CN205528530U - Apparatus for producing of two different butyl esters of 1, 2 - cyclohexane dioctyl phthalate - Google Patents
Apparatus for producing of two different butyl esters of 1, 2 - cyclohexane dioctyl phthalate Download PDFInfo
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- CN205528530U CN205528530U CN201620121052.9U CN201620121052U CN205528530U CN 205528530 U CN205528530 U CN 205528530U CN 201620121052 U CN201620121052 U CN 201620121052U CN 205528530 U CN205528530 U CN 205528530U
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Abstract
The utility model relates to an apparatus for producing of two different butyl esters of 1, 2 - cyclohexane dioctyl phthalate, the device are equipped with the esterifying kettle connected in order through the pipe in, and cauldron, the cauldron that stews, water washing tank, dealcoholize cauldron and decoloration cauldron, still be connected with the esterification column on the esterifying kettle, the esterification column connects gradually with condenser I and water knockout drum and forms closed -loop, water knockout drum, stew cauldron and water washing tank are connected with the water collection tank respectively, the water collection tank all is connected with stills, and stills is connected with pure water collection tank, the utility model discloses simple structure, through esterify, steps such as neutralization, washing, dealcoholize, decoloration, the monoester that produces in reation kettle reaction 100%, the dibasic acid esters reaction 99.5%, the product yield is high, reaction condition is mild, does not have other impurity and produces, retrieve mellow wine as raw materials secondary retrieval and utilization, utilization ratio of material height, neutralization, washing, oil water separator's the pure water that contains distills through the distillation column, lime set circulation retrieval and utilization, and cleaner production, a small amount of cauldron raffinate is collected succeeding crop biochemical treatment and is qualifiedly discharged.
Description
Technical field
This utility model relates to Organic Chemicals preparing technical field, and a kind of 1, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester.
Background technology
Large-scale normal butane method maleic anhydride production many employings solvent absorption process.Relative to water absorption technique, solvent absorption energy consumption is low, and yield is high, and quality is good, and equipment corrosion is little, and cycle of operation is long.The solvent of China Maleic Anhydrite production and application has DIBE1,2-thiacyclohexane dioctyl phthalate diisobutyl ester and DBP dibutyl phthalate, and wherein DIBE is more satisfactory lyosoption.It is characterized in: boiling point is high, and at a temperature of operation, vapour pressure is less, and solvent loss is less, and chemical stability is good, viscosity small flow is good, the most weak with the affinity of water, good with the affinity of cis-butenedioic anhydride, due to minimum without phenyl ring toxicity, shortcoming is that the market price is high, needs from external import.DBP is also preferable cis-butenedioic anhydride lyosoption, but has phenyl ring, and containing toxicity, at a temperature of operation, vapour pressure is slightly higher, and solvent loss is more than DIBE.Owing to DBP product volume is big, the market price is low, 0.3-0.4 times of only DIBE price, the market competition has price advantage.
Enterprise is in order to adapt to the market competition, it is necessary to reduces the procurement price of DIBE, does not has manufacturer owing to DIBE product is domestic, it is necessary first to domestic enterprise oneself can produce DIBE solvent.Through great efforts, domestic to have producer to develop with DIBP diisobutyl phthalate be raw material, and the technique being produced DIBE by hydrogenation method tentatively reduces DIBE cost.There are the following problems for DIBP hydrogenation technique:
1, hydrogenation catalyst easily inactivates, deep desulfuration the to be carried out process of DBP raw material, and catalyst, desulfurizing agent valency are expensive, and cost is high；
2, consume hydrogen, compressor power consumption, affect cost, remain high；
3, the product trans DIBE isomer Han 4-5% after hydrogenation, affects quality；
4, the side reaction of DIBP hydrogenation is many, the magazins' layout difficulty that product contains；
5, mass difference is bigger compared with imported product.
Designing a more preferable process route and produce DIBE product, make energy consumption lower, yield is higher, better quality, to meet the needs of maleic anhydride production and market, becomes current problem demanding prompt solution.
