CN111807960A - Preparation process of isooctyl acrylate - Google Patents

Preparation process of isooctyl acrylate Download PDF

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Publication number
CN111807960A
CN111807960A CN202010764014.6A CN202010764014A CN111807960A CN 111807960 A CN111807960 A CN 111807960A CN 202010764014 A CN202010764014 A CN 202010764014A CN 111807960 A CN111807960 A CN 111807960A
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tower
water
tank
pipe
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CN111807960B (en
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徐忠伟
朱国强
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Zhejiang Yilong New Material Co ltd
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Zhejiang Yilong New Material Co ltd
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds

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Abstract

The invention relates to a preparation process of isooctyl acrylate, which comprises the following steps of 1: adding a polymerization inhibitor, acrylic acid, isooctanol and a water-soluble catalyst into an esterification reaction kettle in sequence, stirring, and carrying out temperature and pressure control reaction to obtain a crude product; step 2: the liquid material on the water layer in the crude product flows to a cooling kettle, and the cooling kettle is cooled to obtain a cooling material by using the generated water recovered by the water regeneration subsystem as a cooling medium; and step 3: transferring the cooling material into a washing tower, washing by using the generated water recovered by the water regeneration subsystem as a washing water source to obtain a washing material, wherein the washing wastewater flows to a catalyst recovery device for catalyst recovery and water body supplement in the water regeneration subsystem; and 4, step 4: transferring the washing material to a light component removing device to remove light components to obtain a light component removing material; and 5: and transferring the light material to a weight removing device, and collecting in an isooctyl acrylate storage tank. The process has the effects of fully utilizing the synthetic raw materials, improving the utilization rate of the synthetic raw materials and meeting the environmental protection requirement.

Description

Preparation process of isooctyl acrylate
Technical Field
The invention relates to the field of acrylate synthesis equipment, in particular to a preparation process of isooctyl acrylate.
Background
The acrylate has the characteristics of good coating gloss and color retention, heat resistance, weather resistance, ageing resistance, strong adhesive force, water resistance, acid and alkali resistance, stain resistance and environmental friendliness, is widely applied to the paint and adhesive industry, the pressure-sensitive adhesive industry and the building industry, is used for a cement modifier and a building sealant in the building field, and is also widely applied to the fields of automobile interior decoration, electronic elements, color enlarging printing, electrical insulation, removable adhesive tapes and the like. The isooctyl acrylate is formed by esterification reaction of acrylic acid and isooctanol under the action of a catalyst, corresponding tail gas can be generated in the reaction process, the main components in the tail gas comprise volatilized acrylic acid and isooctanol, and gaseous acrylic acid and isooctanol are inhaled into human bodies to cause respiratory diseases, so that the tail gas generated by the industrial production of the isooctyl acrylate belongs to forbidden discharge substances and can be discharged into the atmosphere only when being purified to reach the ring discharge standard; and water is generated in the reaction process of the acrylic acid and the isooctanol, the acrylic acid and the slightly water-soluble isooctanol are dissolved in the generated water, so that the generated water cannot be directly discharged into the environment, and the generated water can be discharged to a sewage pipeline only after being subjected to water treatment.
Publication No. CN100395007C discloses an acrylic acid waste gas treatment process, which is suitable for treating acrylic acid waste gas discharged by an acrylic acid device. The acrylic acid waste gas is treated by adopting a catalytic oxidation process, the acrylic acid waste gas is mixed with required air, then the mixture is heated by a waste gas heater and then enters a catalytic reactor for catalytic oxidation reaction, harmful volatile organic compounds are converted into carbon dioxide and water, and then the carbon dioxide and water enter a steam superheater and a waste gas heater for recovering heat and then are discharged into a chimney.
Notice No. CN203360233U discloses a sewage treatment device, including the septic tank, septic tank and anaerobic digestion pond communicate each other, be equipped with the elastic packing layer in the anaerobic digestion pond, anaerobic digestion pond and biological filter are linked together, be equipped with the haydite layer in the biological filter, biological filter and sand filter are linked together, by high to low first sand filtering layer, first filter plate, second sand filtering layer, second filter plate, third sand filtering layer and the third filter plate of being equipped with in proper order in the sand filter, the sand filter is linked together with the clean water basin, the clean water basin is equipped with the outlet pipe, be equipped with the ultraviolet ray disinfection ware that is used for disinfecting the fungus that disappears on the outlet pipe.
The above prior art solutions have the following drawbacks: in the prior art, acrylic acid and isooctyl alcohol in tail gas are catalytically decomposed into carbon dioxide and water by catalytic oxidation; although the problems of tail gas and sewage are solved to a certain extent by adopting the waste water produced by the sewage treatment equipment, in the industrial production, the acrylic acid in the tail gas and the waste water has recycling value as a synthetic raw material, the pollutants in the waste water are single, the waste water after the acrylic acid is removed can be used for cleaning a water source of the synthetic equipment, and the problems of low utilization rate of the synthetic raw material and large material consumption exist by adopting the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a synthesis system utilizing isooctyl acrylate, which can fully utilize synthesis raw materials, reduce the loss of the synthesis raw materials, meet the environmental protection requirement, recycle reaction generated water, reduce the consumption of added water resources, improve the utilization rate of the water resources and save water.
The invention aims to be realized by the following technical scheme: a preparation process utilizing isooctyl acrylate comprises the following steps:
step 1: sequentially adding a polymerization inhibitor, acrylic acid and isooctanol into an esterification reaction kettle, stirring, adding a water-soluble catalyst, stirring, and carrying out temperature and pressure control reaction for 5-6 hours to obtain a crude product;
step 2: conveying a water layer in the crude product to a water regeneration subsystem for recycling, allowing a liquid material on the water layer in the crude product to flow to a cooling kettle for cooling, taking generated water recycled by the water regeneration subsystem as a cooling medium, and cooling for 1-2 hours to obtain a cooled material;
and step 3: introducing the cooling material into a washing tower, washing for 2-3 hours by using the generated water recovered by the water regeneration subsystem as a washing water source to obtain a washing material, wherein the washing wastewater flows to a catalyst recovery device for catalyst recovery and water body supplement in the water regeneration subsystem;
and 4, step 4: introducing the washing material into a light component removal device, adding a polymerization inhibitor of isooctyl acrylate into the light component removal device, wherein the pressure of the light component removal device is-95.0 Kpa to-99.5 Kpa, the temperature is 130 ℃ to 145 ℃, the light component removal time is 2-4 hours, and removing light components to obtain a light component removal material;
and 5: introducing the light weight removal material into a weight removal device, adding a polymerization inhibitor of isooctyl acrylate into the weight removal device, wherein the pressure of the weight removal device is-95.0 Kpa to-99.5 Kpa, the temperature is 130-150 ℃, the weight removal time is 2-4 hours, and obtaining a target product isooctyl acrylate which is collected in an isooctyl acrylate storage tank;
waste gas generated by the esterification reaction kettle, the cooling kettle, the washing tower and the water regeneration subsystem is collected in the tail gas treatment subsystem, the generated water in the water regeneration subsystem can be used as an extraction water source of the tail gas treatment subsystem, and water separated by the tail gas treatment subsystem can be supplemented to the water regeneration subsystem; the material extracted by the tail gas treatment subsystem can be used as a synthetic raw material of isooctyl acrylate. .
By adopting the technical scheme, the reaction generated water is extracted and recovered through the water regeneration subsystem to generate water and acrylic acid, the recovered generated water can be used for cooling a cooling medium of the kettle and a washing water source of the washing tower, the cooling medium of the cooling kettle can be recovered in the water regeneration subsystem after heat exchange and washing materials of the water source enter the catalyst recovery device, the catalyst is recovered, and the water is evaporated and collected in the water regeneration subsystem, so that the consumption of external water resources is reduced for the water, the reaction generated water is recycled, the utilization rate of the water resources is improved, and the water is saved; for the synthetic raw materials, the acrylic acid in the wastewater is extracted and reused, the synthetic raw materials are fully utilized, the utilization rate of the synthetic raw materials is improved, the loss of the synthetic raw materials is reduced, and the synthetic raw materials meet the requirement of environmental protection; meanwhile, the tail gas treatment subsystem is utilized, the water body of the water regeneration subsystem is used as a water source, after the acrylic acid which can be recycled in the waste gas is extracted, the water layer is recovered in the water regeneration subsystem, the extracted acrylic acid can be used as a synthetic raw material, the water is further generated by cyclic utilization reaction, and the utilization rate of the synthetic raw material is improved.
The present invention in a preferred example may be further configured to: the step 1: esterification synthesis is carried out to prepare a crude product;
step 1.1: sequentially adding a polymerization inhibitor, acrylic acid and isooctyl alcohol into an esterification reaction kettle, stirring, adding a water-soluble catalyst, and continuously stirring;
step 1.2: vacuumizing to-38.0 Kpa to-43.0 Kpa, reacting at 88.0-92.0 ℃ for 0.8-1.2 hours;
step 1.3: vacuumizing to-53.0 Kpa to-58.0 Kpa, reacting at 95.0-97.5 ℃ for 0.8-1.2 hours;
step 1.4: vacuumizing to-70.0 Kpa to-72.5 Kpa, reacting at 103.0-107.0 ℃ for 0.8-1.2 hours;
step 1.5: vacuumizing to-77.5 Kpa to-82.5 Kpa, reacting at 110.0-115.0 deg.C for 2.0-3.0 hr.
By adopting the technical scheme, the heat energy released by the esterification reaction can be controlled, the condition that the temperature of the system is increased too fast due to the heat release of the esterification is avoided, the reaction temperature is controlled, the esterification rate of acrylic acid and isooctyl ester is ensured, the reaction safety is improved, and the utilization rate of materials is improved; the good temperature control is improved, the esterification reactant isooctyl acrylate is prevented from generating polyester, and the yield of the target product is improved.
The present invention in a preferred example may be further configured to: the water regeneration subsystem comprises a water recovery tower communicated with the esterification reaction kettle, a generated water recovery tank communicated with the water recovery tower and communicated with the washing tower, an extraction layer collecting tank communicated with the water recovery tower and communicated with the esterification reaction kettle, an extractant storage tank communicated with the water recovery tower, a condensation pool communicated with the upper part of a jacket layer of the cooling kettle, a mixing mechanism arranged in the water recovery tower and used for mixing an extractant and generated water, and a water collecting mechanism communicated with the bottom of the side wall of the water recovery tower, wherein the generated water recovery tank is communicated with the lower part of the jacket layer of the cooling kettle; the condensation tank is communicated with the generated water recovery tank; the catalyst recovery device is communicated with the esterification reaction kettle; the condensation tank is communicated with the catalyst recovery device; the side wall of the upper part of the water recovery tower is communicated with a generated water inlet pipe used for transferring the generated water in the esterification reaction kettle into the water recovery tower; the side wall of the lower part of the water recovery tower is communicated with an extractant inlet pipe used for transferring the extractant in the extractant storage tank into the water recovery tower.
