranged outside the distillation still body through a stirring shaft 22, the acid inlet is connected with a discharge port of the acid storage tank through an anticorrosive metering pump 12, the still body is internally provided with a spray head 23 connected with an acid inlet through an acid inlet pipe 24, the alcohol steam outlet 25 of the distillation still is connected with a condensation steam inlet 19 of the condenser, the condenser is provided with a cooling water inlet 17 and a discharge port of the acid storage tank, the distillation tank, the condensate outlet of the distillation liquid is connected with a condensate liquid inlet of a condensate pump 20, the condensate pump of the distillation liquid storage tank, the condensate pump 20, the condensate of the distillation still is connected with a condensate tank, the condensate tank 32 of the condensate tank, the condensate tank is connected with a condensate tank 32 of the condensate tank, the condensate tank is connected with a condensate tank, the condensate tank 32 of the condensate tank, the condensate tank is connected with a condensate tank, the condensate tank is connected.

In order to facilitate the practical operation of the process, the present embodiment adopts the process flow of three ethanol storage tanks, and in the practical production, one or more ethanol storage tanks can be adopted according to the process requirements to realize the technical effects of the present invention.

When the utility model is produced, the acid storage tank is stored with inorganic strong acid, such as sulfuric acid and hydrochloric acid, the specific type of the acid can be selected from the inorganic acid according to the process requirements, and the sulfuric acid is used in the embodiment; pumping the washing waste liquid into an acid preparation distillation kettle from a feed inlet, starting stirring, starting an anticorrosive metering pump, and spraying sulfuric acid into the washing waste liquid through a spray head, wherein the spray head is adopted because the sulfuric acid can emit a large amount of heat when being mixed with the washing waste liquid, and the mixing uniformity of the sulfuric acid and the washing waste liquid can be improved by adding the sulfuric acid through the spray head in order to prevent bumping or condensation reaction; the PH value of the material mixed solution is read from an online PH monitor, the acid addition is stopped after the process setting requirement is met, then steam is introduced into a steam jacket for distillation, volatile impurities such as free ammonia in the raw water washing waste liquid are not volatilized any more due to the reaction with acid to generate ammonium salt, and after the distillation is finished, the residual liquid is discharged from a discharge hole of a distillation still for concentration and crystallization to obtain the ammonia nitrogen fertilizer.

The utility model discloses a distillation process be the gradient distillation mode, carry out the distillation to the washing waste liquid under different temperatures promptly, carry out many gradients distillation respectively to the distillate under each temperature again. When an ethanol storage tank is adopted, low-temperature primary distillation is carried out at the temperature below 82 ℃, primary distillate is condensed into primary ethanol solution under the action of a condenser, the ethanol content in the primary ethanol solution is higher, the primary ethanol distillate is discharged for later use after the distillation temperature reaches 82 ℃, then the temperature is continuously increased, secondary distillation is continuously carried out at the distillation temperature of 82-90 ℃, secondary ethanol distillate is discharged for later use after the temperature reaches 90 ℃, tertiary distillation is carried out at the distillation temperature of 90-95 ℃, the tertiary ethanol distillate is discharged for later use after the distillation temperature reaches 90 ℃, the difference of each stage of ethanol distillate lies in that the ethanol content is reduced along with the increase of the distillation temperature, after the tertiary distillation is finished, residual liquid in an acid preparation distillation kettle is discharged into a waste liquid storage tank through a waste liquid discharge valve, and then the primary ethanol distillate is discharged for later use, Respectively pumping the second-stage ethanol distillate and the third-stage ethanol distillate into an acid-preparation distillation kettle for second gradient distillation, wherein the distillation temperature of the second gradient distillation is 82-95 ℃, the first-stage ethanol solution with higher concentration can obtain qualified recovered ethanol after the second gradient distillation, the gradient distillation times can be increased for the second-stage and third-stage ethanol with lower concentration to obtain qualified products, the gradient distillation is repeatedly carried out on the second-stage and third-stage ethanol, and finally, the ethanol distillate of each stage can obtain raw material ethanol with the content of more than 95 percent for recovery; the waste liquid in the waste liquid storage tank can be used as ammonia nitrogen liquid fertilizer or crystallized to produce solid fertilizer after the pH value is adjusted to be neutral or alkalescent.

