CN205676397U - Plasticizer of mixed ester pilot-plant - Google Patents

Plasticizer of mixed ester pilot-plant Download PDF

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Publication number
CN205676397U
CN205676397U CN201620543964.5U CN201620543964U CN205676397U CN 205676397 U CN205676397 U CN 205676397U CN 201620543964 U CN201620543964 U CN 201620543964U CN 205676397 U CN205676397 U CN 205676397U
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charging aperture
discharging opening
centrifuge
reactor
condenser
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CN201620543964.5U
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黄裕娥
仓理
张东海
王翔
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Nanjing Polytechnic Institute
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Nanjing Polytechnic Institute
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

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Abstract

The utility model discloses a kind of plasticizer of mixed ester pilot-plant.The charging aperture of the discharging opening and the first centrifuge that purify still is connected, and the first discharge hole of centrifugal machine is connected with the charging aperture of decolouring still, and the discharging opening of decolouring still is connected with defecator charging aperture, and the discharging opening of defecator is connected with the charging aperture of cooling tank;The discharging opening of cooling tank and the charging aperture of the second centrifuge are connected, and the discharging opening of the second centrifuge is connected with the charging aperture of reactor, and the top liquid outlet of reactor and the charging aperture of the first condenser are connected;The discharging opening of the first condenser is connected with the charging aperture of decanter, and oil phase is returned reactor by the liquid outlet of decanter;Discharging opening and the second condenser charging aperture bottom reactor are connected, and the charging aperture of the second condenser discharging opening and the 3rd centrifuge is connected, and two discharging openings of the 3rd centrifuge connect the charging aperture of the collecting tank of catalyst recycling can and collection mixed ester respectively.The product of this utility model synthesis can reduce waste discharge, conservation of nature environment.

