CN201587916U - Continuous production device for nonandioic acid refining and purification - Google Patents
Continuous production device for nonandioic acid refining and purification Download PDFInfo
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- CN201587916U CN201587916U CN2009202068291U CN200920206829U CN201587916U CN 201587916 U CN201587916 U CN 201587916U CN 2009202068291 U CN2009202068291 U CN 2009202068291U CN 200920206829 U CN200920206829 U CN 200920206829U CN 201587916 U CN201587916 U CN 201587916U
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Abstract
The utility model discloses a continuous production device for nonandioic acid refining and purification, which comprises a reaction kettle, a first section refining system, a second section refining system and a third section refining system, wherein impurities as chlorine ions and sulphate ions are removed from the commercial-grade nonandioic acid in the reaction kettle through the complexing of the complexing agent at the first place, then the nonandioic acid enters the first section refining system for ultrapure water crystallization, enters the second section refining system for ethyl acetate crystallization, and enters the third section refining system for ultrapure water crystallization, so that the nonandioic acid refining and purification is realized by removing the single acids and the dibasic acids under the C9 contained in the commercial-grade nonandioic acid through repeated crystallization. The whole set of device has the advantages of excellent controllability, high stability and repeatability of the process, high product purity and excellent yield coefficient, and can realize the continuous production of nonandioic acid refining and purification. The continuous production device not only fills the gap of high purity electronic grade nonandioic acid demand in domestic market, but also is of great significance in improving the comprehensive utilization of energy and resource.
Description
Technical field
The utility model relates to a kind of serialization Chemicals production equipment, is specifically related to the refining serialization production equipment of purifying of a kind of nonane diacid.
Background technology
Nonane diacid is a kind of important organic synthesis intermediate, and industrial application is very extensive.Especially in recent years, along with the development of synthetic organic chemical manufacturing industry, the market requirement of nonane diacid day by day increases.Nonane diacid mainly is to produce nonane diacid class softening agent in industrial purposes, next is used to produce the lubricant Polymer Synthesizing, also can be used for the preparation of electrolytic condenser manufacturing, skin diseases treatment, the production of spices finish, thermoplastic mould resist, flocculation agent, fire retardant and stablizer etc.The high added value of nonane diacid depends on the purity of product, and for example why common nonane diacid product can not be used to produce the electrolytic condenser intermediate, and reason just is that its nonane diacid and foreign matter content do not reach set quota.Domestic nonane diacid manufacturing enterprise lacks the technology and the equipment of effective purification nonane diacid at present, and domestic product of the same race is dependence on import all.Patent " a kind of separation purification method of nonane diacid " (application number: 200810045090.0) disclose a kind of separation purification method of nonane diacid, by oxidation liquid underpressure distillation that unsaturated fatty acids ozonize-oxygenolysis is obtained remove desolvate and n-nonanoic acid after, residue oxidation liquid is transferred to the thin-film evaporator distillation and obtains the nonane diacid crude product, thick nonane diacid is through extraction, recrystallization, obtain the nonane diacid crystal, in the nonane diacid recrystallization process, the low carbon dicarboxylic acid of C4-C8 is dissolved in cold water in the nonane diacid, thereby gets rid of with crystalline mother solution; Adopt membrane separation unit to reclaim remaining nonane diacid in the crystalline mother solution simultaneously, the nonane diacid that obtains is transferred to the climbing-film evaporator drying and dehydrating, the nonane diacid that obtains after the dehydration obtains the nonane diacid product through thin film evaporation; Patent " a kind of refinement and purification method of nonane diacid " (application number: 200810061651.6) disclose a kind of refinement and purification method of nonane diacid, by with the rectification under vacuum of nonane diacid mixture, component and the n-nonanoic acid of boiling point before n-nonanoic acid steamed, carry out steam then and dash steaming, make and do not steam the monoprotic acid weight ratio content sum of material mid-boiling point before n-nonanoic acid and be not more than 3%, to not steam material again and carry out rectification under vacuum, steam dashes and steams, and steams the crude product nonane diacid; Again with the crude product nonane diacid that steams with after solvent mixes by a certain percentage, after several steps, the centrifugal crystalline product that obtains obtaining final nonane diacid product with crystalline product through the decompression oven dry at last by intensification, insulated and stirred and crystallisation by cooling.
More than two technical matters complexity, be used for industrialization and produce constantly, operational condition is restive, quality product is difficult to stablize, and carries out the construction of production equipment at these two kinds of methods, equipment has high input, the production cost height.
Therefore, need a kind of production equipment, can carry out the refining serialization production of purifying of nonane diacid, and technology is simple and easy to control, favorable reproducibility, purified nonane diacid product purity height, quality is good.
The utility model content
In view of this, the purpose of this utility model provides the refining serialization production equipment of purifying of a kind of nonane diacid, can carry out the refining serialization production of purifying of nonane diacid, and technology is simple and easy to control, favorable reproducibility, purified nonane diacid product purity height, and quality is good.