Through adopting above-mentioned technical scheme, the first flow channel of first reposition of redundant personnel makes the liquid material reposition of redundant personnel, and the second flow channel of the adjacent second reposition of redundant personnel in first reposition of redundant personnel below collects, through liquid material reposition of redundant personnel, collects many times for extractant and formation water mix fully, have improved the extraction efficiency of extractant to the acrylic acid of aquatic and slightly soluble isooctanol, have realized water purification, make full use of acrylic acid and isooctanol reduce the material loss, promote resource utilization.
The present invention in a preferred example may be further configured to: the tail gas treatment subsystem comprises a tail gas storage tank, a tail gas absorption tower, a waste gas conveying pipe and a nitrogen generator, wherein the tail gas storage tank is communicated with the esterification reaction kettle, the cooling kettle, the washing tower and the water recovery tower; a water absorption chamber communicated with the condensation tank, a spraying absorption chamber communicated with the water absorption chamber and a terminal absorption chamber communicated with the spraying absorption chamber are formed in the tail gas absorption tower from top to bottom; the spraying absorption chamber is communicated with a spraying mechanism which extracts water in the water absorption chamber to spray and absorb tail gas in the spraying absorption chamber; a purification mechanism for ensuring the quality of the treated tail gas is arranged in the terminal absorption chamber; the water absorption chamber is communicated with a recovery device; the recovery device is communicated with the esterification reaction kettle.
By adopting the technical scheme, the nitrogen generating device generates nitrogen to protect acrylic acid in the tail gas, the tail gas mixed with the nitrogen firstly enters the water absorption chamber, and the water body of the water absorption chamber dissolves and absorbs the acrylic acid and isooctanol in the tail gas for recycling; the gas passing through the water absorption chamber enters the spraying absorption chamber, the spraying mechanism extracts water in the water absorption chamber to spray and absorb the gas in the spraying absorption chamber, the content of acrylic acid and isooctanol in tail gas is further reduced, and the spraying water flows back to the water absorption chamber; the gas passing through the spraying absorption chamber enters the terminal absorption chamber, and the purification mechanism further adsorbs residual trace pollutants, so that the quality of the discharged gas is ensured, and the environmental pollution is avoided; the water body that has absorbed acrylic acid and isooctanol in the water absorption chamber gets into recovery unit, with the water layer, has extracted the extraction layer separation of acrylic acid and isooctanol, carries out the reuse to acrylic acid and isooctanol, has promoted the utilization ratio to acrylic acid and isooctanol in the tail gas, reduces the material consumption of the resources, has improved resource utilization.
The present invention in a preferred example may be further configured to: the washing tower comprises a washing tower main body, a plurality of material mixing plates fixedly connected to the inner wall of the washing tower main body, a plurality of material mixing holes formed in the material mixing plates, a material passing pipe communicated with the lower portion of the side wall of the washing tower and communicated with the cooling kettle, a second extraction pump communicated with the material passing pipe, a material discharging pipe communicated with the bottom of the washing tower and a stirring mechanism arranged on the washing tower main body, wherein the intervals between the adjacent material mixing plates are equal; the mixing holes penetrate through the upper surface and the lower surface of the mixing plate; the stirring mechanism comprises a driving motor fixedly connected to the top of the washing tower main body, a stirring rod fixedly connected to an output shaft of the driving motor, and a plurality of stirrers fixedly connected to the circumference of the stirring rod, wherein the stirring rod penetrates through the material mixing plate and is rotatably connected with the material mixing plate; the stirrer is positioned between the adjacent mixing plates; the stirrer comprises a fixed ring fixedly connected with the circumference of the stirring rod and a plurality of stirring blades fixedly connected with the circumference of the fixed ring; the stirring blade penetrates through the surface and is provided with a plurality of through holes; the stirring blades are uniformly arranged around the central axis of the fixing ring.
By adopting the technical scheme, when the generated water and the materials flow in opposite directions when passing through the through hole and the liquid materials flow between the mixing plates, the rotating stirring blades stir the generated water and the materials, so that the generated water and the materials do irregular motion, and the generated water and the materials are in full contact to more effectively remove the water-soluble catalyst in the materials.
The present invention in a preferred example may be further configured to: in step 3 the catalyst recovery device comprises a multi-effect evaporator communicated with the discharge pipe, a condensation pipe communicated with the multi-effect evaporator and used for condensing steam, and a catalyst recovery tank communicated with the multi-effect evaporator, wherein one end of the condensation pipe is communicated with the multi-effect evaporator, the other end of the condensation pipe is communicated with the condensation pool, the condensation pipe is arranged in the condensation pool, and the circumferential direction of the condensation pipe is surrounded by a water body.
By adopting the technical scheme, the water body dissolved with the catalyst is guided into the multi-effect evaporator by the discharge pipe, the multi-effect evaporator concentrates the water body, most of water is evaporated to obtain a catalyst concentrated solution, the catalyst concentrated solution is transferred to the catalyst recovery tank, and when the isooctyl acrylate is synthesized, the catalyst concentrated solution in the catalyst recovery tank is transferred to the esterification reaction kettle, so that the catalyst is recycled, and the consumption of the catalyst is reduced; meanwhile, evaporated water is collected in the condensation tank, and can be used for cooling the cooling kettle and cleaning cooling materials after being radiated in the open air, so that the water consumption is reduced, and water resources are saved.
The present invention in a preferred example may be further configured to: in the step 4, the light component removing device comprises a light component removing tower, a first inlet pipe communicated with the top of the light component removing tower and communicated with a discharge pipe, a plurality of first mixing plates fixedly connected to the inner wall of the light component removing tower and having the same structure as the mixing plates, a first return pipe communicated with the bottom of the light component removing tower, a first detection pipe sequentially communicated with the first return pipe along the material flowing direction, a first storage tank, a first centrifugal pump communicated with the first return pipe and the first storage tank, a first constant boiling tank communicated with one end of the return pipe, which faces away from the light component removing tower, a first return pipe communicated with the top of the first constant boiling tank, a first condenser communicated with the top of the light component removing tower and a light component collecting tank communicated with the first condenser, wherein the light component collecting tank is communicated with the top of the light component removing tower; the communication position of the first gas return pipe and the light component removal tower is positioned in the middle of the light component removal tower and between the adjacent first mixing plates; the light component removal tower, the first condenser and the light component collection tank are communicated through a first communication pipe; the bottom surface of the first constant boiling tank and the bottom surface of the light component removal tower are positioned in the same plane, and the height of the first constant boiling tank is lower than that of the light component removal tower.
By adopting the technical scheme, the continuous production can be carried out, the heating is carried out until the constant boiling point of the isooctyl acrylate and the isooctyl alcohol, and the isooctyl acrylate and the isooctyl alcohol in the material are removed by distillation; and meanwhile, the isooctyl acrylate and the isooctyl alcohol are collected, so that the isooctyl acrylate and the isooctyl alcohol can be recycled conveniently at the later stage, and the resource utilization rate is improved.
The present invention in a preferred example may be further configured to: the weight removing device in the step 5 comprises a weight removing tower communicated with the first storage tank, a second inlet pipe communicated between the weight removing tower and the first storage tank, a plurality of second mixing plates fixedly connected to the inner wall of the weight removing tower and having the same structure as the mixing plates, a second return pipe communicated with the bottom of the weight removing tower, a second detection pipe sequentially communicated with the second return pipe along the material flowing direction, a second storage tank, a second centrifugal pump communicated with the second return pipe and the second storage tank, and a second constant boiling tank communicated with one end of the second return pipe, which is opposite to the weight removing tower; the second air return pipe is communicated with the top of the second constant boiling tank, the second condenser is communicated with the top of the de-weighting tower, and the isooctyl acrylate collecting tank is communicated with the second condenser and is communicated with the top of the de-weighting tower; the second air return pipe is communicated with the heavy component removal tower, is positioned in the middle of the heavy component removal tower and is positioned between the adjacent second mixing plates; the isooctyl acrylate collection tank is communicated with the isooctyl acrylate storage tank; the de-weighting tower, the second condenser and the isooctyl acrylate collecting tank are communicated through a second communicating pipe; the bottom surface of the second constant boiling tank and the bottom surface of the heavy component removal tower are positioned in the same plane, and the height of the second constant boiling tank is lower than that of the heavy component removal tower.
By adopting the technical scheme, continuous production can be carried out, heavy components in materials are effectively removed, and pure isooctyl acrylate is obtained; meanwhile, the heavy components are collected, so that the heavy components can be reprocessed conveniently in the later period, secondary utilization is realized, and the resource utilization rate is improved.
The present invention in a preferred example may be further configured to: further comprising the step 6: and (3) introducing the heavy components separated in the step (5) into a cracking device, wherein the pressure of the cracking device is-95.0 Kpa to-99.5 Kpa, the temperature is 155-165 ℃, and the cracking time is 2-4 hours, so as to obtain a recyclable cracking substance.
By adopting the technical scheme, the recyclable isooctyl acrylate, acrylic acid and isooctyl alcohol are obtained by cracking the heavy components, the reutilization rate of the heavy components is improved, and the utilization rate of the whole resources is improved.
The present invention in a preferred example may be further configured to: the cracking device in the step 6 comprises a cracking tower communicated with the weight removal device, a third inlet pipe communicated between the cracking tower and the second storage tank, a plurality of third mixing plates fixedly connected to the inner wall of the cracking tower and having the same structure as the mixing plates, a third return pipe communicated with the bottom of the cracking tower, a third detection pipe sequentially communicated with the third return pipe along the material flowing direction, a residue storage tank, a third centrifugal pump communicated with the third return pipe and the third storage tank, a third constant boiling tank communicated with one end of the third return pipe, which is opposite to the cracking tower, a third return pipe communicated with the top of the third constant boiling tank, a third condenser communicated with the top of the cracking tower and a cracking component collection tank communicated with the third condenser, wherein the third return pipe is communicated with the cracking tower at the middle part of the cracking tower and is positioned between the adjacent third mixing plates; the cracking tower, the third condenser and the cracking component collecting tank are communicated through a third communicating pipe; the bottom surface of the third constant boiling tank and the bottom surface of the cracking tower are positioned in the same plane, and the height of the third constant boiling tank is lower than that of the cracking tower.
By adopting the technical scheme, continuous production can be carried out, and the cracking efficiency of the heavy components is improved; the heavy component is effectively cracked into the recyclable isooctyl acrylate, acrylic acid and isooctanol, the isooctyl acrylate, the acrylic acid and the isooctanol are recycled, the utilization rate of the heavy component is improved, the synthetic raw materials are saved, and the resource utilization rate is improved.