Description

Plasticizer of mixed ester pilot-plant
Technical field
This utility model belongs to the preparation field of chemistry carboxylate, trial assembly in more particularly a kind of plasticizer of mixed ester Put.
Background technology
Pyromellitic acid anhydride, is called for short PMDA, is a kind of important industrial chemicals, is widely used as intermediate.All benzene four Formic acid dianhydride is prepared with air gaseous oxidation by durol.Owing to course of reaction existing selectivity of catalyst, Activity, the various factors such as the control of reaction condition and exchange of reaction heat, thus there will be side reaction in various degree, Causing containing impurity in the pyromellitic acid anhydride product obtained, these impurity are cis-butenedioic anhydride, inclined acid anhydride, dimethyl phthalic anhydride and durene quinone Deng, content is all between 2%-5%.If these impurity are not used, not only result in the pollution of environment, and waste a large amount of Important resource.And diisooctyl maleate and the different monooctyl ester of trimellitic acid three are all the plasticising that performance is the most excellent Agent, is also critically important industrial chemicals simultaneously.
Diisooctyl maleate is a kind of important fine chemical product, can be used for coating, binding agent, rubber, stone The aspects such as oil additive, are also the main intermediate of synthesis penetrating agent, and itself also has good permeability, grinding at insecticides adjuvant System plays a very important role.
The different monooctyl ester of trimellitic acid three (being called for short TOTM) is the plasticizer that a kind of performance is the most excellent, has volatility little, Animal migration is low, Heat stability is good, has the features such as the fabulous compatibility and processability with polrvinyl chloride, can be widely used in polychlorostyrene second The processing aid of the various kinds of resin such as the copolymer such as alkene, polyethylene, celluloid, cellulose acetate, cellulose butyrate, the suitableeest For manufacturing heatproof, electrical insulating property requires high polyvinyl chloride resin electricity plastics;Phthalic acid di-isooctyl (being called for short DOTP) is polychlorostyrene second Alkene new plasticizer, extraction heat-resisting, cold-resistant, anti-, flexibility is good and PVC has the good compatibility.
The liquid acid such as esterification concentrated sulphuric acid are as catalyst, although catalysis activity is high, response speed is fast, but easily Generation three-waste pollution, etching apparatus are serious, product is difficult to reclaim.The liquid acid catalysts such as concentrated sulphuric acid are badly in need of being substituted.With The raising of people's living standard, environmental conservation is proposed the highest requirement.
1979, the Hino of Japan really et al. successfully synthesized for the first time without any halogen can be at 500 DEG C of high temperature The SO42-/WxOy type solid super-strong acid of lower application.It is with some metal-oxide as carrier, consolidating with SO42-as loaded article Body catalyst.Later, wolframic acid and molybdate dipping ZrO2 were prepared WO3/ZrO2, MoO3/ZrO2 solid super strong again by Arata etc. Acid, although its acidity is more slightly lower than SO42-/ZrO2 but still stronger 100 times than 100%H2SO4.Owing to this kind of solid super-strong acid holds Easily preparation and preservation, particularly it is compared with halogen-containing solid super-strong acid in liquid acid, has not etching apparatus, does not pollute ring Border, can at up to 500 DEG C the feature such as use, cause people and obtain broad interest.Root is according to the literature, it has been found that this kind of Alkane isomerization, olefines double bond isomerizing, esterification, dehydration of alcohols, acylated, polymerization, methane ethylene are gathered by halogen-free solid super-strong acid Many reactions such as conjunction, lique faction of coal all show the highest catalysis activity, even also show that some reaction at normal temperatures very High activity and selectivity, illustrates that they are very promising new catalytic materials of class.Document report SO42-/ ZrO2-Fe2O3-SiO2 is successfully prepared butanoic acid acetonyl ester, and rare-earth solid superacid SO42-/TiO2/La3+ successfully synthesizes horse Carrying out dibutyl phthalate, SO42-/ZrO2-TiO2 is successfully prepared Fructus Fragariae Ananssae ester etc..SO42-/TiO2 has good catalysis activity, as Fruit adds Al in preparation process, can improve catalytic performance, carry out Pyromellitic Acid four with SO42-/TiO2-Al2O3 different The preparation of monooctyl ester has had document to report.
Some external developed countries, the high-carbon plasticizer produced such as the country such as the U.S., West Europe is evolving, and yield is not Disconnected increase, and the production of China's current more than C9 high-carbon plasticizer alcohol is the most blank.There is the equal benzene tetramethyl of set more than 70 in the whole nation at present Acid device, the most about produces more than 100,000 tons C10 mixed acid anhydride by-products, and current its by-product of all production enterprises is all committee Torr fixed-end forces company processes, and processing cost is high, does not meets cleaning production, energy-saving and emission-reduction, the social consensus of recycling economy and warp Ji theory, does not more play the using value of its by-product, causes the wasting of resources, if its by-product can comprehensively utilize Come, on the one hand can produce certain economic benefit, on the other hand can reduce environmental pollution.