When the three ethanol storage tank process in the embodiment is adopted, low-temperature primary distillation is carried out at the temperature below 82 ℃, the first condensing valve is opened, the second condensing valve and the third condensing valve are closed, the primary ethanol distillate is collected by the first ethanol storage tank, the first condensing valve and the third condensing valve are closed after the distillation temperature reaches 82 ℃, the second condensing valve is opened to carry out secondary distillation at the distillation temperature of 82-90 ℃, the secondary ethanol distillate is collected by the second ethanol storage tank, the first condensing valve and the second condensing valve are closed after the distillation temperature reaches 90 ℃, the third condensing valve is opened to carry out tertiary distillation at the distillation temperature of 90-95 ℃, the tertiary ethanol distillate is collected by the third ethanol storage tank, after the tertiary distillation is finished, the residual liquid in the acid preparation distillation kettle is discharged to the waste liquid storage tank through the waste liquid discharge valve, and then the reflux valves of the first ethanol distillate storage tanks are respectively opened to carry out the primary distillation, And respectively pumping the second-stage ethanol distillate and the third-stage ethanol distillate back to the acid-blending distillation kettle, and respectively and independently carrying out multi-gradient distillation on each stage of ethanol distillate to obtain a qualified ethanol solution. The adoption of a plurality of ethanol storage tanks can reduce the production procedures, improve the production efficiency and reduce the process cost.

After the embodiments of the present invention have been described in detail, those skilled in the art can clearly understand that various changes and modifications can be made without departing from the scope and spirit of the above claims, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention all fall within the scope of the technical solution of the present invention, and the present invention is not limited to the embodiments of the examples given in the specification.

Claims (3)

1. The device for recovering the ethanol gradient in the α -linolenic acid water washing waste liquid is characterized by comprising an acid storage tank, an acid preparation distillation kettle, a condenser, a waste liquid storage tank and an ethanol storage tank, wherein the acid preparation distillation kettle comprises a kettle body, a distillation kettle feed inlet, a distillation kettle discharge outlet, a steam jacket, an acid inlet, an acid measurement port, a temperature measurement port and an ethanol steam outlet are arranged on the kettle body, a stirrer is arranged in the distillation kettle body and connected with an output end of a stirring motor arranged outside the distillation kettle body through a stirring shaft, the acid inlet is connected with a discharge outlet of the acid storage tank through an anticorrosive metering pump, the temperature measurement port is provided with a thermometer, the distillation kettle discharge outlet is connected with the waste liquid storage tank through a waste liquid discharge valve, a spray head connected with the acid inlet is arranged in the kettle body, the ethanol steam outlet of the acid preparation distillation kettle is connected with a condensation steam inlet of the condenser, a cooling water inlet and a cooling water outlet are arranged on the condenser, the ethanol storage tank is provided with an ethanol feed inlet, an emptying pipe, an ethanol storage tank and a reflux inlet are connected with the ethanol storage tank, and a condensate outlet of the distillation kettle are connected.
2. 2. The α -gradient recovery device for ethanol in linolenic acid water-washing waste liquid of claim 1, wherein the device for gradient recovery for ethanol in α -linolenic acid water-washing waste liquid is provided with a first ethanol storage tank, a second ethanol storage tank and a third ethanol storage tank, the first ethanol storage tank, the second ethanol storage tank and the third ethanol storage tank are respectively connected with a condensate outlet of a condenser through a first condensing valve, a second condensing valve and a third condensing valve, and the discharge ports of the first ethanol storage tank, the second ethanol storage tank and the third ethanol storage tank are respectively connected with a reflux pump through a first reflux valve, a second reflux valve and a third reflux valve.
3. 3. The α -gradient recovery device for ethanol in linolenic acid washing waste liquid as claimed in claim 1, wherein the acid measuring port is provided with a pH on-line monitor, a pipeline between the waste liquid discharge valve and the distillation still discharge port is connected with a discharge branch pipe, and the discharge branch pipe is provided with a sampling valve.

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