Mother liquor recycling device for bronopol production

By combining equipment such as vacuum distillation kettles and distillation columns, the problems of resource waste and environmental pollution in the treatment of bromoninitol production mother liquor have been solved, and the efficient recovery and purity improvement of useful components in the mother liquor have been achieved.

CN224009049UActive Publication Date: 2026-03-20WEIFANG YUKAI CHEM
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Patent Information

Application Number
CN202520469805.4
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-03-17
Publication Date
2026-03-20
Estimated Expiration
2035-03-17

AI Technical Summary

Technical Problem

The current methods for treating the mother liquor in the production of bromonitol are crude, resulting in resource waste and environmental pollution, as well as low recovery efficiency, low product purity, and excessive energy consumption.

Method used

The mother liquor recovery and utilization device, which consists of equipment such as a vacuum distillation kettle, a distillation column, a reaction kettle, and a macroporous adsorption resin tank, separates and recovers useful components from the mother liquor through steps such as vacuum distillation, distillation, extraction, and oxidation.

Benefits of technology

This method enables the efficient recovery of useful components from the mother liquor, improves product purity and resource utilization, reduces production costs, and minimizes environmental pollution.

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Abstract

The utility model discloses a mother liquor recycling device for bronopol production, and relates to the technical field of bronopol production, an inlet of a reduced pressure distillation kettle is communicated with a mother liquor tank through a pipeline, an outlet of the reduced pressure distillation kettle is communicated with a rectifying tower through a pipeline, and a top outlet of the rectifying tower is communicated with a first condenser through a pipeline; and an outlet of the first condenser is communicated with a bronopol tank through a pipeline. The reduced pressure distillation kettle is used for distilling the mother liquor under a reduced pressure condition, so that the boiling point of each component in the mother liquor is reduced, the energy consumption is reduced, and the decomposition or side reaction of bronopol and other components at high temperature is avoided. The mother liquor subjected to primary concentration and separation through reduced pressure distillation enters a rectifying tower, bronopol and other impurities with similar boiling points are further separated through rectification, and primary purification is achieved. The bronopol steam at the top of the tower is condensed by the first condenser and then is collected to the bronopol tank, so that the bronopol product with higher purity is obtained, and the key step of recovering bronopol from the mother liquor is coherently realized in the whole process.
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Description

TECHNICAL FIELD

[0001] The utility model relates to bromine nitro alcohol production technical field, specifically to a kind of mother liquor recycling device for bromine nitro alcohol production. BACKGROUND

[0002] Bromine nitro alcohol is an important industrial bactericide and preservative, and has a wide application in many fields. In the production process of bromine nitro alcohol, a large amount of mother liquor will be produced. In addition to containing unreacted raw materials such as 2-nitro-1,3-propanediol and bromine, the mother liquor also contains bromine nitro alcohol and various by-products. At present, many enterprises treat the bromine nitro alcohol production mother liquor in a rough way, mostly directly discharged, which not only leads to a lot of resources wasted, increases the production cost, but also causes serious pollution to the environment due to the harmful substances contained in the mother liquor, such as bromide ions that may destroy the ecological balance of water bodies. If conventional treatment methods such as simple distillation and crystallization are used, it is difficult to effectively separate and recover the useful components in the mother liquor, and there are problems such as low recovery efficiency, low product purity and high energy consumption. SUMMARY

[0003] The technical problem to be solved by the utility model is to provide a mother liquor recycling device for bromine nitro alcohol production to reduce the waste of raw materials and improve the economic benefit of the product in view of the deficiencies of the prior art.

[0004] To solve the above technical problems, the technical scheme of the utility model is:

[0005] A mother liquor recycling device for bromine nitro alcohol production, comprising a vacuum distillation kettle, an inlet of the vacuum distillation kettle is communicated with a mother liquor tank through a pipeline, an outlet of the vacuum distillation kettle is communicated with a rectifying tower through a pipeline, a top outlet of the rectifying tower is communicated with a first condenser through a pipeline, and an outlet of the first condenser is communicated with a bromine nitro alcohol tank through a pipeline.

