CN213113165U - Continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid - Google Patents
Continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid Download PDFInfo
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- CN213113165U CN213113165U CN202021456724.4U CN202021456724U CN213113165U CN 213113165 U CN213113165 U CN 213113165U CN 202021456724 U CN202021456724 U CN 202021456724U CN 213113165 U CN213113165 U CN 213113165U
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Abstract
The utility model discloses a continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid, which comprises a dissolving kettle, more than two stages of esterification kettles connected in series and connected with a discharge port of the dissolving kettle, and an esterification dehydration tower connected with gas outlets of the esterification kettles at all stages, wherein a liquid phase outlet at the bottom of the esterification dehydration tower is communicated with a reflux port of a first-stage esterification kettle; the gas phase outlet of the esterification dehydration tower is communicated with the material inlet of the first condenser, the material outlet of the first condenser is communicated with the oil-water separator, and the oil outlet of the oil-water separator is communicated with the reflux port of the esterification dehydration tower; the last esterification kettle is sequentially connected with a dealcoholization kettle, a distillation kettle, a third condenser, an alkali washing kettle, a water washing kettle and a refining kettle. The utility model discloses a tertiary cauldron of esterifying establishes ties successive layer and progressively esterifies in succession, and the result is via dealcoholizing the cauldron after, retrieves the butanol and flows back to the first order cauldron of esterifying and continue the reaction, the bigger comprehensive recycle ratio who has improved the mellow wine.
Description
Technical Field
The utility model relates to an ester serialization production field especially relates to a by nylon acid preparation production mixing binary dibutyl's serialization apparatus for producing.
Background
Nylon acid, commonly known as mixed dibasic acid, is a byproduct material in the industrial production of adipic acid, and comprises the main components of succinic acid (15-25%), glutaric acid (50-65%), adipic acid (15-25%), a metal salt catalyst (about 0.5%) and a small amount of solid impurities through analysis.
According to the current domestic production technology level, roughly estimated, 5-6 million tons of nylon acid auxiliary materials are generated in the production of adipic acid in China every year, and the nylon acid auxiliary materials are resources which can be well utilized. The effective utilization of nylon acid is mainly used for preparing nylon acid dimethyl ester, has excellent material chemical characteristics, is widely used as a coating resin solvent, and can also replace solvents such as isophorone and propylene glycol ether in certain formulas.
There are also some reports on the relevant technology for preparing mixed dibutyl dibasic acid by using nylon acid, and there is a patent (publication No. CN102226013A, Von Liang Jiang Ping) that nylon acid and n-butanol are subjected to esterification reaction under the catalysis of concentrated sulfuric acid to obtain dibutyl nylon acid. In another patent (publication No. CN104945248A, Zhang Shiyuan, Jiangsu Ruitai chemical), the method adopts nylon acid and isobutyl alcohol to synthesize diisobutyl nylon acid by esterification under the condition of a super-strong solid catalyst, and lacks of a post-treatment process, and the product obtained by the method has a high acid value (3-5 mgKOH/g) and does not meet the application requirements of some special products.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a by nylon acid preparation production mixing binary dibutyl's serialization apparatus for producing.
The utility model discloses an innovation point lies in the utility model provides a prepare the serialization apparatus for producing mixed binary dibutyl by nylon acid, adopt tertiary cauldron series connection successive layer progressive type of esterifying to esterify in succession, tertiary cauldron temperature of esterifying risees in proper order, vapor phase evaporation material gets into the dehydration tower of esterifying through the cauldron gas outlet of esterifying at different levels in the reaction process, condenser and oil water separator, by-product water is discharged, the mellow wine flows back to the first order and esterifies the cauldron continuation reaction, the maximize impels the reaction in the cauldron of esterifying at different levels to go on to the positive direction, make final esterification rate reach more than 99%. And after the product of the third esterification kettle is dealcoholized by the dealcoholization kettle, the recovered butanol flows back to the first-stage esterification kettle for continuous reaction, so that the comprehensive recovery utilization rate of the alcohol is greatly improved. The utility model discloses but possess serialization production, practice thrift the production energy consumption, reduce a great deal of advantages such as "three wastes" production, reduction in production cost. According to the utility model discloses the characteristics such as mixed binary dibutyl ester product that obtain has that acid value is low, the content is high, the color and luster is shallow can be applied to and use as excellent viscosity reduction plasticizer in plastics, the rubber products to reduce enterprise user's manufacturing cost.