In summary, the invention has the following beneficial technical effects:
1. through the steps of 1: adding a polymerization inhibitor, acrylic acid, isooctanol and a water-soluble catalyst into an esterification reaction kettle in sequence, stirring, and carrying out temperature and pressure control reaction to obtain a crude product; step 2: the liquid material on the water layer in the crude product flows to a cooling kettle, and the cooling kettle is cooled to obtain a cooling material by using the generated water recovered by the water regeneration subsystem as a cooling medium; and step 3: transferring the cooling material into a washing tower, washing by using the generated water recovered by the water regeneration subsystem as a washing water source to obtain a washing material, wherein the washing wastewater flows to a catalyst recovery device for catalyst recovery and water body supplement in the water regeneration subsystem; and 4, step 4: transferring the washing material to a light component removing device to remove light components to obtain a light component removing material; and 5: the invention has the advantages of fully utilizing the synthetic raw materials, reducing the loss of the synthetic raw materials, improving the utilization rate of the synthetic raw materials and meeting the environmental protection requirement.
2. Through the esterification reaction kettle, the cooling kettle, the washing tower, the catalyst recovery device, the light removal device, the heavy removal device, the isooctyl acrylate storage tank, the cracking device, the tail gas treatment subsystem and the water regeneration subsystem, the invention fully utilizes the synthetic raw materials, reduces the loss of the synthetic raw materials, improves the utilization rate of the synthetic raw materials, meets the environmental protection requirement, recycles the reaction generated water, reduces the consumption of the added water resource, improves the utilization rate of the water resource and saves the water.
3. The tail gas is absorbed by a tail gas absorption tower, a tail gas pipe, a water absorption chamber, a spraying absorption chamber, a terminal absorption chamber, a nitrogen generation device, a spraying mechanism, a purification mechanism and a recovery device; the invention can recycle the tail gas, improve the utilization rate of the acrylic acid and the isooctanol and reduce the material consumption.
4. The system comprises a water regeneration subsystem, an esterification reaction kettle, a water recovery tower, a generated water recovery tank, an extraction layer collection tank, an extractant storage tank, a cooling kettle jacket layer, a condensation tank, a mixing mechanism, a generated water inlet pipe and an extractant inlet pipe.
Drawings
FIG. 1 is a diagram of the layout of the synthesis equipment required to carry out the process for the preparation of isooctyl acrylate of the present invention.
FIG. 2 is a diagram showing the connection structure of the water regeneration subsystem with the esterification reaction kettle, the cooling kettle and the washing tower;
FIG. 3 is a schematic diagram of the water regeneration subsystem;
FIG. 4 is a schematic structural view of the first flow divider plate;
FIG. 5 is a schematic structural view of the second splitter plate;
FIG. 6 is a schematic diagram of a scrubber;
FIG. 7 is an enlarged view of a portion of FIG. 6 at A;
FIG. 8 is a schematic view of the structure of the lightness-removing apparatus;
FIG. 9 is a schematic view of the structure of the weight removing device;
FIG. 10 is a schematic diagram of the structure of the cracking device;
FIG. 11 is a structural representation of an exhaust gas treatment subsystem;
FIG. 12 is a schematic view of a tail gas absorption tower;
fig. 13 is a partial enlarged view at B in fig. 12;
FIG. 14 is a schematic view of the structure of the composite adsorbent;
fig. 15 is a schematic view of the structure of the composite web.
In the figure, 1, an esterification reaction kettle; 11. cooling the kettle; 12. a washing tower; 121. a material passing pipe; 122. a second extraction pump; 123. a washing tower main body; 124. a material mixing plate; 125. a mixing hole; 126. a discharge pipe; 1261. discharging and pipe dividing; 127. a stirring mechanism; 1271. a drive motor; 1272. a stirring rod; 1273. a stirrer; 1274. a fixing ring; 1275. a stirring blade; 1276. a through hole; 128. a return pipe; 13. a catalyst recovery unit; 131. a multi-effect evaporator; 132. a condenser tube; 133. a catalyst recovery tank; 14. a light component removal device; 141. a light component removal tower; 142. a first inlet pipe; 143. a first mixing plate; 144. a first return pipe; 1441. a first detection tube; 1442. a first storage tank; 1443. a first centrifugal pump; 145. a first constant boiling tank; 1451. a first gas return pipe; 146. a first communication pipe; 147. a first condenser; 148. a light component collection tank; 149. a first agent storage tank; 15. a de-weighting device; 151. a de-weighting tower; 152. a second inlet pipe; 153. a second mixing plate; 154. a second return pipe; 1541. a second detection tube; 1542. a second storage tank; 1543. a second centrifugal pump; 155. a second constant boiling tank; 1551. a second muffler; 156. a second communicating pipe; 157. a second condenser; 158. a iso-octyl acrylate collection tank; 1581. a detection tube; 159. a second agent storage tank; 1590. a third agent storage tank; 16. an isooctyl acrylate storage tank; 17. a cracking unit; 171. a cracking tower; 172. a third inlet pipe; 173. a third mixing plate; 174. a third return pipe; 1741. a third detection tube; 1742. a residue storage tank; 1743. a third centrifugal pump; 175. a third constant boiling tank; 1751. a third air return pipe; 176. a third communicating pipe; 177. a third condenser; 178. a cracked component collection tank; 179. a cracked component storage tank; 2. a water regeneration subsystem; 21. a water recovery tower; 211. generating a water inlet pipe; 212. an extractant inlet pipe; 22. generating a water recovery tank; 221. a washing water addition pipe; 23. an extraction layer collection tank; 231. an extractant recovery tube; 24. an extractant storage tank; 25. a condensation tank; 26. a mixing mechanism; 261. a first splitter plate; 2611. a first manifold body; 2612. a connecting strip; 2613. a first flow channel; 262. a second splitter plate; 2621. a second manifold body; 2622. a second flow channel; 27. a water collection mechanism; 271. a first water outlet pipe; 272. a second water outlet pipe; 273. a U-shaped pipe; 274. extracting an interface line; 275. connecting pipes; 3. a tail gas treatment subsystem; 30. a tail gas storage tank; 31. a tail gas absorption tower; 311. a sixth partition plate; 32. an exhaust gas delivery pipe; 321. a nitrogen generator; 33. a stirring device; 331. driving a motor; 332. a stirring rod member; 333. a pitched blade stirring paddle; 4. a second separator; 40. a first separator; 401. a third partition plate; 402. a fourth separator; 403. a vent hole; 41. a breather pipe; 42. a sandwich cavity; 43. a fifth partition plate; 5. a water absorption chamber; 51. a spray water recovery pipe; 6. a spray absorption chamber; 60. a spraying mechanism; 601. a first spray header; 602. a water supply pipe; 603. a water pump; 604. a first spray branch pipe; 605. a second spray branch pipe; 606. a water supply branch pipe; 61. a first spray chamber; 62. a second spray chamber; 63. a third spray chamber; 7. a terminal absorption chamber; 71. a first terminal absorption chamber; 72. a second terminal absorption chamber; 73. a third terminal absorption chamber; 74. a composite adsorbent; 741. a composite adsorbent body; 742. a composite web; 7421. warp threads; 7422. a weft; 7423. polyacrylonitrile-based activated carbon fiber; 7424. polyamide fibers; 743. a zeolite plate; 744. bamboo charcoal fiber felt; 745. air diffusing holes; 75. a chimney; 8. a purification mechanism; 9. a recovery device; 90. an extraction tank; 901. a stirring assembly; 902. a feed pipe; 903. an extractant inlet pipe; 904. a discharge pipe; 9041. a water discharging pipe; 9042. and a discharge main pipe.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples.
Referring to fig. 1, the synthesis equipment required for implementing the preparation process of isooctyl acrylate of the invention comprises an esterification reaction kettle 1, wherein the esterification reaction kettle 1 is communicated with a water regeneration subsystem 2 and a tail gas treatment subsystem 3; the esterification reaction kettle 1 is communicated with a cooling kettle 11, and the cooling kettle 11 is communicated with the water regeneration subsystem 2; the cooling kettle 11 is communicated with a washing tower 12, and the washing tower 12 is communicated with the water regeneration subsystem 2; the washing tower 12 is communicated with a lightness-removing device 14; the washing tower 12 is communicated with a catalyst recovery device 13; the catalyst recovery device 13 is communicated with the washing tower 12, the esterification reaction kettle 1 and the water regeneration subsystem 2; the light weight removing device 14 is communicated with a weight removing device 15; the weight removal device 15 is communicated with an isooctyl acrylate storage tank 16; the de-weighting device 15 is communicated with a cracking device 17 for recovering heavy components generated by the reaction.
Referring to fig. 2, the water regeneration subsystem 2 includes a water recovery tower 21 communicated with the esterification reaction kettle 1, the water recovery tower 21 is communicated with a generated water recovery tank 22, and the generated water recovery tank 22 is communicated with the washing tower 12 and used as a washing water source cleaning cooling material of the washing tower 12. The water recovery tower 21 is communicated with an extraction layer collecting tank 23 for recovering extraction layer materials, the extraction layer collecting tank 23 is communicated with the esterification reaction kettle 1, and the materials in the extraction layer collecting tank 23 can be used as synthetic raw materials of isooctyl acrylate, so that the material consumption is reduced. The water recovery tower 21 is communicated with an extracting agent storage tank 24, isooctanol stored in the extracting agent storage tank 24 is used for extracting acrylic acid dissolved in generated water, and the isooctanol is a synthetic raw material of isooctyl acrylate and can be used as the synthetic raw material, so that the material consumption is further reduced, and repeated purification is avoided. The generated water recovery tank 22 is communicated with the lower part of the jacket layer of the cooling kettle 11, and cooling medium is input into the jacket layer; the upper part of the jacket layer of the cooling kettle 11 is communicated with a condensation tank 25 for collecting the water body after heat exchange through the jacket layer, the condensation tank 25 is communicated with the generated water recovery tank 22, and the water body flowing into the condensation tank 25 is supplemented into the generated water recovery tank 22, so that the generated water body is recycled, the consumption of water resources is reduced, the utilization rate of the generated water is improved, and the process has good environmental protection performance.
Referring to fig. 2, a product water inlet pipe 211 for transferring the product water in the esterification reaction tank 1 into the water recovery tower 21 is connected to the upper side wall of the water recovery tower 21, and a centrifugal pump may be installed in the product water inlet pipe 211 to pump the product water into the upper portion of the water recovery tower 21. The sidewall of the lower part of the water recovery tower 21 is communicated with an extracting agent inlet pipe 212 for transferring the extracting agent isooctanol in the extracting agent storage tank 24 into the water recovery tower 21, and a centrifugal pump can be arranged on the extracting agent inlet pipe 212, and the isooctanol is pumped into the water recovery tower 21 by the centrifugal pump.
Referring to fig. 3, in order to ensure the effect of extracting acrylic acid dissolved in water by isooctanol, a mixing mechanism 26 for mixing an extracting agent and produced water is provided in the water recovery tower 21. The mixing mechanism 26 comprises a plurality of first splitter plates 261 fixedly connected to the inner wall of the water recovery tower 21 and a plurality of second splitter plates 262 fixedly connected to the inner wall of the water recovery tower 21 and located in the middle of the first splitter plates 261, and the distances between adjacent second splitter plates 262 are equal; adjacent first flow distribution plates 261 are equally spaced.