The refining serialization production equipment of purifying of nonane diacid of the present utility model, comprise reactor, steam heating system, water coolant plenum system and pumped vacuum systems, described steam heating system is provided with the steam heating pipeline, described water coolant plenum system is provided with cooling water circulation pipeline, described pumped vacuum systems comprises vacuum system I, vacuum system II and vacuum system III, material between the device shifts by vacuum system and realizes, avoids the pollution of material;
Also comprise one section refining system, two-section refinement system, three sections refining systems;
Described one section refining system comprises the elementary insulation filtration unit that sets gradually along the material direct of travel, one section crystalline element and one section Minton dryer, the material outlet of described reactor is communicated with the material inlet of elementary insulation filtration unit, described one section crystalline element comprises one section crystallization kettle and one section equipment for separating liquid from solid, the material outlet of described one section crystallization kettle links to each other with the material inlet of one section equipment for separating liquid from solid, described one section crystalline element is 1-3 cover and series connection successively, described reactor, each overlaps one section crystallization kettle and one section Minton dryer and vacuum orifice is set respectively and is communicated with vacuum system I;
Described two-section refinement system comprises two sections crystalline elements and two sections Minton dryers, described two sections crystalline elements comprise two sections crystallization kettles and two sections equipment for separating liquid from solid, the material outlet of described two sections crystallization kettles is communicated with the material inlet of two sections equipment for separating liquid from solid, described two sections crystalline elements are 2-4 cover and series connection successively, the material outlet of described one section Minton dryer is communicated with the material inlet of two sections crystallization kettles of first cover, the solid material outlet of two sections equipment for separating liquid from solid of tail cover is communicated with the material inlet of two sections Minton dryers, described ethyl acetate plenum system is provided with the ethyl acetate supply line and is communicated with material inlet of two sections crystallization kettles of each cover, and each overlaps two sections crystallization kettles and two sections Minton dryers and vacuum orifice is set respectively and is communicated with vacuum system II;
Described three sections refining systems comprise the dissolution kettle that sets gradually along the material direct of travel, secondary insulation filtration unit, three sections crystalline elements and three sections Minton dryers, described three sections crystalline elements comprise three sections crystallization kettles and three sections equipment for separating liquid from solid, the material outlet of three sections crystallization kettles is communicated with the material inlet of three sections equipment for separating liquid from solid, described three sections crystalline elements are 4-6 cover and series connection successively, the material of described two sections Minton dryers enters secondary insulation filtration unit filtration after entering the dissolution kettle dissolving, filtrate is more successively through three sections crystallization kettle crystallizations of each cover, the material outlet of three sections crystallization kettles of end cover is communicated with the material outlet of three sections equipment for separating liquid from solid, the solid material outlet of three sections equipment for separating liquid from solid is communicated with dissolution kettle with three sections Minton dryer material inlets, each overlaps three sections crystallization kettles and three sections Minton dryers and vacuum orifice is set respectively and is communicated with vacuum system III;
Also comprise ultrapure water plenum system and refrigerating fulid plenum system, described ultrapure water plenum system is provided with the ultrapure water supply line, described refrigerating fulid plenum system is provided with the refrigerating fulid circulation line, the inner chamber of described reactor, one section crystallization kettle, dissolution kettle and three sections crystallization kettles is communicated with the ultrapure water supply line respectively, and the heating interlayer of reactor, one section crystallization kettle, two sections crystallization kettles, dissolution kettle and three sections crystallization kettles all is communicated with steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line.
During operation, in reactor, add ultrapure water and industrial grade azelaic acid successively, after raw material stirred intensification, add the impurity complexing agent with chlorion, complexing such as iron ion and sulfate ion, again by elementary insulation filtration unit with the complex compound filtering, the one section crystalline element that respectively overlaps that filtrate enters in one section refining system successively carries out the ultrapure water crystallization, the ultrapure water crystallisation process comprises intensification, insulation, cooling and freezing and pass through the steam heating pipeline respectively, cooling water circulation pipeline and refrigerating fulid circulation line are realized, most of C9 is dissolved in water with place an order acid and diprotic acid in the ultrapure water crystallisation process, and the nonane diacid crystallization is separated out, solidliquid mixture is separated through one section equipment for separating liquid from solid, separating obtained solid obtains one section nonane diacid product by one section Minton dryer drying, separating obtained liquid enters water treatment system, water treatment system is a prior art, not within the utility model protection domain, by one section Minton dryer drying, can further reduce the nonane diacid product impurities that enters the two-section refinement system; Again one section nonane diacid product is changed over to the two-section refinement system and carry out repeatedly ethyl acetate crystallization by two sections crystalline elements of each cover successively, the ethyl acetate crystallisation process comprises intensification, insulation, cooling and refrigerating process also pass through the steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are realized, the ethyl acetate crystallisation process can further be removed one section monoprotic acid and water-fast impurity in the nonane diacid product, two sections nonane diacid products that obtain behind two sections crystalline element crystallizing and dryings of last cover enter three sections refining systems and further purify, and collect the unified processing in back and respectively overlap two sections separating obtained ethyl acetate solutions of equipment for separating liquid from solid; In three sections refining systems, at first in dissolution kettle, adopt ultrapure water that two sections nonane diacid products are dissolved fully, again the solution in the dissolution kettle is incubated to filter and change filtrate over to three sections crystalline elements and carries out the ultrapure water crystallization, ultrapure water crystallisation process herein comprises intensification, insulation, cooling and freezing and pass through the steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are realized, insulation is filtered can further remove two sections water-fast impurity in the nonane diacid product aqueous solution, the ultrapure water crystallisation process can further be removed two sections C9 in the nonane diacid product with acid and the diprotic acid of placing an order, and the nonane diacid product that makes through three sections refining systems can reach required purity.