In order to realize the purpose of the utility model, the technical proposal of the utility model is that: a continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid comprises a dissolving kettle, more than two stages of esterification kettles connected in series and connected with a discharge port of the dissolving kettle, and an esterification dehydration tower connected with an air outlet of each stage of esterification kettles, wherein a liquid phase outlet at the bottom of the esterification dehydration tower is communicated with a reflux port of a first stage of esterification kettle; the gas phase outlet of the esterification dehydration tower is communicated with the material inlet of the first condenser, the material outlet of the first condenser is communicated with the oil-water separator, and the oil outlet of the oil-water separator is communicated with the reflux port of the esterification dehydration tower; the water outlet of the oil-water separator is communicated with a recovery tower through a pipeline, the gas outlet of the recovery tower is communicated with a material inlet of a second condenser, and a material outlet of the second condenser is communicated with a reflux port of the oil-water separator; the last stage esterification kettle is sequentially connected with a dealcoholization kettle, a distillation kettle, a third condenser, an alkali washing kettle, a water washing kettle and a refining kettle; and the air outlet of the dealcoholization kettle is connected with a butanol recovery tank.
Furthermore, a filter is arranged on a connecting pipeline of the dissolving kettle and the first-stage esterification kettle. The filter can effectively filter out insoluble substances in the materials.
Further, the butanol recovery tank is communicated with a return port of the first-stage esterification kettle. And after the product of the third esterification kettle is dealcoholized by the dealcoholization kettle, the recovered butanol flows back to the first esterification kettle to continue the reaction, so that the comprehensive recovery utilization rate of the alcohol is greatly improved, the reaction in the first esterification kettle is promoted to be carried out in the positive direction, and the esterification rate of each esterification kettle is further improved.
Further, the esterification kettle has three stages. Each stage of esterification kettle adopts successive progressive continuous esterification, the temperature of each stage of esterification kettle can be independently controlled, the stability of product quality is improved, and the final esterification rate reaches more than 99 percent.
Further, a heating device and a stirring device are arranged in the esterification kettle and the dissolving kettle. The heating device effectively controls the temperature of the esterification reaction, and ensures the esterification rate of each stage of esterification kettle; the stirring device ensures that the reaction materials react more fully in each stage of esterification kettle, and improves the esterification degree.
Further, a filter is arranged on a connecting pipeline of the final esterification kettle and the dealcoholization kettle. The filter can effectively filter out heavy metal salts and other insoluble substances in the water.
Furthermore, a filter is arranged on a pipeline connecting the dealcoholization kettle and the distillation kettle. The filter can further filter out heavy metal salts and other insoluble substances.
The utility model has the advantages that:
1. the utility model discloses a thought of a dehydration tower of esterifying of tertiary cauldron sharing, guarantee that the dehydration tower of esterifying is in an optimum tower efficiency state all the time, the utilization ratio of dehydration tower of esterifying has been improved, a large amount of energy consumptions have been saved, and the gas phase evaporation material gets into the dehydration tower of esterifying through the cauldron gas outlet of esterifying at different levels among the reaction process, condenser and oil water separator, last accessory substance is discharged, the mellow wine flows back to the first order cauldron of esterifying and continues the reaction, the maximize makes the reaction go on to the positive direction, make final esterification rate reach more than 99%.
2. The utility model discloses the product that well third grade esterification cauldron obtained is after dealcoholizing via dealcoholizing the cauldron, retrieves the butanol and flows back to first order esterification cauldron and continue the reaction, and bigger improvement comprehensive recycle rate of mellow wine practices thrift manufacturing cost.
3. The utility model discloses in the cauldron of esterifying at different levels adopt successive layer progressive type to esterify in succession, the cauldron of esterifying at different levels can the independent control temperature, and the mixed binary dibutyl ester product that obtains has advantages such as the color and luster is light, the acid number is low, the content is high, impurity is few, can extensively use as cosolvent, the viscosity reduction plasticizer of coating.
4. The utility model discloses carry out abundant recycle to the by-product material nylon acid of adipic acid, both resources are saved is favorable to the environment again, has great economic benefits and social.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings.
