Production device for comprehensive utilization of cyclopentadecanolide spice production wastewater resources

Abstract

The utility model discloses a production device for comprehensive utilization of cyclopentadecanolide perfume production wastewater resources, which relates to the technical field of cyclopentadecanolide perfume production and comprises a pretreatment neutralization kettle, an acid-containing wastewater head tank and a 30% sodium hydroxide solution head tank. The acid-containing wastewater head tank and the 30% sodium hydroxide solution head tank are respectively connected with the pre-treatment neutralization kettle through pipelines, and the pre-treatment neutralization kettle is also connected with a low-temperature vacuum evaporator through a pipeline. And the method is not limited by brine concentration.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the production technology field of cyclotridecanolide perfume, and particularly relates to a production device for comprehensive utilization of cyclotridecanolide perfume production wastewater resources. BACKGROUND

[0002] The compound of the macrolide mainly refers to a molecule with at least one ester bond in a skeleton of a macrocycle with more than 12 carbon atoms, and cyclotridecanolide is also called hibiscusine, which is a very important macrolide musk, has musk fragrance, and has ambergris fragrance, and has the advantages of rich and long-lasting fragrance, delicate fragrance, strong penetration, and is widely applied to the blending of perfume, cosmetics and food essence. Meanwhile, the cyclotridecanolide has good fixing effect, and is widely used in daily essence such as woody, oriental, fantasy, amber and floral, and is also an important medical synthetic intermediate and is applied to daily chemical industry, medicine and other industries. The cyclotridecanolide is an indispensable raw material in the blending of high-grade essence, and is widely applied to the blending of shampoo, high-grade perfume, various soaps, detergents, powder and personal care products. The cyclotridecanolide can also be used as a food additive, and when used in food essence, it can be used together with general macrolides and has better effect. Since the cyclotridecanolide can improve the palatability of food and increase appetite without harm to health, it is widely applied to food essence such as nuts, herbs, berries, western wine, cakes and the like.

[0003] Since the natural cyclotridecanolide is rare, the cyclotridecanolide sold on the market is mainly obtained by chemical synthesis. At present, only a few countries abroad can produce the cyclotridecanolide in small scale, and the price is very high. The process for synthesizing the cyclotridecanolide is complex, has many operation steps, and uses benzene or toluene and other solvents, so some wastewater with high CODcr concentration, high salt content, high toluene content and deep color is inevitably produced in the production process, and therefore it is of extremely important economic value and social benefit to develop an environment-friendly cyclotridecanolide production process.

[0004] The cyclotridecanolide perfume production belongs to typical fine chemical production, and the fine chemical wastewater has the characteristics of large discharge amount, high CODcr concentration, deep color, high toxicity, complex pollutant composition and difficult biodegradation. In the production process of cyclotridecanolide perfume, toluene is used as a solvent, and wastewater containing a high content of acetic acid or acetate is generated. The discharged wastewater mainly includes: light blue process wastewater generated by hydrolysis of addition ester process, main pollutants are toluene, cyclic ketone organic matter, ester organic matter and sodium acetate, red-brown process wastewater generated by oxidation process, main pollutants are toluene, cyclic ketone organic matter, ether organic matter and acetic acid, and deep blue process wastewater generated by decomposition and neutralization process, main pollutants are toluene and sodium acetate. At present, for the process wastewater with high toluene content, high salt content and high concentration CODcr generated by cyclotridecanolide, the treatment of this kind of wastewater is often through dilution to reduce the salt content of the wastewater. The discharged wastewater with reduced salt content not only causes environmental deterioration, but also leads to soil and watershed salinization. In addition, the organic matter in the wastewater contains benzene ring organic matter, which has poor biodegradability, high biological toxicity and great environmental safety hidden danger, and even affects people's daily life. After pretreatment by three-effect evaporation, the process wastewater is treated by subsequent biochemical comprehensive treatment process. However, the salt water concentration in these conventional treatment methods cannot be too high, and the energy consumption is high when applied, and the treatment cost is too high, so it cannot meet the demand of wastewater treatment. Practical new type content

[0005] To solve the problems in the above background art, the utility model provides a cyclotridecanolide perfume production wastewater resource comprehensive utilization production device.

[0006] The purpose of the utility model can be realized by the following technical schemes.