[0006] As an improved technical scheme, it further comprises a reaction kettle, an inlet of the reaction kettle is respectively communicated with the mother liquor tank and a macroporous adsorption resin tank, an outlet of the reaction kettle is communicated with a filter, and a liquid phase outlet of the filter is communicated to the vacuum distillation kettle through a pipeline.

[0007] As an improved technical scheme, a bottom outlet of the rectifying tower is communicated with an adjusting tank through a pipeline, an inlet of the adjusting tank is communicated with a sodium carbonate solution tank through a pipeline, an outlet of the adjusting tank is communicated with a first extraction tank through a pipeline, the first extraction tank is communicated with an extractant feeding tank, an outlet of the first extraction tank is communicated with a liquid separation tank, an outlet of the liquid separation tank is communicated with a distillation tank through a pipeline, and a lower outlet of the distillation tank is communicated with a 2-nitro-1,3-propanediol recovery tank.

[0008] The upper outlet of the distillation tank is communicated with an extractant recovery tank.

[0009] The outlet of the distribution tank is communicated with an oxidation tank through a pipeline, the inlet of the oxidation tank is respectively communicated with an acid liquid tank and a chlorinated water tank through pipelines, the outlet of the oxidation tank is communicated with a second extraction tank through a pipeline, the inlet of the second extraction tank is communicated with a carbon tetrachloride tank through a pipeline, the outlet of the second extraction tank is communicated with an evaporation tank through a pipeline, the top outlet of the evaporation tank is communicated with a second condenser through a pipeline, and the outlet of the second condenser is communicated with a bromine tank.

[0010] The bottom outlet of the evaporation tank is communicated with a carbon tetrachloride recovery tank.

[0011] Due to the adoption of the above technical scheme, the present application has the following beneficial effects:

[0012] The utility model discloses a mother liquor recycling device for bromine nitromethanol production, including the vacuum distillation kettle, the inlet of vacuum distillation kettle is communicated with the mother liquor tank through the pipeline, the outlet of vacuum distillation kettle is communicated with the rectifying column through the pipeline, the top outlet of rectifying column is communicated with the first condenser through the pipeline, and the outlet of first condenser is communicated with the bromine nitromethanol tank through the pipeline. The mother liquor is distilled under the condition of reducing pressure in the vacuum distillation kettle, the boiling point of each component in the mother liquor is reduced, the energy consumption is reduced, and the bromine nitromethanol and other components are prevented from decomposing or reacting at high temperature. The mother liquor after preliminary concentration and separation by vacuum distillation enters the rectifying column, and the bromine nitromethanol and other impurities with similar boiling points are further separated by rectification to realize preliminary purification. The bromine nitromethanol steam at the top is condensed by the first condenser and collected in the bromine nitromethanol tank to obtain the bromine nitromethanol product with high purity. The key steps of recovering the bromine nitromethanol from the mother liquor are realized in the whole process.

[0013] The utility model discloses still include the reaction kettle, the inlet of reaction kettle is communicated with mother liquor tank and macroporous adsorption resin tank respectively, the outlet of reaction kettle is communicated with the filter, and the liquid phase export of filter is communicated to vacuum distillation kettle through the pipeline. In the reaction kettle, macroporous adsorption resin can selectively adsorb the pigment, part organic by -product and macromolecular impurity of possibly interfering subsequent recovery process in the mother liquor under the condition of stirring. The macroporous adsorption resin and other insoluble impurities after adsorbing impurities are intercepted by the filter, and its liquid phase export is connected to the vacuum distillation kettle, so that the purified mother liquor enters the subsequent distillation link. The purity of the mother liquor entering the vacuum distillation kettle is effectively improved, the interference of impurities to subsequent operation is reduced, the purity of bromine nitromethanol product is helped to improve, the service life of subsequent equipment is prolonged, and the maintenance cost caused by problems such as impurity blockage is reduced.