Utility model content
The cost existed for above-mentioned existing DIBE production technology is high, product quality differ the problem such as bigger compared with imported product, and this utility model provides one 1, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester.
For solving above-mentioned technical problem, the technical solution adopted in the utility model is:
A kind of 1, the process units of 2 ~ cyclohexane cyclohexanedimethanodibasic diisobutyl ester, this device is provided with esterifying kettle, neutralization still, standing still, water washing tank, dealcoholysis still and the decolouring still being sequentially connected with by conduit, it is also associated with esterification column on described esterifying kettle, esterification column is in turn connected to form closed-loop path with condenser I and water knockout drum, described water knockout drum, standing still and water washing tank are connected to water collecting tank, and described water collecting tank is all connected with distillating still, and distillating still is connected with alcohol water collecting tank.
Described dealcoholysis still is connected with condenser II through dealcoholysis tower, and condenser II is connected with recovery alcohol tank and Condensed water collection tank respectively by Liang Ge branch.
Described decolouring still is connected with finished pot through active carbon filter.
It is equipped with material pump on described esterifying kettle, the connecting line neutralized between still, standing still, water washing tank, dealcoholysis still and decolouring still.
The beneficial effects of the utility model:
The 1 of this utility model offer, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, the monoesters reaction 100% that raw material produces in a kettle., dibasic acid esters reaction 99.5%, product yield is high；Raw material HHPA is referred to as cis HHPA, and the product 100% after esterification is cis, without transisomer；Reaction condition is mild, produces without other impurity；Reclaim alcohol as raw material secondary returning use, raw material availability height；Neutralization, washing, the containing alcohol water of oil water separator distill through distillation column, lime set circulating and recovering, and cleaning produces, and make the qualified discharge of biochemical treatment after the collection of a small amount of still residual liquid；Except raw material cost, processing charges is the lowest, and the total cost producing DIBE is only about the 0.3-0.4 of imported product, and can reach the quality level that imported product is same.
Accompanying drawing explanation
Fig. 1 this utility model structural representation；
nullReference: 1、Esterifying kettle，2、Esterification column，3、Condenser I，4、Water knockout drum，5、Solidifying water pot，6、Material pump I，7、Neutralize still，8、Material pump II，9、Stand still，10、Water collecting tank I，11、Material pump III，12、Water washing tank，13、Water collecting tank II，14、Material pump IV，15、Alcohol Water Sproading pump，16、Dealcoholysis still，17、Dealcoholysis tower，18、Condenser II，19、Material pump V，20、Reclaim alcohol tank，21、Reclaim alcohol pump，22、Chilled water heat exchanger，23、Vacuum buffer tank，24、Condensed water collection tank，25、Vacuum pump，26、Decolouring still，27、Finished pot，28、Active carbon filter，29、Material pump VI，30、Distillating still，31、Distillation column，32、Condenser III，33、Alcohol water collecting tank，34、Material pump VII，35、Residual liquid collecting tank.
Detailed description of the invention
Below in conjunction with detailed description of the invention, this utility model is further elaborated.
As shown in the figure: a kind of 1, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, this device is provided with the esterifying kettle 1 being sequentially connected with by conduit, neutralize still 7, stand still 9, water washing tank 12, dealcoholysis still 16 and decolouring still 26, described esterifying kettle 1 and the connecting line neutralized between still 7 are provided with material pump I 6, neutralize still 7 and the connecting line stood between still 9 is provided with material pump II 8, stand the connecting line between still 9 and water washing tank 12 and be provided with material pump III 11, connecting line between water washing tank 12 and dealcoholysis still 16 is provided with material pump IV 14, connecting line between dealcoholysis still 16 and decolouring still 26 is provided with material pump V 19；It is also associated with esterification column 2 on described esterifying kettle 1, esterification column 2 is in turn connected to form closed-loop path with condenser I 3 and water knockout drum 4, solidifying water pot 5 it is also associated with on water knockout drum 4, stand to connect on still 9 and have water collecting tank I 10, connect on water washing tank 12 and have water collecting tank II 13, described solidifying water pot 5, water collecting tank I 10 and water collecting tank II 13 are all connected with distillating still 30, distillating still 30 is connected with condenser III 32 through distillation column 31, condenser III 32 is connected with alcohol water collecting tank 33, alcohol water collecting tank 33 connects and has material pump VII 34；Described dealcoholysis still 16 is connected with condenser II 18 through dealcoholysis tower 17, condenser II 18 is by Liang Ge branch, one branch is connected with reclaiming alcohol tank 20, reclaim to connect on alcohol tank 20 and have recovery alcohol pump 21, another branch is connected with vacuum buffer tank 23 by chilled water heat exchanger 22, and vacuum buffer tank 23 and Condensed water collection tank 24 connect；Being also associated with vacuum pump 25 on vacuum buffer tank 23, described decolouring still 26 is connected with finished pot 27 through active carbon filter 28, is provided with material pump VI 29 between decolouring still 26 and active carbon filter 28.