Referring to fig. 3, the junction of the produced water inlet pipe 211 and the water recovery tower 21 is located at the upper portion of the first splitter plate 261 having the highest vertical distance from the bottom of the water recovery tower 21; the junction of the extractant inlet pipe 212 and the water recovery column 21 is located at the lower portion of the first diversion plate 261 having the lowest vertical distance from the bottom of the water recovery column 21. Referring to fig. 4, the first flow dividing plate 261 includes a first flow dividing plate main body 2611, the first flow dividing plate main body 2611 is integrally formed with a plurality of connecting strips 2612 in the circumferential direction, the connecting strips 2612 uniformly surround the central axis of the first flow dividing plate main body 2611, the connecting strips 2612 are located in the same plane, and the connecting strips 2612 are welded to the inner wall of the water recovery tower 21, so that the first flow dividing plate 261 is fixed to the inner wall of the water recovery tower 21. A first flow channel 2613 having a vertical projection in a ring shape is formed between the first flow dividing plate body 2611 and the inner wall of the water recovery tower 21, and the extractant and the generated water are mixed while passing through the first flow channel 2613, so that the extractant extracts acrylic acid in the generated water. Referring to fig. 5, the second splitter plate 262 includes a second splitter plate main body 2621, a second flow channel 2622 is formed through a center of the second splitter plate main body 2621 along a central axis of the second splitter plate main body 2621, and a vertical projection of the second flow channel 2622 is located at the center of the second splitter plate main body 2621 and is rectangular with a length-to-width ratio of 1: 15. The liquid materials which are shunted by the first flow channel 2613 can be converged and flow through the second flow channel 2622, so that the extracting agent and the generated water are more fully mixed, the acrylic acid in the generated water is extracted by the extracting agent more quickly and effectively, and the quality of the generated water after the acrylic acid is extracted by the extracting agent is ensured.
Referring to fig. 3 and fig. 2, the bottom of the sidewall of the water recovery tower 21 is communicated with a water collecting mechanism 27, which can quickly collect the water purified by extraction, thereby realizing continuous operation. The water collecting mechanism 27 comprises a first water outlet pipe 271 communicated with the bottom of the side wall of the water recovery tower 21, a second water outlet pipe 272 communicated with the lower part of the side wall of the generated water recovery tank 22, and a U-shaped pipe 273 with one end communicated with the first water outlet pipe 271 and the other end communicated with the second water outlet pipe 272, wherein the U-shaped pipe 273 is in an inverted U shape and is communicated with the first water outlet pipe271. The second water outlet pipe 272 is communicated, the middle part of the U-shaped pipe 273 is communicated with a connecting pipe 275 communicated with the top of the water recovery tower 21, and the connecting pipe 275 is used for balancing the air pressure in the water recovery tower 21. The height H of the U-shaped pipe 273 of the extraction interface line 274 formed in the water recovery tower 213Depending on the vertical distance H from the bottom of the water recovery column 21 to the extraction interface line 2741And the vertical distance H from the extraction interface line 274 to the upper surface of the extraction layer2Height H of U-shaped tube 2733Water (W)H1Extract (Cuiyu)H2Water (W)Where ρ isWater (W)Density of the aqueous layer; rhoExtract (Cuiyu)Density of the extraction layer; when the interface of the extraction layer and the water layer was flush with the extraction interface line 274, the vertical distance from the upper surface of the extraction layer to the lowest position of the product water inlet pipe 211 was 0.30 m. In order to collect the extraction layer, the extraction layer collection tank 23 is communicated with an extraction agent recovery pipe 231, and the lowest part of the communication port of the extraction agent recovery pipe 231 and the water recovery tower 21 is flush with the extraction interface line 274.
Referring to fig. 3, in conjunction with fig. 2, the valve on the extracting agent recycling pipe 231 is in a closed state, so that the extracting layer does not flow to the extracting layer collecting tank 23, and the water collecting mechanism 27 is in a communicated state; adding the water generated in the esterification reaction kettle 1 into the water recovery tower 21 from the upper part of the water recovery tower 21 through a generated water inlet pipe 211; adding the extractant in the extractant storage tank 24 into the water recovery tower 21 from the lower part of the water recovery tower 21 through an extractant inlet pipe 212, and controlling the adding amount of the extractant and the water recovery tower 21 so that an extraction interface formed by the extractant and the water recovery tower is flush with an extraction interface line 274; closing a valve of the extracting agent inlet pipe 212, stopping adding the extracting agent, adding the reaction product water in the esterification reaction kettle 1 into the upper part of the water recovery tower 21, when the liquid level of the upper surface of the extracting layer rises due to the addition of the product water, ensuring that the vertical distance from the upper surface of the extracting layer to the maximum position of the extracting agent inlet pipe 212 is less than 0.30m, pressing the water body of the water layer into the product water recovery tank 22 under the action of liquid pressure, ensuring that the product water which just enters the water recovery tower 21 is positioned at the upper part of the water recovery tower 21 and is contacted with the extracting layer, ensuring that the water body of the product water penetrates the extracting layer to enter the water layer under the action of density difference, extracting the acrylic acid in the product water into the extracting layer, realizing continuous purification treatment of the product water, obtaining the usable water body and storing the usable water body.
Referring to fig. 3 and fig. 2, when the extraction layer in the water recovery tower 21 needs to be collected, the addition of the extractant and the generated water to the water recovery tower 21 is stopped, the water collection mechanism 27 is closed, the extractant recovery pipe 231 is opened, the extraction layer is collected in the extraction layer collection tank 23, and the liquid material in the extraction layer collection tank 23 can be conveyed to the esterification reaction kettle 1 to be reused as a synthetic raw material, so that the utilization rate of acrylic acid is improved.
Referring to fig. 3, in conjunction with fig. 2, a washing water addition pipe 221 is connected to the lower portion of the side wall of the generated water recovery tank 22; the washing water addition pipe 221 has one end connected to the lower part of the side wall of the generated water recovery tank 22 and the other end connected to the upper part of the side wall of the washing tower 12, and the generated water purified in the generated water recovery tank 22 can be transferred to the washing tower 12 by a centrifugal pump to wash the cooled material and remove the water-soluble catalyst.
Referring to fig. 3, in conjunction with fig. 6, the washing tower 12 includes a washing tower main body 123, a plurality of material mixing plates 124 are fixedly connected to an inner wall of the washing tower main body 123, and the distances between adjacent material mixing plates 124 are equal; the material mixing plate 124 penetrates through the upper surface and the lower surface and is provided with a plurality of material mixing holes 125, and the aperture ratio of the material mixing plate 124 is 50%; a material passing pipe 121 is communicated with the lower part of the side wall of the washing tower 12, one end of the material passing pipe 121 is communicated with the lower part of the side wall of the washing tower 12, and the other end of the material passing pipe 121 is communicated with the bottom of the side wall of the cooling kettle 11; the connection position of the material passing pipe 121 and the washing tower main body 123 is positioned at the lower part of the material mixing plate 124 with the lowest vertical distance from the bottom of the washing tower 12, and the connection position of the washing water adding pipe 221 and the washing tower main body 123 is positioned at the upper part of the material mixing plate 124 with the highest vertical distance from the bottom of the washing tower 12; the material passing pipe 121 is fixedly communicated with a second extraction pump 122 for adding the cooling material in the cooling kettle 11 into the washing tower 12. The bottom of the washing tower 12 is communicated with a discharge pipe 126, and a water layer positioned at the lower part of the washing tower 12 can be discharged into the catalyst recovery device 13 through the discharge pipe 126 to recycle the water-soluble catalyst in the water layer; when the water layer at the lower part is drained, the washed material is transferred to the light component removal device 14 for light component removal through a discharge pipe 1261 which is communicated with the upper part of the side wall of the light component removal device 14 on a discharge pipe 126.
Referring to fig. 3 in conjunction with fig. 2, the discharge pipe 126 communicates with the catalyst recovery device 13 to recover and reuse the water-soluble catalyst. Catalyst recovery unit 13 includes the multiple effect evaporimeter 131 with discharging pipe 126 intercommunication, and multiple effect evaporimeter 131 intercommunication has the condenser pipe 132 that is used for the comdenstion water vapour, and condenser pipe one end communicates in multiple effect evaporimeter 131 and the other end communicates in condensate sump 25, and condenser pipe 132 arranges and locates in condensate sump 25, and condenser pipe 132 circumference is surrounded by the water for lower the temperature to the vapour in condenser pipe 132, make its condensation collect in condensate sump 25. The bottom of the multi-effect evaporator 131 is communicated with a catalyst recovery tank 133, the catalyst recovery tank 133 is communicated with the esterification reaction kettle 1, and the water-soluble catalyst solution concentrated by the multi-effect evaporator 131 is collected in the catalyst recovery tank 133 and can be added into the esterification reaction kettle 1 as a synthetic catalyst, so that the using amount of the catalyst is reduced, and the utilization rate of the catalyst is improved.
Referring to fig. 3, in combination with fig. 2, the washing water in the washing tower 12 is evaporated by the multi-effect evaporator 131, and the water in the washing water is changed into steam to be condensed and collected in the condensation tank 25, which can be supplemented to the generated water recovery tank 22, so that the generated water can be recycled; the water-soluble catalyst in the washing water body is retained in the multi-effect evaporator 131, is concentrated due to the evaporation of water, is transferred to the esterification reaction kettle 1 through the catalyst recovery tank 133, can be reused as a synthetic raw material, and improves the resource utilization rate.
Referring to fig. 6, in conjunction with fig. 2, the material cooled by the cooling kettle 11 enters the washing tower 12 through the material passing pipe 121 from the lower portion of the sidewall of the washing tower 12; the generated water enters the washing tower 12 from the upper part of the side wall of the washing tower 12 through the washing water adding pipe 221, and because the density of the cooled materials is less than that of the generated water, the cooled materials move from the lower part of the washing tower 12 to the upper part of the washing tower 12, and the generated water moves from the upper part to the lower part; when the liquid level of the generated water is higher than the lowest vertical distance of the mixing plate 124 at the bottom of the washing tower 12 as the liquid materials of the two materials are added, the cooled materials moving upwards and the generated water are mixed and washed in the mixing holes 125 of the mixing plate 124, and the p-toluenesulfonic acid in the cooled materials is dissolved in the washing water for recycling; along with the continuous addition of the liquid materials, the interface formed by the generated water and the cooled materials moves upwards, and the cooled materials are mixed with the generated water for multiple times through the mixing holes 125 of the plurality of mixing plates 124 in the upward movement process from the lower part of the washing tower 12, so that the water-soluble catalyst in the cooled materials is dissolved in the water more quickly, the catalyst in the cooled materials is effectively removed, and the purity of the cooled materials is ensured.