Further, also comprise four sections ethyl acetate recovery systems, described four sections ethyl acetate recovery systems comprise the ethyl acetate withdrawing can, the ethyl acetate still kettle, ethyl acetate distillate storage tank, ethyl acetate distillation tail washings storage tank, four sections equipment for separating liquid from solid, four sections Minton dryers and nonane diacid holding tank, the liquid material outlet of respectively overlapping two sections equipment for separating liquid from solid in the described two-section refinement system is communicated with the material inlet of ethyl acetate withdrawing can, the material outlet of ethyl acetate withdrawing can is communicated with the material inlet of ethyl acetate still kettle, the distillate that the ethyl acetate still kettle produces enters ethyl acetate distillate storage tank, the distillation tailing that produces enters four sections equipment for separating liquid from solid, the liquid material outlet of four sections equipment for separating liquid from solid is communicated with the material inlet of ethyl acetate withdrawing can, Gu the material outlet is communicated with the material inlet of nonane diacid holding tank through four sections Minton dryers, described ethyl acetate still kettle is provided with vacuum orifice and is communicated with vacuum system II, the inner chamber of ethyl acetate still kettle is communicated with the ethyl acetate supply line, the heating interlayer of ethyl acetate still kettle respectively with the steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with; By four sections ethyl acetate recovery systems the ethyl acetate filtrate that the two-section refinement system produces is distilled recovery, reduce production costs and protect environment.
Further, also comprise five sections nonane diacid recovery systems, described five sections nonane diacid recovery systems comprise five sections crystallization kettles, five sections equipment for separating liquid from solid and five sections Minton dryers, the material that described nonane diacid holding tank is collected enters five sections equipment for separating liquid from solid after five sections crystallization kettle crystallizations, the solid material outlet of described five sections equipment for separating liquid from solid is communicated with the material inlet of five sections Minton dryers, the liquid material outlet of five sections equipment for separating liquid from solid is communicated with the material inlet of five sections crystallization kettles, described five sections crystallization kettles are provided with vacuum orifice and are communicated with vacuum system II, five sections crystallization kettle inner chambers are communicated with the ethyl acetate supply line, the heating interlayer of five sections crystallization kettles and steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with; The nonane diacid solid of four sections ethyl acetate recovery system generations is further reclaiming by ethyl acetate in five sections crystallization kettles, and the nonane diacid solid of recovery can be got back to and make with extra care purification in the reactor again, reduces the loss of nonane diacid.
Further, also comprise the ethyl acetate relay tank, the liquid material outlet of described five sections equipment for separating liquid from solid communicates through the material inlet of ethyl acetate relay tank with the ethyl acetate still kettle; During device work, can be temporary by the ethyl acetate solutions that five sections equipment for separating liquid from solid are separating obtained at the ethyl acetate relay tank, treat repeatedly to collect make the storage of ethyl acetate relay tank full after, the property separation is purified again, saves Production Flow Chart.
Further, described three sections refining systems also comprise the assisted vacuum drying installation, described assisted vacuum drying installation is two covers and is separately positioned on after three sections crystallization kettles of preceding two covers and is communicated with the material inlet of three sections crystallization kettles of next crystalline element separately, described assisted vacuum drying installation is provided with vacuum orifice and is communicated with vacuum system III, by the assisted vacuum drying installation nonane diacid solid that three sections equipment for separating liquid from solid of preceding two covers produce is carried out drying, reduce the impurity that enters follow-up crystallisation process, improve the device purification efficiency, supplementary unit is set to two covers, cuts down the consumption of energy.
Further, described vacuum system III comprises vacuum sub-system I, vacuum sub-system II and vacuum sub-system III, the vacuum orifice of described dissolution kettle, three sections crystallization kettles of first cover and first cover assisted vacuum drying installation is communicated with vacuum sub-system I, the 2nd vacuum orifice that overlaps three sections crystallization kettles and the 2nd cover assisted vacuum drying installation is communicated with vacuum sub-system II respectively, and the vacuum orifice of back 2-4 three sections crystallization kettles of cover and three sections Minton dryers is communicated with vacuum sub-system III respectively; Vacuum system is separate, and the dust that can further prevent working stage generation is avoided the pollution between the system by entering next working stage in the vacuum-lines, ensures refining effect.