Embodiment 1
One utilizes device as above production 1, the method for 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isobutanol are added esterifying kettle 1 according to mol ratio 1:1, add catalyst methane cupric sulfophenate, its consumption is 1%% for accounting for reaction raw materials molar percentage, then heat to 60 DEG C of esterifications 10h, the water vapour and the isobutanol steam that produce in reaction enter condenser I 3 through esterification column 2, condensed fluid is isolated isobutanol in water knockout drum 4 and is returned esterifying kettle 1, and aqueous phase enters solidifying water pot 5；
Step 2: the esterifying liquid generated in esterifying kettle 1 is sent into and neutralized in still 7, neutralize with alkali liquor, described alkali liquor is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali liquor by generation ester amount 20%, the neutral temperature of alkali liquor is 60 DEG C, it is then fed into standing still 9 stratification, separating aqueous phase and enter water collecting tank I 10, thick ester is sent in water washing tank 12 and is washed, and the temperature of washing is 60 DEG C, water consumption is the 20% of ester amount, and washings are put in water collecting tank II 13 after separating；
Step 3: after washing, product is sent into dealcoholysis still 16 and removed isobutanol, material is heated to 60 DEG C in dealcoholysis still 16, the dealcoholysis time 3～4h, through dealcoholysis tower 17, in temperature less than 145 DEG C,-0.097MPa vacuum condition gasified, entering condenser II 18, condensed fluid is segregated into reclaiming alcohol tank 20, and the chilled water-to-water heat exchanger of fixed gas 22 enters after vacuum buffer tank 23 separates lime set and extracted out by vacuum pump 25, maintaining system vacuum, lime set enters recycling can 24；After dealcoholysis, the product of gained is sent to the still 26 that decolours, and decolours through activated carbon adsorption, and the finished product decoloured through activated carbon adsorption delivers to active carbon filter 28 removal activity carbon powder again, and filter pressing temperature of charge is 80 DEG C, and the finished product after decolouring sends into finished pot 27；
Step 4: the containing alcohol water in water pot 5 solidifying in step one, step 2, water collecting tank I 10 and water collecting tank II 13 is sent to distillating still 30 and is heated to 90 DEG C, enter alcohol water collecting tank 33 after alcohol-water azeotrope is condensed, be then sent to water washing tank 12 repetitive cycling and use.