Referring to fig. 6, in order to reduce the water consumption for washing and increase the utilization rate of water resources, the bottom of the washing tower body 123 is communicated with a return pipe 128, one end of the return pipe 128 is communicated with the bottom of the washing tower body 123 and the other end is communicated with the top of the washing tower body 123, a centrifugal pump can be loaded on the return pipe 128 to pump the water at the bottom of the washing tower body 123 to the top of the washing tower body 123, and the water-soluble catalyst in the cooled material is fully extracted.
Referring to fig. 6, in order to ensure the mixing effect of the generated water and the cooled material, the washing tower main body 123 is provided with a stirring mechanism 127, the stirring mechanism 127 comprises a driving motor 1271 fixedly connected to the top of the washing tower main body 123, and an output shaft of the driving motor 1271 is fixedly connected with a stirring rod 1272; the stirring rod 1272 is fixedly connected with a plurality of stirrers 1273 in the circumferential direction, and the stirring rod 1272 penetrates through the material mixing plate 124 and is rotatably connected with the material mixing plate 124; the agitator 1273 is positioned between adjacent mixer plates 124.
Referring to fig. 6 in conjunction with fig. 7, the agitator 1273 includes a fixing ring 1274 fixedly attached to the circumference of the agitator shaft 1272, the fixing ring 1274 having a plurality of agitator blades 1275 fixedly attached to the circumference; the stirring blades 1275 penetrate through the surface and are provided with a plurality of through holes 1276, and the stirring blades 1275 are uniformly arranged around the central axis of the fixing ring 1274; the stirring blades 1275 have an aperture ratio of 75%, and the water and the materials are stirred to be fully contacted with each other, so that the water-soluble catalyst in the materials is more effectively removed.
Referring to fig. 8, the lightness-removing apparatus 14 includes a lightness-removing column 141, a first storage tank 149 for storing copper N, N-di-N-butyldithiocarbamate is fixedly communicated with the top of the lightness-removing column 141, and the dropping speed of the copper N, N-di-N-butyldithiocarbamate between the first storage tank 149 and the lightness-removing column 141 can be controlled by an electromagnetic valve. The top of the lightness-removing column 141 is communicated with a first inlet pipe 142 communicated with a discharge branch pipe 1261; the inner wall of the lightness-removing tower 141 is fixedly connected with a plurality of first mixing plates 143 with the same structure as the mixing plates 124; the bottom of the lightness-removing tower 141 is communicated with a first return pipe 144, the first return pipe 144 is sequentially communicated with a first detection pipe 1441 for collecting materials in the lightness-removing tower 141 and using the materials for detecting and judging whether the lightness-removing materials are qualified or not and a first storage tank 1442 for storing the qualified materials, a first centrifugal pump 1443 for extracting the qualified materials is communicated between the first return pipe 144 and the first storage tank 1442, and when the mass percentage of isooctyl alcohol in the materials flowing out of the first detection pipe 1441 is lower than 0.1%, the materials are qualified and can be collected in the first storage tank 1442.
Referring to fig. 8, one end of the return pipe 144 is connected to the bottom of the light component removal column 141, the other end is connected to the first constant boiling tank 145, the top of the first constant boiling tank 145 is connected to the first return pipe 1451, and the connection between the first return pipe 1451 and the light component removal column 141 is located in the middle of the light component removal column 141 and between the adjacent first mixing plates 143. The top of the lightness-removing tower 141 is communicated with a first condenser 147, and the first condenser 147 is communicated with a vacuum pump for vacuum pumping; the first condenser 147 is communicated with a light component collecting tank 148, the light component collecting tank 148 is communicated with the light component removing tower 141, and light components in the light component collecting tank 148 are refluxed into the light component removing tower 141 through a centrifugal pump; when the content of isooctanol in the light component collection tank 148 is lower than that of isooctyl acrylate, the amount of light component refluxing to the lightness-removing column 141 is increased, and the amount of the material entering the lightness-removing column 141 through the discharge pipe 126 is reduced. The light component removal column 141, the first condenser 147, and the light component collection tank 148 are communicated through a first communication pipe 146. The bottom surface of first constant boiling tank 145 and the bottom surface of light component removal column 141 are in the same plane and the height of first constant boiling tank 145 is lower than the height of light component removal column 141.
Referring to fig. 8, the vacuum pump is used to evacuate the lightness-removing device 14, heating steam is continuously introduced into the jacket layer formed on the outer wall of the first constant boiling tank 145 to heat the material in the first constant boiling tank 145, the temperature is maintained to the constant boiling point of isooctanol and isooctyl acrylate, isooctanol and acrylic acid in the material are changed into steam, the steam enters the lightness-removing tower 141 through the first air return pipe 1451, the heat energy of a part of the steam is used to heat the material in the lightness-removing tower 141, the other part of the steam enters the first condenser 147 from the first connecting pipe 146 to be condensed, condensed liquid is collected in the light component collecting tank 148 through the first connecting pipe 146, the isooctanol in the material is removed, the isooctanol and the isooctyl acrylate are collected and utilized, and the utilization rate of the whole resource is improved.
Referring to fig. 8, by controlling the material feeding amount in the first feeding pipe 142, the light component reflux amount in the light component collecting tank 148 to the light component removing tower 141 and the condensed material amount in the first condenser 147, the sum of the material feeding amount and the light component reflux amount in the light component removing tower 141 is equal to the condensed material amount, so that the continuous light component removing of the material can be realized, the production efficiency is improved, and the human cost is reduced.
Referring to fig. 9, the de-weighting device 15 includes a de-weighting tower 151 having a top portion communicating with a first storage tank 1442, a second agent tank 159 for storing the high-efficiency substance 705 and a third agent tank 1590 for storing p-hydroxyanisole are fixedly communicated with the top portion of the de-weighting tower 151, and the dropping speed of the high-efficiency substance 705 and the dropping speed of the p-hydroxyanisole can be controlled by electromagnetic valves between the second agent tank 159 and the de-weighting tower 151 and between the third agent tank 1590 and the de-weighting tower 151. The de-weighting tower 151 is communicated with the first storage tank 1442 through the second inlet pipe 152, and the material of the first storage tank 1442 without isooctanol can be transferred to the de-weighting tower 151 for de-weighting operation by installing a centrifugal pump on the second inlet pipe 152.
Referring to fig. 9, a plurality of second mixing plates 153 having the same structure as the mixing plate 124 are fixedly connected to the inner wall of the de-weighting tower 151; the bottom of the de-weighting tower 151 is communicated with a second return pipe 154, the second return pipe 154 is sequentially communicated with a second detection pipe 1541 for collecting materials in the de-weighting tower 151 and detecting and judging whether the de-weighting materials are qualified or not and a second storage tank 1542 for storing the detected qualified materials along the material flowing direction, a second centrifugal pump 1543 for collecting the detected qualified materials is communicated between the second return pipe 154 and the second storage tank 1542, and the isooctyl acrylate content in the materials flowing out of the second detection pipe 1541 is judged to be qualified if the isooctyl acrylate content is lower than 30% and can be collected in the second storage tank 1542.
Referring to fig. 9, one end of the second return pipe 154 is communicated with the bottom of the de-heavy column 151 and the other end is communicated with a second constant boiling tank 155; the top of the second constant boiling tank 155 is communicated with a second air return pipe 1551, and the communication between the second air return pipe 1551 and the de-weighting tower 151 is positioned in the middle of the de-weighting tower 151 and between the adjacent second mixing plates 153. The top of the de-heavy tower 151 is communicated with a second condenser 157, and the second condenser 157 is communicated with a vacuum pump for vacuum pumping; the second condenser 157 is communicated with an isooctyl acrylate collecting tank 158, the isooctyl acrylate collecting tank 158 is communicated with a detection pipe 1581, and the isooctyl acrylate collecting tank 158 is communicated with an isooctyl acrylate storage tank 16. The de-weighting tower 151, the second condenser 157 and the isooctyl acrylate collecting tank 158 are communicated through a second communicating pipe 156. The bottom surface of the second constant boiling tank 155 and the bottom surface of the de-heavy column 151 are in the same plane and the height of the second constant boiling tank 155 is lower than that of the de-heavy column 151.
Referring to fig. 9, an isooctyl acrylate collection tank 158 is communicated with the top of the de-weighting tower 151, isooctyl acrylate of the isooctyl acrylate collection tank 158 is refluxed into the de-weighting tower 151 by a centrifugal pump, and when the isooctyl acrylate content of the isooctyl acrylate collection tank 158 is less than 99.5% and has a large difference from 99.5%, the amount of isooctyl acrylate refluxed into the de-weighting tower 151 is increased; when the isooctyl acrylate content of the isooctyl acrylate collection tank 158 is greater than 99.5%, the isooctyl acrylate from the isooctyl acrylate collection tank 158 is transferred to the isooctyl acrylate storage tank 16.
Referring to fig. 9, the de-weighting device 15 is evacuated to be empty by using a vacuum pump, heating steam is continuously introduced into a jacket layer formed on the outer wall of the second constant boiling tank 155 to heat the material in the second constant boiling tank 155, the temperature is maintained at 145 ℃, isooctyl acrylate in the material is changed into steam, the steam enters the de-weighting tower 151 through the second gas return pipe 1551, the heat energy of part of the steam is used for heating the material in the de-weighting tower 151, the other part of the steam enters the second condenser 157 through the second communicating pipe 156 to be condensed, the condensed liquid flows into the isooctyl acrylate collecting tank 158 through the second communicating pipe 156, and when the content of isooctyl acrylate in the isooctyl acrylate collecting tank 158 is greater than 99.5%, isooctyl acrylate in the isooctyl acrylate collecting tank 158 is transferred to the isooctyl acrylate storage tank 16.
Referring to fig. 9, by controlling the material feeding amount in the second feeding pipe 152, the isooctyl acrylate amount refluxed to the de-weighting tower 151, and the amount of isooctyl acrylate condensed by the second condenser 157, the sum of the material feeding amount and the isooctyl acrylate amount refluxed to the de-weighting tower 151 is equal to the amount of isooctyl acrylate collected by condensation, so that continuous de-weighting of raw materials can be realized, the production efficiency is improved, and the human cost is reduced. And discharging the material from the second detection pipe 1541 for detection, wherein the mass percent of the isooctyl acrylate in the material is lower than 0.5%, collecting the material in the second storage tank 1542, wherein the material is a heavy component, mainly polymer of the isooctyl acrylate, phenothiazine, copper salt, high-efficiency 705 and p-hydroxyanisole, and separating the isooctyl acrylate from the heavy component is realized.