[0007] A cyclotridecanolide perfume production wastewater resource comprehensive utilization production device, comprising a pretreatment neutralization kettle, an acid-containing wastewater high tank and a 30% sodium hydroxide solution high tank, and the acid-containing wastewater high tank and the 30% sodium hydroxide solution high tank are connected with the pretreatment neutralization kettle through pipelines respectively, and the pretreatment neutralization kettle is also connected with a low-temperature vacuum evaporator through a pipeline, wherein,

[0008] The low-temperature vacuum evaporator comprises an evaporation tank, the evaporation tank is connected with a defoaming agent high tank through a pipeline, the evaporation tank is connected with a condensed water receiving tank through a No. 1 condenser, the evaporation tank is also connected with a heater through a concentrated liquid circulating pump, the evaporation tank is connected with a sedimentation tank through a concentrated liquid discharge pump, and the sedimentation tank is connected with a solid-liquid separation tank through a pipeline.

[0009] As a further preferred of the technical solution: the low-temperature vacuum evaporator further comprises a feed proportioning valve arranged on a pipeline between the pretreatment neutralization tank and the low-temperature vacuum evaporator and used for controlling the flow of the wastewater into the low-temperature vacuum evaporator.

[0010] As a further preferred of the technical solution: the condensate water receiving tank is connected with a condensate water storage tank through a pipeline, the solid-liquid separation tank is connected with a crystallization tank through a pipeline, the crystallization tank is connected with an ethanol high-level tank and a centrifuge through pipelines respectively, the centrifuge is connected with a mother liquor tank through a pipeline, the mother liquor tank is connected with a flash tank through a pipeline, the flash tank is connected with an ethanol receiving tank through a second condenser, and the ethanol receiving tank is connected with the ethanol high-level tank through a pipeline.

[0011] As a further preferred of the technical solution: the settling tank and the solid-liquid separation tank are jointly connected with the fractionation tank through a pipeline.

[0012] As a further preferred of the technical solution: the fractionation tank is connected with a toluene vacuum receiving tank through a spiral plate heat exchanger, and the toluene vacuum receiving tank is connected with a toluene temporary storage tank through a pipeline.

[0013] Compared with the prior art, the beneficial effects of the present application are:

[0014] 1、The present application realizes the recycling and cyclic utilization of valuable resources such as sodium acetate, toluene and ethanol in cyclopentadecanolide perfume production wastewater, through pretreatment neutralization, low-temperature vacuum evaporation, solid-liquid separation, recrystallization and fractionation, not only the harmful substances in the wastewater are effectively removed, but also high-purity sodium acetate is extracted, toluene and ethanol are recovered, these resources can be directly used in the production process, greatly reducing the production cost and improving the resource utilization efficiency.

[0015] 2、The wastewater treated by the production device has reached the environmental protection standard, the CODcr content, toluene content and TOC content are far lower than the relevant emission standard, which means that the wastewater discharge reaches the standard, thereby significantly reducing the pollution to the environment, showing good environmental protection benefits, and since the recycling of resources is realized, the use of fresh water and the discharge of wastewater are reduced, and the risk of environmental pollution is avoided. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 It is a device schematic diagram for cyclopentadecanolide perfume production wastewater treatment resource comprehensive utilization.

[0017] Legend: 1, pretreatment neutralization kettle; 2, acid-containing wastewater high tank; 3, 30% sodium hydroxide high tank; 4, defoaming agent high tank; 5, low-temperature vacuum evaporator; 5-1, feed proportioning valve; 5-2, evaporation tank; 5-3, heater; 5-4, concentrated liquid circulating pump; 5-5, No. 1 condenser; 5-6, condensate water receiving tank; 5-7, concentrated liquid discharge pump; 5-8, settling tank; 5-9, solid-liquid separation tank; 6, condensate water storage tank; 7, crystallization kettle; 8, ethanol high tank; 9, centrifuge; 10, mother liquor tank; 11, flash kettle; 12, No. 2 condenser; 13, ethanol receiving tank; 14, fractional distillation kettle; 15, spiral plate heat exchanger; 16, toluene vacuum receiving tank; 17, toluene temporary storage tank. DETAILED DESCRIPTION

[0018] The technical solutions of the present application will be described clearly and completely below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0019] Embodiment one:

[0020] Please refer to Figure 1The application provides a production device for comprehensive utilization of cyclopentadecanolide perfume production wastewater resources, which comprises a pretreatment neutralization kettle 1, an acid-containing wastewater high tank 2 and a 30% sodium hydroxide solution high tank 3, and the acid-containing wastewater high tank 2 and the 30% sodium hydroxide solution high tank 3 are connected with the pretreatment neutralization kettle 1 through pipelines respectively, and the pretreatment neutralization kettle 1 is also connected with a low-temperature vacuum evaporator 5 through a pipeline, wherein the low-temperature vacuum evaporator 5 comprises an evaporation tank 5-2, the evaporation tank 5-2 is connected with a defoaming agent high tank 4 through a pipeline, the evaporation tank 5-2 is connected with a condensed water receiving tank 5-6 through a first condenser 5-5, the evaporation tank 5-2 is also connected with a heater 5-3 through a concentrated liquid circulating pump 5-4, the evaporation tank 5-2 is connected with a sedimentation tank 5-8 through a concentrated liquid discharge pump 5-7, the sedimentation tank 5-8 is connected with a solid-liquid separation tank 5-9 through a pipeline, the low-temperature vacuum evaporator 5 further comprises a feeding proportioning valve 5-1 arranged on a pipeline between the pretreatment neutralization kettle 1 and the low-temperature vacuum evaporator 5 and used for controlling the flow of wastewater into the low-temperature vacuum evaporator 5, the condensed water receiving tank 5-6 is connected with a condensed water storage tank 6 through a pipeline, the solid-liquid separation tank 5-9 is connected with a crystallization kettle 7 through a pipeline, the crystallization kettle 7 is connected with an ethanol high tank 8 and a centrifuge 9 through pipelines respectively, the centrifuge 9 is connected with a mother liquor tank 10 through a pipeline, the mother liquor tank 10 is connected with a flash kettle 11 through a pipeline, the flash kettle 11 is connected with an ethanol receiving tank 13 through a second condenser 12, and the ethanol receiving tank 13 is connected with the ethanol high tank 8 through a pipeline, the sedimentation tank 5-8 and the solid-liquid separation tank 5-9 are jointly connected with a fractional distillation kettle 14 through a pipeline, the fractional distillation kettle 14 is connected with a toluene vacuum receiving tank 16 through a spiral plate heat exchanger 15, and the toluene vacuum receiving tank 16 is connected with a toluene temporary storage tank 17 through a pipeline.

[0021] Specifically, the acetic acid-containing acid wastewater from the oxidation process of the cyclopentadecanolide perfume production process is collected separately and fed into a neutralization pretreatment kettle 1, stirring is started, and 30% sodium hydroxide solution is metered from a sodium hydroxide head tank 3 and slowly added to the neutralization pretreatment kettle 1, the wastewater is neutralized to a pH of 7-9, and the end point is detected, forming organic wastewater containing sodium acetate salt, the salt-containing, high-toluene-content wastewater from the addition process and decomposition and neutralization process of the cyclopentadecanolide production process is collected and transferred from a production workshop wastewater collection tank to the neutralization pretreatment kettle 1 by a pump, and is mixed uniformly with the above-mentioned neutralized acetic acid wastewater, and then is fed into an evaporation tank 5-2 of a low-temperature vacuum evaporator 5 by a metering pump through a feed proportioning valve, while an antifoaming agent is metered from an antifoaming agent head tank 4 into the evaporation tank 5-2 to prevent the generation of a large amount of foam, and evaporation and condensation are carried out under the conditions of 1000 Pa high vacuum and 28-38°C low temperature, the water phase is condensed by a No. 1 condenser 5-5 to obtain evaporation condensate water of the water phase, and the tank bottom material is transferred to a heater 5-3 by a concentrated liquid circulating pump 5-4 for heating and then backflows to the evaporation tank 5-2 for evaporation and concentration to obtain concentrated waste liquid of the organic phase, then the obtained evaporation condensate water is collected and transferred to a condensate water storage tank 6 through a condensate water receiving tank 5-6 for reuse in the water washing and washing process of the cyclopentadecanolide production process, then the obtained concentrated waste liquid is transferred into a settling tank 5-8 of the low-temperature vacuum evaporator 5 by a concentrated liquid discharge pump 5-7 for preliminary separation, and then is transferred into a solid-liquid separation tank 5-9 for solid-liquid separation to obtain sodium acetate solids containing crystal water and organic concentrated liquid, respectively; and are transferred into a recrystallization kettle 7 and a fractional distillation kettle 14, respectively, and the collected organic concentrated liquid is transferred into the fractional distillation kettle 14, the steam valve of the fractional distillation kettle 14 is opened, the fractional distillation kettle 14 is heated to a kettle temperature of 60-80°C, toluene is recovered under the conditions of 33333 Pa low vacuum and negative pressure, and when the overhead temperature drops or no material is discharged, the collection of toluene is ended, the recovered toluene is condensed by a spiral plate heat exchanger 15, is recovered by a toluene vacuum receiving tank 16, and is transferred into a toluene temporary storage tank 17 for reuse, then ethanol is metered from an ethanol head tank 8 into the recrystallization kettle 7, stirring is started, then the obtained sodium acetate solids are added into the recrystallization kettle 7, the jacket steam valve is opened, the steam in the kettle is condensed by a condenser and backflows to the recrystallization kettle 7, then the cooling water valve is opened to cool and precipitate crystals, the mother liquor tank 10 is vacuumized, the recrystallized solid-liquid mixture is transferred into a centrifuge 9, the centrifuge 9 is started for solid-liquid separation, finally, the mother liquor separated by solid-liquid separation is transferred into a flash kettle 11 through the mother liquor tank 10, ethanol is recovered at 75-80°C under normal pressure for reuse, the ethanol is condensed by a No. 2 condenser 12, is transferred into the ethanol head tank 8 through an ethanol receiving tank 13 for reuse, and the solid crystals remain in the centrifuge 9 to obtain sodium acetate for reuse as raw material sodium acetate in the cyclopentadecanolide addition ester process.