Further, described two sections crystalline elements are 3 covers, described three sections crystalline elements are 5 covers, when ensureing the nonane diacid refining effect, reduce device laid down cost, described elementary insulation filtration unit and secondary insulation filtration unit are hot-water filter, described one section equipment for separating liquid from solid, two sections equipment for separating liquid from solid, three sections equipment for separating liquid from solid, four sections equipment for separating liquid from solid and five sections equipment for separating liquid from solid are whizzer, described one section Minton dryer, two sections Minton dryers, three sections Minton dryers, four sections Minton dryers, five sections Minton dryers and assisted vacuum drying installation are DoubletaperedVacuumdrier, reduce material in drying process pollution and avoid the material surface hardening, ensure the physics of nonane diacid product simultaneously, stablizing of chemical property.
Further, the negative pressure pipe of described four sections Minton dryers and five sections Minton dryers is communicated with vacuum system II, reduces the device manufacturing cost and avoids mutual pollution between the system.
Further, described five sections crystallization kettles and ethyl acetate still kettle are shared, and described four sections equipment for separating liquid from solid and five sections equipment for separating liquid from solid are shared, and described four sections Minton dryers and five sections Minton dryers are shared, reduce the device manufacturing cost.
Further, also comprise holding tank, the vacuum orifice of described reactor, dissolution kettle, ethyl acetate still kettle, each section crystallization kettle, each section Minton dryer and assisted vacuum drying installation is provided with holding tank respectively and is communicated with pumped vacuum systems by holding tank, the material dust of being taken away by vacuum system is collected jar interception and storage, reduce material loss, increase economic efficiency.
The beneficial effects of the utility model are: the refining serialization production equipment of purifying of nonane diacid of the present utility model is provided with one section refining system, two-section refinement system and three sections refining systems, ultrapure water crystallisation process by the complexing process in reactor, the ultrapure water crystallisation process of one section refining system, the intrasystem ethyl acetate crystallisation process of two-section refinement and three sections exquisite systems is realized the refining purification of nonane diacid, and product yield is good, purity high (can reach 99.5% high purity); This production equipment flow process is simple, favorable reproducibility is easily controlled, reacted to process stabilizing, condition, can realize the refining serialization production of purifying of nonane diacid, not only fully filled up the blank that domestic high purity electronic-grade nonane diacid is produced, also brought significance for the comprehensive utilization that improves the energy and resource.
Description of drawings
Below in conjunction with drawings and Examples utility model is further described.
Fig. 1 is the utility model schema;
Fig. 2 is the utility model first part structure iron;
Fig. 3 is the utility model second section structure iron, a point in the map interlinking 2 of b point among Fig. 3;
Fig. 4 is the utility model third part structural representation, c point in the map interlinking 3 of d point among Fig. 4.
Embodiment
Fig. 1 is the utility model schema; Fig. 2 is the utility model first part structure iron; Fig. 3 is the utility model second section structure iron, a point in the map interlinking 2 of b point among Fig. 3; Fig. 4 is the utility model third part structural representation, c point in the map interlinking 3 of d point among Fig. 4.
As shown in the figure:
The refining serialization production equipment of purifying of nonane diacid of the present utility model, comprise reactor 1, steam heating system, water coolant plenum system and pumped vacuum systems, described steam heating system is provided with steam heating pipeline 2, described water coolant plenum system is provided with cooling water circulation pipeline, described cooling water circulation pipeline comprises water inlet pipe 41 and rising pipe 42, and described pumped vacuum systems comprises vacuum system I 4, vacuum system II 5 and vacuum system III;
Also comprise one section refining system, two-section refinement system, three sections refining systems;
Described one section refining system comprises the elementary insulation filtration unit 6 that sets gradually along the material direct of travel, one section crystalline element and one section Minton dryer 7, described one section crystalline element comprises one section crystallization kettle 8 and one section equipment for separating liquid from solid 9, each material outlet that overlaps one section crystallization kettle 8 of one section crystalline element links to each other with the material inlet of one section equipment for separating liquid from solid, in the present embodiment, one section crystalline element is 2 covers and series connection successively, described reactor, each overlaps one section crystallization kettle and one section Minton dryer and vacuum orifice is set respectively and is communicated with vacuum system I, certainly, in the present embodiment, one section crystalline element is 1 cover or can realizes the purpose of this utility model equally more than 2 covers, is set to reduce cost when two advantages of overlapping are to ensure product purity;
Described two-section refinement system comprises two sections crystalline elements and two sections Minton dryers 10, described two sections crystalline elements comprise two sections interchanger, two sections crystallization kettles 11 and two sections equipment for separating liquid from solid 12, two sections crystallization kettle material outlets in two sections crystalline elements are communicated with two sections equipment for separating liquid from solid material inlets, in the present embodiment, two sections crystalline elements are 3 covers and connect successively along the material direct of travel, certainly, in the present embodiment, two sections crystalline elements are can realize the purpose of this utility model equally more than 2 covers or 4 covers reach, the material outlet of described one section Minton dryer is communicated with the material inlet of two sections crystallization kettles of first cover, the solid material outlet of two sections equipment for separating liquid from solid of tail cover is communicated with the material inlet of two sections Minton dryers 10, described ethyl acetate plenum system is provided with ethyl acetate supply line 13 and is communicated with material inlet of two sections crystallization kettles of each cover, and each overlaps two sections crystallization kettles and two sections Minton dryers and vacuum orifice is set respectively and is communicated with vacuum system II 5;
In the present embodiment, corresponding 34, the two sections crystallization kettle tops of interchanger that are provided with two sections crystallization kettles of every cover are provided with gas outlet and are communicated with the heat transfer tube of interchanger in the two-section refinement system, by interchanger enhancing ethyl acetate backflow, reduce the wastage.