[0014] The bottom outlet of the rectifying tower is communicated with a regulating tank through a pipeline, the inlet of the regulating tank is communicated with a sodium carbonate solution tank through a pipeline, the outlet of the regulating tank is communicated with a first extraction tank through a pipeline, the inlet of the first extraction tank is communicated with an extractant feeding tank, the outlet of the first extraction tank is communicated with a liquid separation tank, the outlet of the liquid separation tank is communicated with a distillation tank through a pipeline, the lower outlet of the distillation tank is communicated with a 2-nitro-1,3-propanediol recovery tank, and the upper outlet of the distillation tank is communicated with an extractant recovery tank. The remaining mother liquor at the bottom outlet of the rectifying tower enters the regulating tank, the sodium carbonate solution tank adds sodium carbonate solution to the regulating tank, the pH value of the mother liquor is adjusted, the acidic impurities in the mother liquor are reacted, and the existence form of raw materials such as 2-nitro-1,3-propanediol is changed, so that the subsequent separation is promoted. The mother liquor after the pH value is adjusted enters the first extraction tank, the extractant feeding tank provides an extractant such as ethyl acetate, under the condition of stirring, 2-nitro-1,3-propanediol is transferred to the extractant phase. The liquid separation tank realizes two-phase separation, the extractant phase containing 2-nitro-1,3-propanediol enters the distillation tank, through normal pressure distillation, the extractant is evaporated and recovered to the extractant recovery tank, and the remaining residue is collected to the 2-nitro-1,3-propanediol recovery tank. Unreacted 2-nitro-1,3-propanediol raw materials in the mother liquor are efficiently recovered, the resource utilization rate is improved, the production cost is reduced, meanwhile, the recycling of the extractant is realized, and the green chemistry concept is met.

[0015] The outlet of the liquid separation tank is communicated with an oxidation tank through a pipeline, the inlet of the oxidation tank is respectively communicated with an acid liquid tank and a chlorine water tank through pipelines, the outlet of the oxidation tank is communicated with a second extraction tank through a pipeline, the inlet of the second extraction tank is communicated with a carbon tetrachloride tank through a pipeline, the outlet of the second extraction tank is communicated with an evaporation tank through a pipeline, the top outlet of the evaporation tank is communicated with a second condenser through a pipeline, and the outlet of the second condenser is communicated with a bromine tank. The bottom outlet of the evaporation tank is communicated with a carbon tetrachloride recovery tank through a pipeline. In the oxidation tank, bromide ions in the mother liquor are oxidized into bromine. The liquid after oxidation enters the second extraction tank, the carbon tetrachloride tank provides carbon tetrachloride as an extractant, and the bromine is extracted into the carbon tetrachloride phase. The carbon tetrachloride phase containing bromine enters the evaporation tank, the bromine is evaporated through heating, the top steam is condensed into the bromine tank through the second condenser, and the carbon tetrachloride in the bottom residue is recovered into the carbon tetrachloride recovery tank. The bromine in the mother liquor is effectively recovered, the pollution of bromide ions to the environment is avoided, the recycling of resources is realized, and the production cost is further reduced. BRIEF DESCRIPTION OF DRAWINGS

[0016] The utility model is further explained below in combination with the drawings and examples.

[0017] Figure 1 It is the structural schematic diagram of the utility model embodiment;

[0018] Wherein: 1, vacuum distillation still; 2, mother liquor tank; 3, rectifying column; 4, first condenser; 5, bromine nitromethanol tank; 6, reaction kettle; 7, macroporous adsorption resin tank; 8, filter; 9, adjusting tank; 10, sodium carbonate solution tank; 11, first extraction tank; 12, extraction agent feeding tank; 13, liquid-liquid separator; 14, distillation tank; 15, 2-nitro-1, 3-propanediol recovery tank; 16, extractant recovery tank; 17, oxidation tank; 18, acid tank; 19, chlorinated water tank; 20, second extraction tank; 21, carbon tetrachloride tank; 22, evaporation tank; 23, second condenser; 24, bromine tank; 25, carbon tetrachloride recovery tank. DETAILED DESCRIPTION

[0019] The utility model is further explained below in combination with the drawings and examples.