[0022] In summary, by physical and chemical means, the quality of the evaporated condensate collected from the effluent is detected, the CODcr content is 20.3 mg / L, the toluene content is 0.15 mg / L, the TOC content is 5-10 mg / L, the sodium acetate obtained by recrystallization contains 1 crystal water, and the content of sodium acetate monohydrate is 98.1%. Not only the wastewater discharge meets the standard, but also the resource recycling is realized, the energy consumption of wastewater treatment is reduced, and the salt water concentration is not limited.

[0023] The above examples are only used to illustrate the technical method of the utility model and are not limited. Although the utility model has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical method of the utility model can be modified or replaced equivalently without departing from the spirit and scope of the technical method of the utility model.

Claims

1. A production apparatus for the comprehensive utilization of wastewater from the production of cyclopentadecanol flavoring, characterized in that: It comprises a pretreatment neutralization kettle (1), an acid-containing wastewater high tank (2) and a 30% sodium hydroxide solution high tank (3), and the acid-containing wastewater high tank (2) and the 30% sodium hydroxide solution high tank (3) are connected with the pretreatment neutralization kettle (1) through pipelines respectively, the pretreatment neutralization kettle (1) is also connected with a low-temperature vacuum evaporator (5) through a pipeline, wherein, The low-temperature vacuum evaporator (5) comprises an evaporation tank (5-2), the evaporation tank (5-2) is connected with a defoaming agent high tank (4) through a pipeline, the evaporation tank (5-2) is connected with a condensed water receiving tank (5-6) through a No. 1 condenser (5-5), the evaporation tank (5-2) is also connected with a heater (5-3) through a concentrated liquid circulating pump (5-4), the evaporation tank (5-2) is connected with a sedimentation tank (5-8) through a concentrated liquid discharge pump (5-7), and the sedimentation tank (5-8) is connected with a solid-liquid separation tank (5-9) through a pipeline.

2. The production device for comprehensive utilization of cyclopentadecanolide perfume production wastewater resources according to claim 1, characterized in that, The low-temperature vacuum evaporator (5) further comprises a feed proportioning valve (5-1) arranged on the pipeline between the pretreatment neutralization kettle (1) and the low-temperature vacuum evaporator (5) and used for controlling the flow of wastewater into the low-temperature vacuum evaporator (5).

3. The production device for comprehensive utilization of cyclopentadecanolide perfume production wastewater resources according to claim 2, characterized in that, The condensed water receiving tank (5-6) is connected with a condensed water storage tank (6) through a pipeline, the solid-liquid separation tank (5-9) is connected with a crystallization kettle (7) through a pipeline, the crystallization kettle (7) is connected with an ethanol high tank (8) and a centrifugal machine (9) through pipelines respectively, the centrifugal machine (9) is connected with a mother liquor tank (10) through a pipeline, the mother liquor tank (10) is connected with a flash kettle (11) through a pipeline, the flash kettle (11) is connected with an ethanol receiving tank (13) through a No. 2 condenser (12), and the ethanol receiving tank (13) is connected with the ethanol high tank (8) through a pipeline.

4. The production device for comprehensive utilization of cyclopentadecanolide perfume production wastewater resources according to claim 3, characterized in that, The sedimentation tank (5-8) and the solid-liquid separation tank (5-9) are jointly connected with a fractional distillation kettle (14) through a pipeline.

5. The production device for comprehensive utilization of cyclopentadecanolide perfume production wastewater resources according to claim 4, characterized in that, The fractional distillation kettle (14) is connected with a toluene vacuum receiving tank (16) through a spiral plate heat exchanger (15), and the toluene vacuum receiving tank (16) is connected with a toluene temporary storage tank (17) through a pipeline.

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