The technique of terephthalic acid residue production DOTP is in yueyang, hunan petrochemical plant industrialized production, and it is industrial Change product index and reach the standard of domestic like product.DOP, TOTM, TOPM technique document all has been reported that, and has built up work Industry process units.So, with mixed acid anhydride and isooctanol, the esterification as raw material is theoretically feasible.With equal four Toluene oxidation its by-product C10 mixed acid anhydride be Material synthesis plasticizer of mixed ester be a kind of novel compound plasticizer, mixed Compound possesses the character of one-component material, and mixed ester has the plasticising performance of mono-ester component, and has compound plasticising effect Really.
Utility model content
1, the purpose of this utility model.
This utility model is in order to solve waste discharge in prior art, the problem polluting environment, it is possible to generate the mixed of environmental protection Close ester plasticiser and propose a kind of plasticizer of mixed ester pilot-plant.
2, the technical scheme that this utility model is used.
The plasticizer of mixed ester pilot-plant that the utility model proposes, including purifying still, decolouring still, reactor;First from Scheming, the second centrifuge, the 3rd centrifuge;Defecator;Isooctanol basin, cooling tank, catalyst recycling can, collecting tank;The One condenser, the second condenser, the 3rd condenser;Decanter;The described discharging opening purifying still and the charging of the first centrifuge Mouth is connected, and the first described discharge hole of centrifugal machine is connected with the charging aperture of decolouring still, the discharging opening of described decolouring still and filtration Device charging aperture is connected, and the discharging opening of defecator is connected with the charging aperture of cooling tank;The discharging opening of cooling tank and second is centrifuged The charging aperture of machine is connected, and the discharging opening of the second centrifuge is connected with the charging aperture of reactor, the top liquid outlet of reactor and the The charging aperture of one condenser is connected;The discharging opening of the first condenser is connected with the charging aperture of decanter, and the liquid outlet of decanter will Oil phase after the layering of water, oil phase returns reactor;After the reaction of reacted still, by the discharging opening bottom reactor and the second condensation Device charging aperture is connected, and the charging aperture of the second condenser discharging opening and the 3rd centrifuge is connected, two discharging openings of the 3rd centrifuge Connect the charging aperture of the collecting tank of catalyst recycling can and collection mixed ester respectively.
In order to collect isooctanol reduce on generate plasticizer of mixed ester impact, the liquid outlet of described decanter with The charging aperture of isooctanol basin is connected, and the discharging opening of isooctanol basin is connected with the charging aperture of reactor.
In order to enter cooling tank cooling process by carrying out Regeneration Treatment liquid after filtration, also include the first pump, described The discharging opening of defecator be connected with the charging aperture of cooling tank through the first pump.
In order to return in reactor by oil phase, also include the second pump, the discharging opening warp of described isooctanol basin Cross the second pump to be connected with the charging aperture of reactor.
For collection catalyst and product mixed ester, also include the 3rd pump, the second described condenser discharging opening Charging aperture through the second pump and the 3rd centrifuge is connected.
In order to use water vapour equilibrium heating, described purification still, the still that decolours, the tank body of reactor use and are passed through water The sandwich of steam.
In order to discharge the mother solution purified in still, described purification still is additionally provided with and connects leakage fluid dram with wastewater treatment equipment.
In order to improve filter effect, described defecator is active carbon filtering device.
In order to discharge aqueous phase, decanter is additionally provided with the discharge outlet processed by aqueous phase to wastewater treatment equipment.
3. the beneficial effects of the utility model.
(1) structure that this utility model is used, can generate with durol oxidation section by-product as primary raw material, Synthesizing plasticizer of mixed ester product with 2-Ethylhexyl Alcohol (isooctanol), this product and its production equipment the most still belong to blank.
(2) this product is to reducing waste discharge, protecting environment extremely advantageous;Effectively prevent environment be contaminated and persecute, Protecting ecology balance, ensure health, meet the requirement of sustainable economic development that there is extensive Utilization prospects.
Accompanying drawing explanation
Fig. 1 is this utility model system logic structure figure.
F101 purifies still, F102 decolours still, F103 reactor;M101 the first centrifuge, M102 the second centrifuge, M103 3rd centrifuge;G101 defecator;V101 isooctanol basin, V102 cooling tank, V103 catalyst recycling can, V104 collect Tank;P101 the first pump, P102 the second pump, P103 the 3rd pump;E101 the first condenser, E102 the second condenser, E103 the 3rd are cold Condenser;Q101 decanter.
Detailed description of the invention
1, embodiment