Referring to fig. 10, the cracking apparatus 17 includes a cracking tower 171, the top of the cracking tower 171 is communicated with a second storage tank 1542, and the cracking tower 171 is communicated with the second storage tank 1542 through a third inlet pipe 172; a plurality of third mixing plates 173 having the same structure as the mixing plates 124 are fixedly connected to the inner wall of the cracking tower 171; the bottom of the cracking tower 171 is communicated with a third return pipe 174, the third return pipe 174 is sequentially communicated with a third detection pipe 1741 for collecting the materials in the cracking tower 171 and detecting and judging whether the materials meet the collection requirements or not and a residue storage tank 1742 for storing the waste materials along the material flowing direction, and a third centrifugal pump 1743 for collecting the waste materials is communicated between the third return pipe 174 and the residue storage tank 1742; one end of the third return pipe 174 is communicated with the bottom of the cracking tower 171, and the other end is communicated with a third constant boiling tank 175, the bottom surface of the third constant boiling tank 175 and the bottom surface of the cracking tower 171 are in the same plane, and the height of the third constant boiling tank 175 is lower than that of the cracking tower 171.
Referring to fig. 10, a third air return pipe 1751 is communicated with the top of the third azeotropic tank 175, and the communication between the third air return pipe 1751 and the cracking tower 171 is located in the middle of the cracking tower 171 and between the adjacent third mixing plates 173. The top of the cracking tower 171 is communicated with a third condenser 177, and the third condenser 177 is communicated with a vacuum pump for vacuum pumping; the third condenser 177 is communicated with a cracking component collecting tank 178, and the cracking tower 171, the third condenser 177 and the cracking component collecting tank 178 are communicated with each other through a third communicating pipe 176; the cracking component collecting tank 178 is communicated with a cracking component storage tank 179. By controlling the feeding amount of the heavy components in the third feeding pipe 172 and the amount of the cracking components condensed by the third condenser 177, the feeding amount of the heavy components is equal to the condensation amount of the cracking components, the continuous decomposition of the heavy components can be realized, the production efficiency is improved, and the human cost is reduced.
Referring to fig. 10, the cracking apparatus 17 is evacuated to an empty state by using a vacuum pump, and heating steam is continuously introduced into a jacket layer formed on the outer wall of the third constant boiling tank 175 to heat the material in the third constant boiling tank 175, the temperature is maintained at 160 ℃, so that the polymer of isooctyl acrylate in the heavy component in the third constant boiling tank 175 is cracked into isooctyl acrylate, acrylic acid and isooctyl ester, and the polymer is recovered in a cracked component collection tank 178 for reuse; when the mass percentage of the polymer of isooctyl acrylate in the effluent is less than 10% by detecting the effluent from the third detecting tube 1741, the waste is collected in the residue storage tank 1742 for collective treatment.
Referring to fig. 11 and fig. 1, the tail gas treatment subsystem 3 includes a tail gas storage tank 30 communicated with the esterification reaction kettle 1, the cooling kettle 11, the washing tower 12 and the water recovery tower 21, the tail gas storage tank 30 is communicated with a tail gas absorption tower 31, and the tail gas absorption tower 31 is in a rectangular parallelepiped shape; the tail gas storage tank 30 is communicated with the tail gas absorption tower 31 through a waste gas conveying pipe 32; a nitrogen generator 321 is communicated with the exhaust gas delivery pipe 32 and is used for preventing acrylic acid from being oxidized; a water absorption chamber 5 communicated with the condensation tank 25, a spraying absorption chamber 6 communicated with the water absorption chamber 5 and a terminal absorption chamber 7 communicated with the spraying absorption chamber 6 are formed in the tail gas absorption tower 31 from top to bottom; the spraying absorption chamber 6 is communicated with a spraying mechanism 60; the terminal absorption chamber 7 is provided with a purification mechanism 8 for ensuring the quality of the treated tail gas; the water absorption chamber 5 is communicated with a recovery device 9.
Referring to fig. 11, the side wall of the tail gas absorption tower 31 is provided with a stirring device 33 for stirring the water in the water absorption chamber 5; the stirring device 33 comprises a driving motor 331 fixedly connected to the side wall of the tail gas absorption tower 31, and an output shaft of the driving motor 331 is fixedly connected with a stirring rod 332; the stirring rod member 332 is circumferentially and fixedly connected with a plurality of inclined blade stirring paddles 333, the inclined blade stirring paddles 333 are axially and fixedly connected to the stirring rod member 332 along the stirring rod member 332, and the distances between the adjacent inclined blade stirring paddles 333 are equal.
Referring to fig. 11, the recovery apparatus 9 includes an extraction tank 90 communicating with the water absorption chamber 5; a stirring assembly 901 with the same structure as the stirring device 33 is arranged in the extraction tank 90, the upper part of the side wall of the extraction tank 90 is communicated with a feeding pipe 902 communicated with the tail gas absorption tower 31, and the feeding pipe 902 is communicated with the lower part of the side wall of the water absorption chamber 5; the upper part of the side wall of the extraction tank 90 is communicated with an extractant inlet pipe 903, the bottom of the extraction tank 90 is communicated with a discharge pipe 904, and the discharge pipe 904 comprises a water discharge pipe 9041 communicated with the generated water recovery tank 22 and a discharge main pipe 9042 communicated with the esterification reaction kettle 1; liquid materials in the water absorption chamber 5 enter the extraction tank 90 through the feeding pipe 902, the extracting agent is added into the extraction tank 90 through the extracting agent inlet pipe 903, isooctyl alcohol can be used as the extracting agent, the stirring component 901 is started for stirring and standing, so that the water body and the extracting agent are layered, acrylic acid and isooctyl alcohol in water are dissolved in the extracting agent and are extracted and floated on the upper layer, the water layer is discharged through the water discharging pipe 9041, and then the extracting agent is collected through the discharging main pipe 9042, so that the separation of water and acrylic acid and isooctyl alcohol is realized. The extracting agent is composed of acrylic acid and isooctyl ester, is a reaction raw material of isooctyl acrylate, can be recycled, improves the utilization rate of acrylic acid and isooctyl alcohol, and saves material consumption.
Referring to fig. 12, a first partition plate 40 and a second partition plate 4 are fixedly connected to the interior of the tail gas absorption tower 31 from top to bottom, and the tail gas absorption tower 31 is divided into a water absorption chamber 5, a spray absorption chamber 6 and a terminal absorption chamber 7 from top to bottom; the upper surface of the first clapboard 40 is vertically and fixedly connected with a third clapboard 401; the lower surface of the second partition plate 4 is vertically and fixedly connected with a fourth partition plate 402, and a first spray chamber 61, a second spray chamber 62 and a third spray chamber 63 are formed in the spray absorption chamber 6 at intervals; the first spray chamber 61 is communicated with the second spray chamber 62; the second spray chamber 62 is communicated with a third spray chamber 63; the tail gas can pass through the first spray chamber 61, the second spray chamber 62 and the third spray chamber 63 in a snake shape and fully contact with a spraying water body, so that the acrylic acid in the tail gas is effectively removed, and the tail gas treatment quality is ensured. The first partition plate 40 is provided with a vent hole 403 communicated with the water absorption chamber 5 and the first spray chamber 61; the second partition 4 is provided with a breather pipe 41 communicated with the third shower chamber 63 and the terminal absorption chamber 7; a spray water recovery pipe 51 is communicated between the third spray chamber 63 and the water absorption chamber 5, one end of the spray water recovery pipe 51 is communicated with the bottom of the side wall of the third spray chamber 63, and the other end is communicated with the upper part of the side wall of the water absorption chamber 5.
Referring to fig. 12 in conjunction with fig. 13, a sandwich cavity 42 is formed inside the second separator 4; the spraying mechanism 60 comprises a plurality of first spraying main pipes 601 which are fixedly connected in the sandwich cavity 42 and are communicated with each other, the first spraying main pipes 601 are parallel to each other, the distance between the adjacent first spraying main pipes 601 is the same, the adjacent first spraying main pipes 601 are communicated with each other through a connecting pipe water supply branch pipe 606, the first spraying main pipes 601 are communicated with a water supply pipe 602, one end of the water supply pipe 602 is communicated with the first spraying main pipes 601, and the other end of the water supply pipe 602 is communicated with the water absorption chamber 5; a water pump 603 is fixedly communicated with the water supply pipe 602, and the water pump 603 is fixedly connected to the side wall of the tail gas absorption tower 31; a plurality of first spray branch pipes 604 are fixedly communicated with the first spray main pipe 601 in the circumferential direction, one end of each first spray branch pipe 604 is vertically and fixedly communicated with the first spray main pipe 601 in the circumferential direction, and the other end of each first spray branch pipe 604 penetrates through a second partition plate 4 to be communicated with the first spray chamber 61; a plurality of second spray branch pipes 605 are fixedly communicated with the first spray main pipe 601 in the circumferential direction, one end of each second spray branch pipe 605 is vertically and fixedly communicated with the first spray main pipe 601 in the circumferential direction, and the other end of each second spray branch pipe 605 penetrates through a second partition plate 4 and is communicated with the second spray chamber 62; the first spray branch pipes 604 are arranged at intervals along the water flow direction of the first spray main pipe 601, and the distance between every two adjacent first spray branch pipes 604 is the same; the second spray branch pipes 605 are arranged at intervals along the water flow direction of the first spray main pipe 601, and the distances between the adjacent second spray branch pipes 605 are the same. The water pump 603 pumps the water in the water absorption chamber 5 to the first spraying main pipe 601, the second spraying chamber 62 is connected with the first spraying main pipe 601 through the second spraying branch pipe 605, the first spraying chamber 61 is connected with the first spraying branch pipe 604, the tail gas passing through the spraying absorption chamber 6 is sprayed and then is absorbed and purified, the acrylic acid and the isooctanol in the air are further absorbed, and the better purification purpose is achieved.
Referring to fig. 12, a fifth partition plate 43 is fixedly connected to the upper surface of the second partition plate 4 in an upward vertical direction; a sixth partition 311 is vertically and downwardly fixedly connected to the inner wall of the top of the tail gas absorption tower 31, and the terminal absorption chamber 7 is formed with a first terminal absorption chamber 71, a second terminal absorption chamber 72 and a third terminal absorption chamber 73 which are communicated with each other. Referring to fig. 14, the purge mechanism 8 includes a composite adsorbent 74 filled in each of the first, second, and third terminal absorbing chambers 71, 72, 73, and the third terminal absorbing chamber 73 is communicated with a chimney 75. The gas treated by the spray absorption chamber 6 can pass through the composite adsorbent 74 of the first terminal absorption chamber 71, the composite adsorbent 74 of the second terminal absorption chamber 72 and the composite adsorbent 74 of the third terminal absorption chamber 73 in a serpentine manner, the three composite adsorbents 74 further perform adsorption purification on the gas treated by the spray absorption chamber 6, further reduce air pollutants in the gas, such as nitrogen oxides, sulfur dioxide, acrylic acid and isooctanol, and the purified gas is discharged from a chimney 75.
Referring to fig. 12, in combination with fig. 14, the composite adsorbent 74 includes a composite adsorbent main body 741 and a composite mesh 742 covering an outer wall of the composite adsorbent main body 741, the composite adsorbent main body 741 includes a plurality of layers of zeolite plates 743 and a bamboo charcoal fiber felt 744 compounded between the zeolite plates 743, and the bamboo charcoal fiber felt 744 is used for absorbing residual acrylic acid and isooctanol; the zeolite plate 743 penetrates through the upper surface and the lower surface to be provided with the air diffusing holes 745, and the air diffusing holes 745 increase the air flow flux of air entering the bamboo charcoal fiber felt 744 from the zeolite plate 743 and can improve the tail gas purification rate.