Example 1: as shown in fig. 1, a continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid, which comprises a dissolving kettle 1, more than two esterification kettles 2 connected in series with a dissolving kettle discharge port 1.1, and an esterification dehydration tower 3 connected with each esterification kettle gas outlet 2.1, wherein the esterification kettles 2 are preferably three-stage, a filter 15 is arranged on a connecting pipeline between the dissolving kettle 1 and the first esterification kettle 2, a heating device and a stirring device 17 are arranged in the dissolving kettle 1 and the esterification kettle 2, and a liquid phase outlet 3.1 of the esterification dehydration tower is communicated with a first esterification kettle return port 2.2; a gas phase outlet 3.2 of the esterification dehydration tower is communicated with a material inlet 4.1 of a first condenser 4, a material outlet 4.2 of the first condenser is communicated with an oil-water separator 5, and an oil outlet 5.1 of the oil-water separator is communicated with a reflux port 3.3 of the esterification dehydration tower; the water outlet 5.2 of the oil-water separator is communicated with a recovery tower 6 through a pipeline, the gas outlet 6.1 of the recovery tower is communicated with a material inlet 7.1 of a second condenser 7, and a material outlet 7.2 of the second condenser is communicated with a reflux port 5.3 of the oil-water separator; the last esterification kettle 2 is sequentially connected with a dealcoholization kettle 8, a distillation kettle 9, a third condenser 10, an alkaline washing kettle 11, a water washing kettle 12 and a refining kettle 13, a filter 15 is arranged on a connecting pipeline of the last esterification kettle 2 and the dealcoholization kettle 8, a filter 15 is arranged on a pipeline connecting the dealcoholization kettle 8 and the distillation kettle 9, a butanol recovery tank 14 is connected with a gas outlet 8.1 of the dealcoholization kettle, and the butanol recovery tank 14 is communicated with a reflux port 2.2 of the first esterification kettle.
Before the continuous production device is started, a water-carrying agent (butanol) which is 2-3 times of the effective volume of the oil-water separator 5 and 50% of water are added into the top of the esterification dehydration tower 3 in advance at one time, so that the esterification dehydration system is in a normal working state. Nylon acid and butanol are added into a dissolving kettle 1 according to the mass ratio of 1: 1.3, preheated to 80 ℃ for dissolving, then sequentially pumped into an esterification kettle 2 until the volume of the kettle is 60 percent, and then sufficient butanol is added until the reaction is excessive, wherein the dosage is determined according to calculation and actual production. And (3) heating the esterification kettles 2 at all stages, and controlling the water interface in the oil-water separator 5 when azeotrope is distilled off from the top of the esterification dehydration tower 3. During continuous esterification, gas-phase evaporation materials in the reaction process of each stage of esterification kettle 2 enter an esterification dehydration tower 3 through a gas outlet 2.1 of each stage of esterification kettle 2, alcohol is separated by the esterification dehydration tower 3 and then flows back to each stage of esterification kettle 2 through a first stage esterification kettle reflux opening 2.2 from a liquid phase outlet 3.1 of the esterification dehydration tower for continuous reaction, the separated alcohol-water mixture is condensed by a condenser 4 and further separated by an oil-water separator 5, and the separated alcohol flows back to the esterification dehydration tower 3 through a pipeline from an oil outlet 5.1 of the oil-water separator for continuous separation; the water separated by the oil-water separator 5 enters a recovery tower 6 for further separation, the wastewater is discharged into a wastewater treatment pool 16, part of alcohol and water enter the oil-water separator 5 for secondary separation after being condensed by a second condenser 7 from a gas outlet 6.1 of the recovery tower, and the alcohol is fully recovered. And (3) controlling the esterification degree of each stage of esterification kettle while heating until the material in the third esterification kettle 2 reaches the preset esterification degree and the acid value is less than 8mgKOH/g, and then starting discharging to enter a later stage process. When the third esterification kettle 2 discharges materials, the materials in the dissolving kettle 1 start feeding the first esterification kettle 2, and the butanol in the butanol recovery tank 14 is pumped into the first esterification kettle 2 according to the amount of the butanol taken away by the discharged esterification liquid. When the esterification kettle 2 discharges normally, the system reaches a stable state, and continuous production of the esterification system is realized. According to the difference of the esterification degree of each stage of esterification kettle 2, the temperature of each stage of esterification kettle 2 is increased in sequence.