Described three sections refining systems comprise the dissolution kettle 14 that sets gradually along the material direct of travel, secondary insulation filtration unit 15, three sections crystalline elements and three sections Minton dryers 17, described three sections crystalline elements comprise three sections crystallization kettles 16 and three sections equipment for separating liquid from solid 18, the material outlet of three sections crystallization kettles is communicated with the material inlet of three sections equipment for separating liquid from solid, in the present embodiment, three sections crystalline elements are 5 covers and series connection successively, certainly, three sections crystalline elements be set to 4 covers or 6 covers and more than can realize the purpose of this utility model equally, the material of two sections Minton dryers 10 enters dissolution kettle 14 and filters by entering secondary insulation filtration unit 15 after the ultrapure water dissolving, filtrate is carried out the ultrapure water crystallisation process 4 times through three sections three sections crystalline elements of each cover more successively, material after crystallization finishes separates the back by three sections equipment for separating liquid from solid again and three sections Minton dryer dryings can obtain highly purified nonane diacid product, and the aqueous solution that the solid-liquid separation process produces in this process enters water treatment system and carries out decontaminated water and handle, in the present embodiment, dissolution kettle, each overlaps three sections crystallization kettles and three sections Minton dryers and vacuum orifice is set respectively and is communicated with vacuum system III, avoids the pollution of system;
Present embodiment also comprises ultrapure water plenum system and refrigerating fulid plenum system, described ultrapure water plenum system is provided with ultrapure water supply line 19, described refrigerating fulid plenum system is provided with the refrigerating fulid circulation line, described refrigerating fulid circulation line comprises liquid-inlet pipe 201 and drain pipe 202, described reactor 1, one section crystallization kettle 8, the inner chamber of dissolution kettle 14 and three sections crystallization kettles 16 is communicated with the ultrapure water supply line respectively, reactor 1, one section crystallization kettle 8, two sections crystallization kettles 11, the heating interlayer of dissolution kettle 14 and three sections crystallization kettles 16 all with the steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with.
As further improvement, present embodiment also comprises four sections ethyl acetate recovery systems, described four sections ethyl acetate recovery systems comprise ethyl acetate withdrawing can 21, ethyl acetate still kettle 22, ethyl acetate distillate storage tank 23, ethyl acetate distillation tail washings storage tank 39, four sections equipment for separating liquid from solid 24, four sections Minton dryers 25 and nonane diacid holding tank 26, the liquid material outlet of respectively overlapping two sections equipment for separating liquid from solid 12 in the two-section refinement system is communicated with the material inlet of ethyl acetate withdrawing can 21, the material outlet of ethyl acetate withdrawing can 21 is communicated with the material inlet of ethyl acetate still kettle 22, the distillate that the ethyl acetate still kettle produces enters ethyl acetate distillate storage tank 23, the distillation tailing that produces enters four sections equipment for separating liquid from solid 24 after ethyl acetate distillation tail washings storage tank 39 is kept in, the liquid material outlet of four sections equipment for separating liquid from solid 24 is communicated with the material inlet of ethyl acetate withdrawing can 21, Gu the material outlet is communicated with the material inlet of nonane diacid holding tank 26 through four sections Minton dryers 25, described ethyl acetate still kettle is provided with vacuum orifice and is communicated with vacuum system II 5, the inner chamber of ethyl acetate still kettle 22 is communicated with ethyl acetate supply line 13, the heating interlayer of ethyl acetate still kettle 22 respectively with the steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with, during work, isolating ethyl acetate solution in the two-section refinement process is deposited in the ethyl acetate withdrawing can 21, again the ethyl acetate solution in the ethyl acetate withdrawing can 21 being squeezed into the ethyl acetate still kettle after repeatedly collecting distills, it is standby that the distillate that obtains of distillation deposits ethyl acetate distillate storage tank 23 in, and the solid that distillation produces is pending through deposit nonane diacid holding tank 26 etc. in after four sections Minton dryer 25 dryings.
In the present embodiment, the ethyl acetate recovery system is provided with interchanger 35, and ethyl acetate still kettle top is provided with vapour outlet and is communicated with the heat transfer tube of interchanger 35, by interchanger ethyl acetate is condensed into liquid, realize the recycling of ethyl acetate, reduce the wastage.