Referring to fig. 15, the composite net 742 is plain-woven from warp threads 7421 and weft threads 7422; the warp 7421 and weft 7422 have the same composition; the warp 7421 comprises polyacrylonitrile-based active carbon fiber 7423 and polyamide fiber 7424, the polyacrylonitrile-based active carbon fiber 7423 not only has the function of adsorbing and removing acrylic acid and isooctanol gas, but also has the function of adsorbing and decomposing sulfur dioxide and nitrogen dioxide in the air, so that the purification quality can be further improved; the better abrasion resistance of the polyamide fibers 7424 ensures durability of the composite web 742.
The invention discloses a preparation process of isooctyl acrylate, which comprises the following steps: the method comprises the following steps:
step 1: esterification synthesis is carried out to prepare a crude product;
step 1.1: 5kg of phenothiazine (special grade, product standard Q/320211NCM03-2018, Wuxi market Mitsumadeng chemical Co., Ltd.), 9.61897 tons of acrylic acid (purity 99.5%, Taitai plastic industry Ningbo Co., Ltd.), 17.38203 tons of isooctanol (purity 99.5%, China petrochemical) are sequentially added into an esterification reaction kettle 1, stirring is started for 10min, 75kg of p-toluenesulfonic acid (industrial grade 99%, Shanghai Kai Yin Co., Ltd.) is added, and stirring is continuously carried out;
step 1.2: continuously stirring, vacuumizing the esterification reaction kettle 1 to-40.0 Kpa by using a vacuum pump, wherein the reaction temperature is 90 ℃, and reacting for 1 hour;
step 1.3: continuously stirring, vacuumizing the esterification reaction kettle 1 to-50.0 Kpa by using a vacuum pump, wherein the reaction temperature is 95 ℃, and reacting for 1 hour;
step 1.4: continuously stirring, vacuumizing the esterification reaction kettle 1 to-70.0 Kpa by using a vacuum pump, wherein the reaction temperature is 105 ℃, and reacting for 1 hour;
step 1.5: continuously stirring, vacuumizing the esterification reaction kettle 1 to-80 Kpa by a vacuum pump, wherein the reaction temperature is 112 ℃, and reacting for 2.0 hours to obtain a crude product;
step 2: cooling the crude product to obtain a cooling material;
step 2.1: conveying the water layer in the crude product in the step 1 to a water recovery tower 21 to extract and recover acrylic acid in the generated water, storing the generated water in a generated water recovery tank 22, and storing the extracted acrylic acid and an extracting agent in an extraction layer collection tank 23;
step 2.2: after the water layer in the crude product is collected, transferring the liquid material on the water layer in the crude product into a cooling kettle 11 for cooling, introducing the generated water stored in a generated water recovery tank 22 as a cooling medium into the jacket layer of the cooling kettle 11, and cooling for 2 hours to obtain a cooled material; wherein the cooling medium which completes heat exchange in the jacket layer flows to the condensation tank 25 and can be supplemented to the generated water recovery tank 22;
and step 3: washing the cooling material, and recovering the p-toluenesulfonic acid to obtain a washing material;
step 3.1: transferring the cooling material obtained in the step 2.2 to a washing tower 12, and washing for 3 hours by using the generated water stored in the generated water recovery tank 22 as a washing water source;
step 3.2: transferring the water layer in the washing tower 12 to a multi-effect evaporator 131, evaporating the water body to obtain a concentrated p-toluenesulfonic acid aqueous solution, wherein the evaporated water body is condensed in a condensation tank 25 for recycling, and the concentrated p-toluenesulfonic acid aqueous solution is collected in a catalyst recovery tank 133 for later use to obtain a washing material;
and 4, step 4: removing light materials are obtained by light material removing operation;
step 4.1: the washing material in the step 3.2 is introduced into a light component removal tower 141, flows to a first constant boiling tank 145 under the action of gravity, copper N, N-di-N-butyl dithiocarbamate is dropwise added into the first constant boiling tank 145 to prevent isooctyl acrylate from polymerizing (product standard Q/320211NCM05-2018, Wuxi city Nakamao chemical Co., Ltd.), the dropwise adding speed is 300g/h,
step 4.2: vacuumizing the light component removal device 14 by using a vacuum pump, wherein the pressure is-99.5 Kpa, the temperature is controlled to be 140 ℃, so that isooctyl alcohol and isooctyl acrylate reach a constant boiling point, and removing the isooctyl alcohol;
step 4.3: after the light component removal time is 2.5 hours, opening a first detection pipe 1441 to collect materials for detection, and if the mass percentage of isooctyl alcohol in the detected materials is lower than 0.1%, starting a first centrifugal pump 1443 to collect the materials in a first storage tank 1442 to obtain light component removal materials; if the mass percent of isooctyl alcohol in the detected material is more than 0.1%, continuing the light removal operation, opening a first detection pipe 1441 to collect the material for detection every 20min until the mass percent of isooctyl alcohol in the detected material is less than 0.1%, opening a first centrifugal pump 1443, collecting the material in a first storage tank 1442, and obtaining the light removed material;
and 5: removing the heavy components to obtain a target product and heavy components;
step 5.1: introducing the light material removed in the step 4.3 into a de-weighting tower 151, enabling the light material to flow to a second constant boiling tank 155 under the action of gravity, and dropwise adding efficient 705 (Wuxi city Zhengmao chemical Co., Ltd.) and p-hydroxyanisole (product standard Q/320211NCM02-2018, Wuxi city Zhengmao chemical Co., Ltd.) into the second constant boiling tank 155 to prevent polymerization of isooctyl acrylate, wherein the dropwise adding speed of the efficient 705 is 3.7g/h, and the dropwise adding speed of the p-hydroxyanisole is 3.7 g/h;
step 5.2: vacuumizing the weight removal device 15 by using a vacuum pump, controlling the pressure to be-99.5 Kpa and the temperature to be 145 ℃, enabling the isooctyl acrylate to reach the boiling point, condensing and collecting in an isooctyl acrylate collection tank 158;
step 5.3: collecting the material in the isooctyl acrylate collecting tank 158 through a detecting pipe 1581, detecting the material, and collecting the material in the isooctyl acrylate storage tank 16 if the content of isooctyl acrylate in the material is more than 99.5%; meanwhile, the material in the second return pipe 154 is collected through a second detection pipe 1541, and the material is detected, and if the content of isooctyl acrylate in the material is less than 30%, the material is collected in a second storage tank 1542 for later use;
step 6: step 5, introducing the heavy component in the second storage tank 1542 into the cracking tower 171, flowing to the third constant boiling tank 175 under the action of gravity, vacuumizing the cracking device 17 by using a vacuum pump, controlling the pressure to be-99.5 Kpa, the temperature to be 160 ℃, and the cracking time to be 4 hours, so that the polymer of isooctyl acrylate in the heavy component in the third constant boiling tank 175 is cracked into isooctyl acrylate, acrylic acid and isooctyl ester, and recycling the isooctyl acrylate, the acrylic acid and the isooctyl ester in the cracking component collection tank 178; when the mass percentage of the polymer of isooctyl acrylate in the effluent is less than 10% by detecting the effluent from the third detecting tube 1741, the waste is collected in the residue storage tank 1742 for collective treatment.
The waste gas generated by the esterification reaction kettle 1, the cooling kettle 11, the washing tower 12 and the water regeneration subsystem 2 is collected in a tail gas storage tank 30 for collective treatment, and in the process of conveying the tail gas to a tail gas absorption tower 31 by a waste gas conveying pipe 32, a nitrogen generator 321 mixes nitrogen into the tail gas to prevent the oxidation of acrylic acid in the tail gas; the tail gas entering the tail gas absorption tower 31 firstly passes through the water absorption chamber 5, acrylic acid and a small amount of isooctyl ester in the tail gas are recovered in a water body of the water absorption chamber 5, the tail gas enters the spray absorption chamber 6, the acrylic acid and the small amount of isooctyl ester in the tail gas are further recovered in the spray water body, the acrylic acid and the small amount of isooctyl ester are gathered in the water body of the water absorption chamber 5 for collective treatment, then the tail gas enters the terminal absorption chamber 7, the residual acrylic acid, the small amount of isooctyl ester, nitrogen oxide and sulfur dioxide in the tail gas are removed under the action of the purification mechanism 8, and finally the tail gas is discharged from a chimney. Wherein, the water collected in the water absorption chamber 5 flows to the extraction tank 90, the acrylic acid in the water is extracted and recovered by adding the extracting agent isooctanol into the extraction tank 90, and can be reused as a synthetic raw material, and simultaneously, the available water is recovered in the generated water recovery tank 22, and the water is reused.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.

Claims (10)

1. A preparation process of isooctyl acrylate is characterized by comprising the following steps: the method comprises the following steps:
step 1: sequentially adding a polymerization inhibitor, acrylic acid and isooctanol into an esterification reaction kettle (1), stirring, adding a water-soluble catalyst, stirring, and carrying out temperature and pressure control reaction for 5-6 hours to obtain a crude product;
step 2: conveying a water layer in the crude product to a water regeneration subsystem (2) for recycling, cooling a liquid material on the water layer in the crude product to a cooling kettle (11), taking generated water recycled by the water regeneration subsystem (2) as a cooling medium, and cooling for 1-2 hours to obtain a cooling material;
and step 3: transferring the cooling material into a washing tower (12), washing for 2-3 hours by using the generated water recovered by the water regeneration subsystem (2) as a washing water source to obtain a washing material, wherein the washing wastewater flows to a catalyst recovery device (13) to carry out catalyst recovery and water body supplement in the water regeneration subsystem (2);
and 4, step 4: introducing the washing material into a light component removal device (14), adding a polymerization inhibitor of isooctyl acrylate into the light component removal device (14), wherein the pressure of the light component removal device (14) is-95.0 Kpa to-99.5 Kpa, the temperature is 130-145 ℃, the light component removal time is 2-4 hours, and removing light components to obtain a light component removal material;
and 5: introducing the light weight removal material into a weight removal device (15), adding a polymerization inhibitor of isooctyl acrylate into the weight removal device (15), wherein the pressure of the weight removal device (15) is-95.0 Kpa to-99.5 Kpa, the temperature is 130-150 ℃, the weight removal time is 2-4 hours, and obtaining the target product isooctyl acrylate which is collected in an isooctyl acrylate storage tank (16);
waste gas generated by the esterification reaction kettle (1), the cooling kettle (11), the washing tower (12) and the water regeneration subsystem (2) is collected in the tail gas treatment subsystem (3), generated water in the water regeneration subsystem (2) can be used as an extraction water source of the tail gas treatment subsystem (3), and water separated by the tail gas treatment subsystem (3) can be supplemented to the water regeneration subsystem (2); the material extracted by the tail gas treatment subsystem (3) can be used as a synthetic raw material of isooctyl acrylate.