[0020] As Figure 1 The mother liquor recovery device for bromine nitromethanol production includes a vacuum distillation still 1, the inlet of the vacuum distillation still 1 is connected with a mother liquor tank 2 through a pipeline, the outlet of the vacuum distillation still 1 is connected with a rectifying column 3 through a pipeline, the top outlet of the rectifying column 3 is connected with a first condenser 4 through a pipeline, and the outlet of the first condenser 4 is connected with a bromine nitromethanol tank 5 through a pipeline. The vacuum distillation still 1 distills the mother liquor under reduced pressure, reduces the boiling points of various components in the mother liquor, reduces energy consumption, and avoids the decomposition or side reaction of bromine nitromethanol and other components at high temperatures. After the preliminary concentration and separation of the mother liquor through vacuum distillation, the mother liquor enters the rectifying column 3, and bromine nitromethanol and other impurities with similar boiling points are further separated through rectification to achieve preliminary purification. The bromine nitromethanol vapor at the top is condensed through the first condenser 4 and collected in the bromine nitromethanol tank 5 to obtain bromine nitromethanol products with high purity. The key steps of recovering bromine nitromethanol from the mother liquor are realized in a coherent process.

[0021] The utility model also includes a reaction kettle 6, the inlet of the reaction kettle 6 is respectively connected with the mother liquor tank 2 and the macroporous adsorption resin tank 7, the outlet of the reaction kettle 6 is connected with a filter 8, and the liquid phase outlet of the filter 8 is connected to the vacuum distillation still 1 through a pipeline. In the reaction kettle 6, the macroporous adsorption resin can selectively adsorb pigments, part of organic by-products and macromolecular impurities that may interfere with the subsequent recovery process under stirring conditions. The filter 8 retains the macroporous adsorption resin and other insoluble impurities after adsorbing impurities, and the liquid phase outlet is connected to the vacuum distillation still 1, so that the purified mother liquor enters the subsequent distillation link. The purity of the mother liquor entering the vacuum distillation still 1 is effectively improved, the interference of impurities on subsequent operations is reduced, the purity of bromine nitromethanol products is improved, the service life of subsequent equipment is prolonged, and the maintenance cost caused by problems such as impurity blockage is reduced.

[0022] The bottom outlet of the rectification tower 3 is communicated with a regulating tank 9 through a pipeline, the inlet of the regulating tank 9 is communicated with a sodium carbonate solution tank 10 through a pipeline, the outlet of the regulating tank 9 is communicated with a first extraction tank 11 through a pipeline, the inlet of the first extraction tank 11 is communicated with an extractant feeding tank 12, the outlet of the first extraction tank 11 is communicated with a liquid separation tank 13, the outlet of the liquid separation tank 13 is communicated with a distillation tank 14 through a pipeline, the lower outlet of the distillation tank 14 is communicated with a 2-nitro-1,3-propanediol recovery tank 15, and the upper outlet of the distillation tank 14 is communicated with an extractant recovery tank 16. The remaining mother liquor at the bottom outlet of the rectification tower 3 enters the regulating tank 9, the sodium carbonate solution tank 10 adds sodium carbonate solution to the regulating tank 9, adjusts the pH value of the mother liquor, reacts with the acidic impurities in the mother liquor, and changes the existence form of the raw materials such as 2-nitro-1,3-propanediol, so as to facilitate the subsequent separation. The mother liquor after adjusting the pH value enters the first extraction tank 11, the extractant feeding tank 12 provides an extractant such as ethyl acetate, and under the condition of stirring, the 2-nitro-1,3-propanediol is transferred to the extractant phase. The liquid separation tank 13 realizes the separation of two phases, the extractant phase containing 2-nitro-1,3-propanediol enters the distillation tank 14, the extractant is evaporated and recovered to the extractant recovery tank 16 through atmospheric distillation, and the remaining residue is collected to the 2-nitro-1,3-propanediol recovery tank 15. The unreacted 2-nitro-1,3-propanediol raw material in the mother liquor is efficiently recovered, the resource utilization rate is improved, the production cost is reduced, the recycling of the extractant is realized at the same time, and the green chemistry concept is met.