The temperature and the degree of esterification of each stage of esterification reactor 2 are shown in the following table 1:
TABLE 1
And (3) feeding the esterification solution sent by the third-stage esterification kettle 2 into a dealcoholization kettle 8, starting a vacuum system to dealcoholize, wherein the vacuum degree is 5-10 kPa, when the temperature of the materials in the dealcoholization kettle 8 is reduced, starting heating, finally controlling the dealcoholization temperature at 140 ℃, finishing dealcoholization, and feeding the crude ester materials into a distillation kettle 9. The temperature of the distillation kettle 9 is 155-160 ℃, the vacuum degree is 100Pa, and the temperature of the top of the tower is 140-145 ℃. When the material at the top of the tower is distilled out, the initial fraction can be sent into the esterification kettle 2 for reaction. The crude ester semi-finished product obtained in the rectification section enters an alkali washing process, a sodium carbonate aqueous solution with the concentration of 8% is selected, the using amount of the alkali water is 40% of the mass of the crude ester, and the temperature is 60-70 ℃; a water washing procedure, wherein the consumption of pure water is 30%, and the water washing temperature is 70 ℃; in the refining process, activated clay, diatomite or active carbon is selected as a decoloring agent, the using amount is 0.3-0.4 kg/ton of the product, the refining temperature is 125-130 ℃, and the vacuum degree is 15-20 kPa. And filtering the material obtained from the refining kettle 13 by a filter to obtain the finished mixed dibutyl dibasic acid. And wastewater generated by the recovery tower 6 and wastewater generated by the alkali washing and water washing processes in the alkali washing kettle 11 and the water washing kettle 12 are discharged into a wastewater treatment tank 16.
The relevant indexes of the obtained mixed dibutyl dibasic acid are shown in the following table 2:
TABLE 2
The described embodiments are only some, but not all embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Claims (7)
1. A continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid is characterized by comprising a dissolving kettle, more than two esterification kettles connected in series and connected with a discharge port of the dissolving kettle, and an esterification dehydration tower connected with air outlets of the esterification kettles, wherein a liquid phase outlet at the bottom of the esterification dehydration tower is communicated with a reflux port of a first-stage esterification kettle; the gas phase outlet of the esterification dehydration tower is communicated with the material inlet of the first condenser, the material outlet of the first condenser is communicated with the oil-water separator, and the oil outlet of the oil-water separator is communicated with the reflux port of the esterification dehydration tower; the water outlet of the oil-water separator is communicated with a recovery tower through a pipeline, the gas outlet of the recovery tower is communicated with a material inlet of a second condenser, and a material outlet of the second condenser is communicated with a reflux port of the oil-water separator; the last esterification kettle is sequentially connected with a dealcoholization kettle, a distillation kettle, a third condenser, an alkali washing kettle, a water washing kettle and a refining kettle; and the air outlet of the dealcoholization kettle is connected with a butanol recovery tank.
2. The continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid as claimed in claim 1, wherein the connecting pipeline of the dissolving kettle and the first stage esterification kettle is provided with a filter.
3. The continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid as claimed in claim 1, wherein the butanol recovery tank is communicated with the reflux port of the first esterification kettle.
4. The continuous production apparatus for preparing and producing mixed dibutyl dibasic acid from nylon acid as claimed in claim 1, wherein the esterification kettle has three stages.
5. The continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid as claimed in claim 1, wherein the esterification kettle and the dissolution kettle are respectively provided with a heating device and a stirring device.
6. The continuous production apparatus for preparing and producing mixed dibutyl dibasic acid from nylon acid as claimed in claim 1, wherein the connecting pipeline of the last esterification kettle and the dealcoholization kettle is provided with a filter.
7. The continuous production device for preparing and producing mixed dibutyl dibasic acid from nylon acid as claimed in claim 1, wherein the pipeline connecting the dealcoholization kettle and the distillation kettle is provided with a filter.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115010633A (en) * | 2022-07-11 | 2022-09-06 | 宁夏汉润生物科技有限公司 | Synthetic method and device of ring closing object |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115010633A (en) * | 2022-07-11 | 2022-09-06 | 宁夏汉润生物科技有限公司 | Synthetic method and device of ring closing object |
| CN115010633B (en) * | 2022-07-11 | 2024-04-12 | 宁夏汉润生物科技有限公司 | Synthesis method and device of ring-closing compound |
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