As further improvement, present embodiment also comprises five sections nonane diacid recovery systems, described five sections nonane diacid recovery systems comprise five sections crystallization kettles 27, five sections equipment for separating liquid from solid 28 and five sections Minton dryers 29, the material that nonane diacid holding tank 26 is collected enters five sections equipment for separating liquid from solid 28 after five sections crystallization kettle 27 crystallizations, the solid material outlet of five sections equipment for separating liquid from solid 28 is communicated with the material inlet of five sections Minton dryers 29, the liquid material outlet of five sections equipment for separating liquid from solid 28 is communicated with the material inlet of five sections crystallization kettles 27, described five sections crystallization kettles 27 are provided with vacuum orifice and are communicated with vacuum system II 5, five sections crystallization kettle 27 inner chambers are communicated with ethyl acetate supply line 13, the heating interlayer of five sections crystallization kettles 27 and steam heating pipeline 2, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with; During work, the nonane diacid solid of collecting in the nonane diacid holding tank 26 enters five sections crystallization kettles 27 and adopts ethyl acetate to carry out crystallization treatment, after the solidliquid mixture that crystallization produces separates by five sections equipment for separating liquid from solid, separating obtained solid is dry and enter and deposit jar 37 storages by drying installation, nonane diacid solid in the storage tank 37 returns reactor in proportion and carries out once more refining the purification, then got back in the ethyl acetate still kettle by five sections equipment for separating liquid from solid, 28 separating obtained ethyl acetate solutions and to distill recovery, distillation is reclaimed the nonane diacid solid that generates and is then adopted storage tank 38 storages because of foreign matter content is higher separately and sell as industrial grade azelaic acid.
As further improvement, in the present embodiment, further, also comprise ethyl acetate relay tank 29, the liquid material outlet of described five sections equipment for separating liquid from solid 28 communicates through the material inlet of ethyl acetate relay tank 29 with ethyl acetate still kettle 22; During device work, can be temporary by the ethyl acetate solutions that five sections equipment for separating liquid from solid 28 are separating obtained at the ethyl acetate relay tank, treat repeatedly to collect make the storage of ethyl acetate relay tank full after, the property separation is purified again, reduces process procedure, reduces cost.
As further improvement, in the present embodiment, three sections refining systems also comprise assisted vacuum drying installation 30, described assisted vacuum drying installation 30 is two covers and is separately positioned on after three sections crystallization kettles of preceding two covers and is communicated with the material inlet of three sections crystallization kettles of next crystalline element separately that described assisted vacuum drying installation is provided with vacuum orifice and is communicated with vacuum system III.
As further improvement, in the present embodiment, described vacuum system III comprises vacuum sub-system I 30, vacuum sub-system II 31 and vacuum sub-system III 32, described dissolution kettle 14, three sections crystallization kettles of first cover and the first vacuum orifice that overlaps the assisted vacuum drying installation are communicated with vacuum sub-system I, the 2nd vacuum orifice that overlaps three sections crystallization kettles and the 2nd cover assisted vacuum drying installation is communicated with vacuum sub-system II 31 respectively, and the vacuum orifice of back 3 three sections crystallization kettles of cover and three sections Minton dryers 17 connects 32 with vacuum sub-system III respectively and leads to.
As improvement, in the present embodiment, two sections crystalline elements are 3 best covers, three sections crystalline elements are 5 best covers, when ensureing the nonane diacid refining effect, reduce device laid down cost, described elementary insulation filtration unit and secondary insulation filtration unit are hot-water filter, described one section equipment for separating liquid from solid, two sections equipment for separating liquid from solid, three sections equipment for separating liquid from solid, four sections equipment for separating liquid from solid and five sections equipment for separating liquid from solid are whizzer, described one section Minton dryer, two sections Minton dryers, three sections Minton dryers, four sections Minton dryers, five sections Minton dryers and assisted vacuum drying installation are DoubletaperedVacuumdrier.
As further improvement, in the present embodiment, the negative pressure pipe of four sections Minton dryers and five sections Minton dryers is communicated with vacuum system II, reduces the device manufacturing cost and avoids mutual pollution between the system.
As further improvement, in the present embodiment, five sections crystallization kettles and ethyl acetate still kettle are shared, and described four sections equipment for separating liquid from solid and five sections equipment for separating liquid from solid are shared, described four sections Minton dryers and five sections Minton dryers are shared, reduce the device manufacturing cost.
As further improvement, present embodiment also comprises holding tank 33, the vacuum orifice of reactor, dissolution kettle, ethyl acetate still kettle, each section crystallization kettle, each section Minton dryer and assisted vacuum drying installation is provided with holding tank respectively and is communicated with pumped vacuum systems by holding tank, the material dust of being taken away by vacuum system is collected jar interception and storage, reduce material loss, increase economic efficiency.
Refrigerating fulid holding tank 36 also is set in the present embodiment, and after each section crystallization kettle refrigerating process finished, it is temporary to wait that getting back to the refrigerating fulid plenum system uses once again that refrigerating fulid enters refrigerating fulid holding tank 36.
Explanation is at last, although the utility model is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical solution of the utility model, and not breaking away from the aim and the scope of technical solutions of the utility model, it all should be encompassed in the middle of the claim scope of the present utility model.