[0023] The outlet of the liquid separation tank 13 is communicated with an oxidation tank 17 through a pipeline, the inlet of the oxidation tank 17 is respectively communicated with an acid liquid tank 18 and a chlorine water tank 19 through pipelines, the outlet of the oxidation tank 17 is communicated with a second extraction tank 20 through a pipeline, the inlet of the second extraction tank 20 is communicated with a carbon tetrachloride tank 21 through a pipeline, the outlet of the second extraction tank 20 is communicated with an evaporation tank 22 through a pipeline, the top outlet of the evaporation tank 22 is communicated with a second condenser 23 through a pipeline, and the outlet of the second condenser 23 is communicated with a bromine tank 24. The bottom outlet of the evaporation tank 22 is communicated with a carbon tetrachloride recovery tank 25 through a pipeline. In the oxidation tank 17, the bromide ion in the mother liquor is oxidized to bromine. The liquid after oxidation enters the second extraction tank 20, the carbon tetrachloride tank 21 provides carbon tetrachloride as an extractant, and the bromine is extracted into the carbon tetrachloride phase. The carbon tetrachloride phase containing bromine enters the evaporation tank 22, the bromine is evaporated by heating, the top steam is condensed by the second condenser 23 and then collected into the bromine tank 24, and the carbon tetrachloride in the bottom residue is recovered into the carbon tetrachloride recovery tank 25. The bromine in the mother liquor is effectively recovered, the pollution of bromide ion to the environment is avoided, the recycling of resources is realized, and the production cost is further reduced.

[0024] It should be understood that the embodiments are only used for illustrating the present application and are not used for limiting the scope of the present application. In addition, it should be understood that after reading the content taught by the present application, those skilled in the art can make various changes or modifications to the present application, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Claims

1. A device for recovering and utilizing mother liquor from the production of bromonitroethanol, characterized in that: The apparatus includes a vacuum distillation kettle, the inlet of which is connected to a mother liquor tank via a pipeline, the outlet of which is connected to a distillation column via a pipeline, the top outlet of which is connected to a first condenser via a pipeline, and the outlet of the first condenser via a pipeline is connected to a bromonitrol tank.

2. The mother liquor recovery and utilization device for bromonitrile production as described in claim 1, characterized in that: It also includes a reaction vessel, the inlet of which is connected to the mother liquor tank and the macroporous adsorption resin tank respectively, and the outlet of the reaction vessel is connected to a filter, the liquid phase outlet of which is connected to the vacuum distillation vessel through a pipeline.

3. The mother liquor recovery and utilization device for bromonitroethanol production as described in claim 1, characterized in that: The bottom outlet of the distillation column is connected to a regulating tank via a pipeline. The inlet of the regulating tank is connected to a sodium carbonate solution tank via a pipeline. The outlet of the regulating tank is connected to a first extraction tank via a pipeline. The inlet of the first extraction tank is connected to an extractant feeding tank. The outlet of the first extraction tank is connected to a separatory tank. The outlet of the separatory tank is connected to a distillation tank via a pipeline. The lower outlet of the distillation tank is connected to a 2-nitro-1,3-propanediol recovery tank.

4. The mother liquor recovery and utilization device for bromonitrile production as described in claim 3, characterized in that: The upper outlet of the distillation tank is connected to an extractant recovery tank.

5. The mother liquor recovery and utilization device for bromonitroethanol production as described in claim 3, characterized in that: The outlet of the separating tank is connected to an oxidation tank via a pipe. The inlet of the oxidation tank is connected to an acid tank and a chlorine water tank via pipes. The outlet of the oxidation tank is connected to a second extraction tank via a pipe. The inlet of the second extraction tank is connected to a carbon tetrachloride tank via a pipe. The outlet of the second extraction tank is connected to an evaporator via a pipe. The top outlet of the evaporator is connected to a second condenser via a pipe. The outlet of the second condenser is connected to a bromine tank.

6. The mother liquor recovery and utilization device for bromonitroethanol production as described in claim 5, characterized in that: The bottom outlet of the evaporator is connected to a carbon tetrachloride recovery tank via a pipe.