Embodiment 2
One utilizes device as above production 1, the method for 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isobutanol are added esterifying kettle 1 according to mol ratio 1:1.5, add catalyst toluenesulfonic acid, its consumption is 1.5% for accounting for reaction raw materials molar percentage, then heat to 100 DEG C of esterifications 15h, the water vapour and the isobutanol steam that produce in reaction enter condenser I 3 through esterification column 2, condensed fluid is isolated isobutanol in water knockout drum 4 and is returned esterifying kettle 1, and aqueous phase enters solidifying water pot 5；
Step 2: the esterifying liquid generated in esterifying kettle 1 is sent into and neutralized in still 7, neutralize with alkali liquor, described alkali liquor is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali liquor by generation ester amount 25%, the neutral temperature of alkali liquor is 70 DEG C, it is then fed into standing still 9 stratification, separating aqueous phase and enter water collecting tank I 10, thick ester is sent in water washing tank 12 and is washed, and the temperature of washing is 70 DEG C, water consumption is the 25% of ester amount, and washings are put in water collecting tank II 13 after separating；
Step 3: after washing, product is sent into dealcoholysis still 16 and removed isobutanol, material is heated to 70 DEG C in dealcoholysis still 16, the dealcoholysis time 3～4h, through dealcoholysis tower 17, in temperature less than 145 DEG C,-0.098MPa vacuum condition gasified, entering condenser II 18, condensed fluid is segregated into reclaiming alcohol tank 20, and the chilled water-to-water heat exchanger of fixed gas 22 enters after vacuum buffer tank 23 separates lime set and extracted out by vacuum pump 25, maintaining system vacuum, lime set enters recycling can 24；After dealcoholysis, the product of gained is sent to the still 26 that decolours, and decolours through activated carbon adsorption, and the finished product decoloured through activated carbon adsorption delivers to active carbon filter 28 removal activity carbon powder again, and filter pressing temperature of charge is 90 DEG C, and the finished product after decolouring sends into finished pot 27；
Step 4: the containing alcohol water in water pot 5 solidifying in step one, step 2, water collecting tank I 10 and water collecting tank II 13 is sent to distillating still 30 and is heated to 100 DEG C, enter alcohol water collecting tank 33 after alcohol-water azeotrope is condensed, be then sent to water washing tank 12 repetitive cycling and use.
Embodiment 3
One utilizes device as above production 1, the method for 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, comprises the following steps:
Step one: raw material HHPA and isobutanol are added esterifying kettle 1 according to mol ratio 1:2, adds catalyst 98%H2SO4Its consumption is 2% for accounting for reaction raw materials molar percentage, then heats to 150 DEG C of esterifications 20h, and the water vapour and the isobutanol steam that produce in reaction enter condenser I 3 through esterification column 2, condensed fluid is isolated isobutanol in water knockout drum 4 and is returned esterifying kettle 1, and aqueous phase enters solidifying water pot 5；
Step 2: the esterifying liquid generated in esterifying kettle 1 is sent into and neutralized in still 7, neutralize with alkali liquor, described alkali liquor is sodium hydroxide solution or Carbon Dioxide sodium solution, the consumption of alkali liquor by generation ester amount 30%, the neutral temperature of alkali liquor is 80 DEG C, it is then fed into standing still 9 stratification, separating aqueous phase and enter water collecting tank I 10, thick ester is sent in water washing tank 12 and is washed, and the temperature of washing is 80 DEG C, water consumption is the 30% of ester amount, and washings are put in water collecting tank II 13 after separating；
Step 3: after washing, product is sent into dealcoholysis still 16 and removed isobutanol, material is heated to 80 DEG C in dealcoholysis still 16, the dealcoholysis time 3～4h, through dealcoholysis tower 17, in temperature less than 145 DEG C,-0.0985MPa vacuum condition gasified, entering condenser II 18, condensed fluid is segregated into reclaiming alcohol tank 20, and the chilled water-to-water heat exchanger of fixed gas 22 enters after vacuum buffer tank 23 separates lime set and extracted out by vacuum pump 25, maintaining system vacuum, lime set enters recycling can 24；After dealcoholysis, the product of gained is sent to the still 26 that decolours, and decolours through activated carbon adsorption, and the finished product decoloured through activated carbon adsorption delivers to active carbon filter 28 removal activity carbon powder again, and filter pressing temperature of charge is 100 DEG C, and the finished product after decolouring sends into finished pot 27；
Step 4: the containing alcohol water in water pot 5 solidifying in step one, step 2, water collecting tank I 10 and water collecting tank II 13 is sent to distillating still 30 and is heated to 120 DEG C, enter alcohol water collecting tank 33 after alcohol-water azeotrope is condensed, be then sent to water washing tank 12 repetitive cycling and use.