2. The process of claim 1 for the preparation of isooctyl acrylate, wherein: the step 1: esterification synthesis is carried out to prepare a crude product;
step 1.1: sequentially adding a polymerization inhibitor, acrylic acid and isooctyl alcohol into the esterification reaction kettle (1), stirring, adding a water-soluble catalyst, and continuously stirring;
step 1.2: vacuumizing to-38.0 Kpa to-43.0 Kpa, reacting at 88.0-92.0 ℃ for 0.8-1.2 hours;
step 1.3: vacuumizing to-53.0 Kpa to-58.0 Kpa, reacting at 95.0-97.5 ℃ for 0.8-1.2 hours;
step 1.4: vacuumizing to-70.0 Kpa to-72.5 Kpa, reacting at 103.0-107.0 ℃ for 0.8-1.2 hours;
step 1.5: vacuumizing to-77.5 Kpa to-82.5 Kpa, reacting at 110.0-115.0 deg.C for 2.0-3.0 hr.
3. The process of claim 1 for the preparation of isooctyl acrylate, wherein: in the step 2, the water regeneration subsystem (2) comprises a water recovery tower (21) communicated with the esterification reaction kettle (1), a generated water recovery tank (22) communicated with the water recovery tower (21) and communicated with the washing tower (12), an extraction layer collection tank (23) communicated with the water recovery tower (21) and communicated with the esterification reaction kettle (1), an extractant storage tank (24) communicated with the water recovery tower (21), a condensation pool (25) communicated with the upper part of a jacket layer of the cooling kettle (11), a mixing mechanism (26) arranged in the water recovery tower (21) and used for mixing an extractant and generated water, and a water collection mechanism (27) communicated with the bottom of the side wall of the water recovery tower (21), wherein the generated water recovery tank (22) is communicated with the lower part of the jacket layer of the cooling kettle (11); the condensation tank (25) is communicated with the generated water recovery tank (22); the condensation tank (25) is communicated with the catalyst recovery device (13), and the catalyst recovery device (13) is communicated with the esterification reaction kettle (1); a generated water inlet pipe (211) for transferring the generated water in the esterification reaction kettle (1) into the water recovery tower (21) is communicated with the side wall of the upper part of the water recovery tower (21); an extractant inlet pipe (212) used for transferring the extractant in the extractant storage tank (24) to the water recovery tower (21) is communicated with the side wall of the lower part of the water recovery tower (21).
4. The process of claim 3 for the preparation of isooctyl acrylate, wherein: the tail gas treatment subsystem (3) comprises a tail gas storage tank (30) communicated with the esterification reaction kettle (1), a cooling kettle (11), a washing tower (12) and a water recovery tower (21), a tail gas absorption tower (31) communicated with the tail gas storage tank (30), a waste gas conveying pipe (32) communicated between the tail gas storage tank (30) and the tail gas absorption tower (31), and a nitrogen generator (321) communicated with the waste gas conveying pipe (32), wherein a water absorption chamber (5) communicated with the condensation tank (25), a spraying absorption chamber (6) communicated with the water absorption chamber (5) and a terminal absorption chamber (7) communicated with the spraying absorption chamber (6) are formed in the tail gas absorption tower (31) from top to bottom; the spraying absorption chamber (6) is communicated with a spraying mechanism (60) for pumping the water body in the water absorption chamber (5) to spray and absorb the tail gas in the spraying absorption chamber (6); the terminal absorption chamber (7) is provided with a purification mechanism (8) for ensuring the quality of the treated tail gas; the water absorption chamber (5) is communicated with a recovery device (9); the recovery device (9) is communicated with the esterification reaction kettle (1).
5. The process of claim 4, wherein the ratio of isooctyl acrylate is as follows: in the step 3, the washing tower (12) comprises a washing tower main body (123), a plurality of material mixing plates (124) fixedly connected to the inner wall of the washing tower main body (123), a plurality of material mixing holes (125) formed in the material mixing plates (124), a material passing pipe (121) communicated with the lower portion of the side wall of the washing tower (12) and communicated with the cooling kettle (11), a second extraction pump (122) communicated with the material passing pipe (121), a material discharging pipe (126) communicated with the bottom of the washing tower (12) and a stirring mechanism (127) arranged on the washing tower main body (123), and the distances between the adjacent material mixing plates (124) are equal; the mixing hole (125) penetrates through the upper surface and the lower surface of the mixing plate (124); the stirring mechanism (127) comprises a driving motor (1271) fixedly connected to the top of the washing tower main body (123), a stirring rod (1272) fixedly connected to an output shaft of the driving motor (1271), and a plurality of stirrers (1273) fixedly connected to the periphery of the stirring rod (1272), wherein the stirring rod (1272) penetrates through the material mixing plate (124) and is rotatably connected with the material mixing plate (124); the stirrer (1273) is positioned between the adjacent mixing plates (124); the stirrer (1273) comprises a fixed ring (1274) fixedly connected to the circumferential direction of the stirring rod (1272) and a plurality of stirring blades (1275) fixedly connected to the circumferential direction of the fixed ring (1274); the stirring blade (1275) penetrates through the surface and is provided with a plurality of through holes (1276); the stirring blades (1275) are uniformly arranged around the central axis of the fixing ring (1274).
6. The process of claim 5 for the preparation of isooctyl acrylate, wherein: in the step 3, the catalyst recovery device (13) comprises a multi-effect evaporator (131) communicated with the discharge pipe (126), a condensation pipe (132) communicated with the multi-effect evaporator (131) and used for condensing water vapor and a catalyst recovery tank (133) communicated with the multi-effect evaporator (131), one end of the condensation pipe (132) is communicated with the multi-effect evaporator (131) and the other end of the condensation pipe is communicated with the condensation pool (25), the condensation pipe (132) is arranged in the condensation pool (25), and the circumferential direction of the condensation pipe (132) is surrounded by a water body.
7. The process of claim 6 for the preparation of isooctyl acrylate, wherein: in the step 4, the light component removing device (14) comprises a light component removing tower (141), a first inlet pipe (142) communicated with the top of the light component removing tower (141) and communicated with a discharge pipe (126), a plurality of first mixing plates (143) fixedly connected with the inner wall of the light component removing tower (141) and having the same structure as the mixing plates (124), a first return pipe (144) communicated with the bottom of the light component removing tower (141), a first detection pipe (1441) sequentially communicated with the first return pipe (144) along the material flowing direction, a first storage tank (1442), a first centrifugal pump (1443) communicated with the first return pipe (144) and the first storage tank (1442), a first constant boiling tank (145) communicated with one end of the first return pipe (144) back to the light component removing tower (141), a first return pipe (1451) communicated with the top of the first constant boiling tank (145), a first condenser (147) communicated with the top of the light component removing tower (141) and a light component collecting tank (148) communicated with the first condenser (147), the light component collecting tank (148) is communicated with the top of the light component removing tower (141); the communication part of the first gas return pipe (1451) and the light component removal tower (141) is positioned in the middle of the light component removal tower (141) and between the adjacent first mixing plates (143); the light component removal tower (141), the first condenser (147) and the light component collection tank (148) are communicated through a first communicating pipe (146); the bottom surface of the first constant boiling tank (145) and the bottom surface of the light component removal tower (141) are positioned in the same plane, and the height of the first constant boiling tank (145) is lower than that of the light component removal tower (141).
8. The process of claim 7 for the preparation of isooctyl acrylate, wherein: in the step 5, the weight removing device (15) comprises a weight removing tower (151) communicated with the first storage tank (1442), a second inlet pipe (152) communicated between the weight removing tower (151) and the first storage tank (1442), a plurality of second mixing plates (153) fixedly connected to the inner wall of the weight removing tower (151) and having the same structure as the mixing plates (124), a second return pipe (154) communicated with the bottom of the weight removing tower (151), a second detection pipe (1541) sequentially communicated with the second return pipe (154) along the material flow direction, a second storage tank (1542), a second centrifugal pump (15413) communicated with the second return pipe (154) and the second storage tank (1542), and a second constant boiling tank (155) communicated with the second return pipe (154) and facing away from one end of the weight removing tower (151); a second air return pipe (1551) communicated with the top of the second constant boiling tank (155), a second condenser (157) communicated with the top of the de-weighting tower (151), and an isooctyl acrylate collecting tank (158) communicated with the second condenser (157), wherein the isooctyl acrylate collecting tank (158) is communicated with the top of the de-weighting tower (151); the second air return pipe (1551) is communicated with the heavy component removal tower (151) and is positioned in the middle of the heavy component removal tower (151) and between the adjacent second mixing plates (153); the iso-octyl acrylate collecting tank (158) is communicated with the iso-octyl acrylate storage tank (16); the de-weighting tower (151), the second condenser (157) and the isooctyl acrylate collecting tank (158) are communicated through a second communicating pipe (156); the bottom surface of the second constant boiling tank (155) and the bottom surface of the heavy component removal tower (151) are in the same plane, and the height of the second constant boiling tank (155) is lower than that of the heavy component removal tower (151).
9. The process of claim 8 for the preparation of isooctyl acrylate, wherein: further comprising the step 6: and (3) introducing the heavy components separated in the step (5) into a cracking device (17), wherein the pressure of the cracking device (17) is-95.0 Kpa to-99.5 Kpa, the temperature is 155-165 ℃, and the cracking time is 2-4 hours, so as to obtain a recyclable cracking substance.
10. The process of claim 9 for the preparation of isooctyl acrylate, wherein: in the step 6, the cracking device (17) comprises a cracking tower (171) communicated with the weight removal device (15), a third inlet pipe (172) communicated between the cracking tower (171) and the second storage tank (1542), a plurality of third mixing plates (173) fixedly connected to the inner wall of the cracking tower (171) and having the same structure as the mixing plates (124), a third return pipe (174) communicated with the bottom of the cracking tower (171), a third detection pipe (1741) sequentially communicated with the third return pipe (174) along the material flowing direction, a residue storage tank (1742), a third centrifugal pump (1743) communicated with the residue storage tank (1742) and the third return pipe (174), a third constant boiling tank (175) communicated with one end of the third return pipe (174) back to the cracking tower (171), a third return pipe (1751) communicated with the top of the third constant boiling tank (175), a third condenser (177) communicated with the top of the cracking tower (171) and a cracking component collection tank (178) communicated with the third sub-condenser (177), the third air return pipe (1751) is communicated with the cracking tower (171) and is positioned in the middle of the cracking tower (171) and between the adjacent third mixing plates (173); the cracking tower (171), the third condenser (177) and the cracking component collecting tank (178) are communicated through a third communicating pipe (176); the bottom surface of the third constant boiling tank (175) and the bottom surface of the cracking column (171) are in the same plane and the height of the third constant boiling tank (175) is lower than the height of the cracking column (171).
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