Claims (9)
1. a nonane diacid is made with extra care the serialization production equipment of purifying, comprise reactor, steam heating system, water coolant plenum system and pumped vacuum systems, described steam heating system is provided with the steam heating pipeline, described water coolant plenum system is provided with cooling water circulation pipeline, it is characterized in that: described pumped vacuum systems comprises vacuum system I, vacuum system II and vacuum system III;
Also comprise one section refining system, two-section refinement system, three sections refining systems;
Described one section refining system comprises the elementary insulation filtration unit that sets gradually along the material direct of travel, one section crystalline element and one section Minton dryer, the material outlet of described reactor is communicated with the material inlet of elementary insulation filtration unit, described one section crystalline element comprises one section crystallization kettle and one section equipment for separating liquid from solid, the material outlet of described one section crystallization kettle links to each other with the material inlet of one section equipment for separating liquid from solid, described one section crystalline element is 1-3 cover and series connection successively, described reactor, each overlaps one section crystallization kettle and one section Minton dryer and vacuum orifice is set respectively and is communicated with vacuum system I;
Described two-section refinement system comprises two sections crystalline elements and two sections Minton dryers, described two sections crystalline elements comprise two sections crystallization kettles and two sections equipment for separating liquid from solid, the material outlet of described two sections crystallization kettles is communicated with the material inlet of two sections equipment for separating liquid from solid, described two sections crystalline elements are 2-4 cover and series connection successively, the material outlet of described one section Minton dryer is communicated with the material inlet of two sections crystallization kettles of first cover, the solid material outlet of two sections equipment for separating liquid from solid of tail cover is communicated with the material inlet of two sections Minton dryers, described ethyl acetate plenum system is provided with the ethyl acetate supply line and is communicated with material inlet of two sections crystallization kettles of each cover, and each overlaps two sections crystallization kettles and two sections Minton dryers and vacuum orifice is set respectively and is communicated with vacuum system II;
Described three sections refining systems comprise the dissolution kettle that sets gradually along the material direct of travel, secondary insulation filtration unit, three sections crystalline elements and three sections Minton dryers, described three sections crystalline elements comprise three sections crystallization kettles and three sections equipment for separating liquid from solid, the material outlet of three sections crystallization kettles is communicated with the material inlet of three sections equipment for separating liquid from solid, described three sections crystalline elements are 4-6 cover and series connection successively, the material of described two sections Minton dryers enters secondary insulation filtration unit filtration after entering the dissolution kettle dissolving, filtrate is more successively through three sections crystallization kettle crystallizations of each cover, the material outlet of three sections crystallization kettles of end cover is communicated with the material outlet of three sections equipment for separating liquid from solid, the solid material outlet of three sections equipment for separating liquid from solid is communicated with dissolution kettle with three sections Minton dryer material inlets, each overlaps three sections crystallization kettles and three sections Minton dryers and vacuum orifice is set respectively and is communicated with vacuum system III;
Also comprise ultrapure water plenum system and refrigerating fulid plenum system, described ultrapure water plenum system is provided with the ultrapure water supply line, described refrigerating fulid plenum system is provided with the refrigerating fulid circulation line, the inner chamber of described reactor, one section crystallization kettle, dissolution kettle and three sections crystallization kettles is communicated with the ultrapure water supply line respectively, and the heating interlayer of reactor, one section crystallization kettle, two sections crystallization kettles, dissolution kettle and three sections crystallization kettles all is communicated with steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line.
2. the refining serialization production equipment of purifying of nonane diacid according to claim 1, it is characterized in that: also comprise four sections ethyl acetate recovery systems, described four sections ethyl acetate recovery systems comprise the ethyl acetate withdrawing can, the ethyl acetate still kettle, ethyl acetate distillate storage tank, ethyl acetate distillation tail washings storage tank, four sections equipment for separating liquid from solid, four sections Minton dryers and nonane diacid holding tank, the liquid material outlet of respectively overlapping two sections equipment for separating liquid from solid in the described two-section refinement system is communicated with the material inlet of ethyl acetate withdrawing can, the material outlet of ethyl acetate withdrawing can is communicated with the material inlet of ethyl acetate still kettle, the distillate that the ethyl acetate still kettle produces enters ethyl acetate distillate storage tank, the distillation tailing that produces enters four sections equipment for separating liquid from solid by ethyl acetate distillation tail washings storage tank, the liquid material outlet of four sections equipment for separating liquid from solid is communicated with the material inlet of ethyl acetate withdrawing can, Gu the material outlet is communicated with the material inlet of nonane diacid holding tank through four sections Minton dryers, the vacuum orifice of described ethyl acetate still kettle and four sections Minton dryers is communicated with vacuum system II respectively, the inner chamber of ethyl acetate still kettle is communicated with the ethyl acetate supply line, the heating interlayer of ethyl acetate still kettle respectively with the steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with.