The purpose of washing is to remove the alkali of residual in oil phase, prevents product saponification number from exceeding standard, if acid number returns liter after Shui Xi, need to mend alkali, to meet the Con trolling index of acid number.If it is the best that alkali liquor neutralization step quality control obtains, can skip washing step, be directly entered dealcoholysis operation；Or the final products skipping washing step still can meet quality index, then can be directly entered dealcoholysis operation；When caustic wash process concentration of lye is higher or acid number is higher, washing tends not to omit.
The monoesters reaction 100% that raw material of the present utility model produces in a kettle., dibasic acid esters reaction 99.5%, product yield is high；Raw material HHPA is referred to as cis HHPA, and the product 100% after esterification is cis, without transisomer；Reaction condition is mild, produces without other impurity；Reclaim alcohol as raw material secondary returning use, raw material availability height；Neutralization, washing, the containing alcohol water of oil water separator distill through distillation column, lime set circulating and recovering, and cleaning produces, and make the qualified discharge of biochemical treatment after the collection of a small amount of still residual liquid；Except raw material cost, processing charges is the lowest, and the total cost producing DIBE is only about the 0.3-0.4 of imported product, and can reach the quality level that imported product is same.
Claims (4)
1. one kind 1, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: this device is provided with the esterifying kettle (1) being sequentially connected with by conduit, neutralize still (7), stand still (9), water washing tank (12), dealcoholysis still (16) and decolouring still (26), esterification column (2) it is also associated with on described esterifying kettle (1), esterification column (2) is in turn connected to form closed-loop path with condenser I (3) and water knockout drum (4), described water knockout drum (4), stand still (9) and water washing tank (12) is connected to water collecting tank, described water collecting tank is all connected with distillating still (30), distillating still (30) is connected with alcohol water collecting tank (33).
The most as claimed in claim 11, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterized in that: described dealcoholysis still (16) is connected with condenser II (18) through dealcoholysis tower (17), condenser II (18) is connected with recovery alcohol tank (20) and Condensed water collection tank (24) respectively by Liang Ge branch.
The process units of the most as claimed in claim 11,2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterised in that: described decolouring still (26) is connected with finished pot (27) through active carbon filter (28).
The most as claimed in claim 11, the process units of 2-cyclohexane cyclohexanedimethanodibasic diisobutyl ester, it is characterised in that: it is equipped with material pump on described esterifying kettle (1), the connecting line neutralized between still (7), standing still (9), water washing tank (12), dealcoholysis still (16) and decolouring still (26).
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| CN201620121052.9U CN205528530U (en) | 2016-02-16 | 2016-02-16 | Apparatus for producing of two different butyl esters of 1, 2 - cyclohexane dioctyl phthalate |
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| CN201620121052.9U CN205528530U (en) | 2016-02-16 | 2016-02-16 | Apparatus for producing of two different butyl esters of 1, 2 - cyclohexane dioctyl phthalate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110551021A (en) * | 2019-07-18 | 2019-12-10 | 中山市马里奥机械科技有限公司 | Dealcoholization device |
| 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 |
| CN115724879A (en) * | 2022-11-29 | 2023-03-03 | 泰安亚荣生物科技有限公司 | Production method and production equipment of flame retardant TCEP |
| US11975991B2 (en) | 2019-09-19 | 2024-05-07 | Lg Chem, Ltd. | Neutralization/water separation device for esterified product and neutralization/water separation method for esterified product |
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2016
- 2016-02-16 CN CN201620121052.9U patent/CN205528530U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110551021A (en) * | 2019-07-18 | 2019-12-10 | 中山市马里奥机械科技有限公司 | Dealcoholization device |
| US11975991B2 (en) | 2019-09-19 | 2024-05-07 | Lg Chem, Ltd. | Neutralization/water separation device for esterified product and neutralization/water separation method for esterified product |
| 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 |
| CN115724879A (en) * | 2022-11-29 | 2023-03-03 | 泰安亚荣生物科技有限公司 | Production method and production equipment of flame retardant TCEP |
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