3. the refining serialization production equipment of purifying of nonane diacid according to claim 2, it is characterized in that: also comprise five sections nonane diacid recovery systems, described five sections nonane diacid recovery systems comprise five sections crystallization kettles, five sections equipment for separating liquid from solid and five sections Minton dryers, the material that described nonane diacid holding tank is collected enters five sections equipment for separating liquid from solid after five sections crystallization kettle crystallizations, the solid material outlet of described five sections equipment for separating liquid from solid is communicated with the material inlet of five sections Minton dryers, the liquid material outlet of five sections equipment for separating liquid from solid is communicated with the material inlet of ethyl acetate still kettle, the vacuum orifice of described five sections crystallization kettles and five sections Minton dryers is communicated with vacuum system II respectively, five sections crystallization kettle inner chambers are communicated with the ethyl acetate supply line, the heating interlayer of five sections crystallization kettles and steam heating pipeline, cooling water circulation pipeline and refrigerating fulid circulation line are communicated with.
4. the refining serialization production equipment of purifying of nonane diacid according to claim 3, it is characterized in that: also comprise the ethyl acetate relay tank, the liquid material outlet of described five sections equipment for separating liquid from solid communicates through the material inlet of ethyl acetate relay tank with the ethyl acetate still kettle.
5. the refining serialization production equipment of purifying of nonane diacid according to claim 4, it is characterized in that: described three sections refining systems also comprise the assisted vacuum drying installation, described assisted vacuum drying installation is two covers and is separately positioned on after three sections crystallization kettles of preceding two covers and is communicated with the material inlet of three sections crystallization kettles of next crystalline element separately that described assisted vacuum drying installation is provided with vacuum orifice and is communicated with vacuum system III.
6. the refining serialization production equipment of purifying of nonane diacid according to claim 5, it is characterized in that: described vacuum system III comprises vacuum sub-system I, vacuum sub-system II and vacuum sub-system III, the vacuum orifice of described dissolution kettle, three sections crystallization kettles of first cover and first cover assisted vacuum drying installation is communicated with vacuum sub-system I, the 2nd vacuum orifice that overlaps three sections crystallization kettles and the 2nd cover assisted vacuum drying installation is communicated with vacuum sub-system II respectively, and the vacuum orifice of back 2-4 three sections crystallization kettles of cover and three sections Minton dryers is communicated with vacuum sub-system III respectively.
7. the refining serialization production equipment of purifying of nonane diacid according to claim 6, it is characterized in that: described two sections crystalline elements are 3 covers, described three sections crystalline elements are 5 covers, described elementary insulation filtration unit and secondary insulation filtration unit are hot-water filter, described one section equipment for separating liquid from solid, two sections equipment for separating liquid from solid, three sections equipment for separating liquid from solid, four sections equipment for separating liquid from solid and five sections equipment for separating liquid from solid are whizzer, described one section Minton dryer, two sections Minton dryers, three sections Minton dryers, four sections Minton dryers, five sections Minton dryers and assisted vacuum drying installation are DoubletaperedVacuumdrier.
8. the refining serialization production equipment of purifying of nonane diacid according to claim 7, it is characterized in that: described five sections crystallization kettles and ethyl acetate still kettle are shared, described four sections equipment for separating liquid from solid and five sections equipment for separating liquid from solid are shared, and described four sections Minton dryers and five sections Minton dryers are shared.
9. the refining serialization production equipment of purifying of nonane diacid according to claim 8, it is characterized in that: also comprise holding tank, the vacuum orifice of described reactor, dissolution kettle, ethyl acetate still kettle, each section crystallization kettle, each section Minton dryer and assisted vacuum drying installation is provided with holding tank respectively and is communicated with pumped vacuum systems by holding tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202068291U CN201587916U (en) | 2009-10-27 | 2009-10-27 | Continuous production device for nonandioic acid refining and purification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202068291U CN201587916U (en) | 2009-10-27 | 2009-10-27 | Continuous production device for nonandioic acid refining and purification |
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|---|---|
| CN201587916U true CN201587916U (en) | 2010-09-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009202068291U Expired - Fee Related CN201587916U (en) | 2009-10-27 | 2009-10-27 | Continuous production device for nonandioic acid refining and purification |
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| CN (1) | CN201587916U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372549A (en) * | 2019-06-19 | 2019-10-25 | 江阴长盛化工有限公司 | A kind of D8 thermo-sensitive material environmental protection preparation system |
| CN111533769A (en) * | 2020-05-09 | 2020-08-14 | 马鞍山市天泰生物科技有限公司 | Preparation method of glucosamine hydrochloride granules |
-
2009
- 2009-10-27 CN CN2009202068291U patent/CN201587916U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372549A (en) * | 2019-06-19 | 2019-10-25 | 江阴长盛化工有限公司 | A kind of D8 thermo-sensitive material environmental protection preparation system |
| CN110372549B (en) * | 2019-06-19 | 2024-07-23 | 江阴长盛化工有限公司 | D8 thermosensitive material environment-friendly preparation system |
| CN111533769A (en) * | 2020-05-09 | 2020-08-14 | 马鞍山市天泰生物科技有限公司 | Preparation method of glucosamine hydrochloride granules |
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