The plasticizer of mixed ester pilot-plant that the utility model proposes, including purifying still F101, decolouring still F102, reactor F103;First centrifuge M101, the second centrifuge M102, the 3rd centrifuge M103;Defecator G101;Isooctanol basin V101, cooling tank V102, catalyst recycling can V103, collecting tank V104;First condenser E101, the second condenser E102, Three condenser E103;Decanter Q101;Described purification still F101, the still F102 that decolours, the tank body of reactor F103 use and are passed through The sandwich of water vapour.
The discharging opening of described purification still F101 and the charging aperture of the first centrifuge M101 are connected, described purification still F101 It is additionally provided with and connects leakage fluid dram with wastewater treatment equipment.
The first described centrifuge M101 discharging opening is connected with the charging aperture of decolouring still F102, described decolouring still F102's Discharging opening is connected with defecator G101 charging aperture, and described defecator G101 is active carbon filtering device, its discharging opening warp The charging aperture crossing the first pump P101 and cooling tank V102 is connected;The discharging opening of cooling tank V102 and the charging of the second centrifuge M102 Mouth is connected, and the discharging opening of the second centrifuge M102 is connected with the charging aperture of reactor F103, the top liquid outlet of reactor F103 It is connected with the charging aperture of the first condenser E101;The discharging opening of the first condenser E101 is connected with the charging aperture of decanter Q101, The liquid outlet of decanter Q101 is connected with the charging aperture of isooctanol basin V101, and decanter Q101 is additionally provided with at aqueous phase to waste water The discharge outlet that reason device processes.
The discharging opening of described isooctanol basin V101 is connected through the charging aperture of the second pump P102 and reactor F103;Warp After reactor F103 reaction, it is connected by the discharging opening bottom reactor F103 and the second condenser E102 charging aperture, described The discharging opening of defecator G101 is connected through the charging aperture of the first pump P101 and cooling tank V102, the two of the 3rd centrifuge M103 Individual discharging opening connects the charging aperture of the collecting tank V104 of catalyst recycling can V103 and collection mixed ester respectively.
2, work process:
1) after nitration mixture and water join purification still F101, chuck is passed through steam, makes nitration mixture dissolve formation after heating full And solution, then it is passed through cold water cooling so that boiling point more much higher unit acid out goes out, thus purifies nitration mixture.Subsequently into One centrifuge M101 centrifugation, mother solution to wastewater treatment equipment processes, and solid enters decolouring still F102.
2) in decolouring still F102, the nitration mixture of purification and water add according to mass ratio 1:5, add the activated carbon of 1% and (account for Raw material ratio), chuck is passed through steam and is heated to 70 DEG C, enter defecator G101 after decolouring 20~30min, after activated carbon filters Carrying out Regeneration Treatment, liquid enters cooling tank V102 cooling through the first pump P101 and processes, and enters the second centrifuge M102 after process, Mother solution processes to wastewater treatment equipment, and solid enters reactor F103.
3) in reactor F103, be separately added into processed nitration mixture, isooctanol, the solid acid catalyst (matter of alcohol and acid anhydride Amount ratio is 3.18:1, and catalyst accounts for the 0.3% of total inventory, and in course of reaction, the isooctanol of excess is as water entrainer, reaction is produced Raw water is taken away in reactor, and steam is after the first condenser E101 condensation, and decanter Q101 carries out water, oil phase divides in entrance Layer, aqueous phase to wastewater treatment equipment processes, and oil phase returns in reactor F103, after reacting 3 hours, terminates reaction.
4), after reaction terminates, unreacted isooctanol is steamed from reactor F103, does not enter reactor, enter into In isooctanol basin V101, after isooctanol steams completely, bottom F103, release product and catalyst.
5) product and catalyst are after the second condenser E102 condensation, enter into the 3rd through the 3rd pump P103 and are centrifuged Being centrifuged in machine M103 separating, solid returns in catalyst recycling can V103 and reuses, and liquid is product mixed ester, enters Enter in product collecting tank V104.

Claims (9)

1. a plasticizer of mixed ester pilot-plant, it is characterised in that: include purifying still (F101), decolouring still (F102), reaction Still (F103);First centrifuge (M101), the second centrifuge (M102), the 3rd centrifuge (M103);Defecator (G101);Different Capryl alcohol basin (V101), cooling tank (V102), catalyst recycling can (V103), collecting tank (V104);First condenser (E101), Second condenser (E102), the 3rd condenser (E103);Decanter (Q101);The discharging opening of described purification still (F101) and The charging aperture of one centrifuge (M101) is connected, described the first centrifuge (M101) discharging opening and the charging aperture of decolouring still (F102) Being connected, the discharging opening of described decolouring still (F102) is connected with defecator (G101) charging aperture, and defecator (G101) goes out Material mouth is connected with the charging aperture of cooling tank (V102);The discharging opening of cooling tank (V102) and the charging aperture of the second centrifuge (M102) Being connected, the discharging opening of the second centrifuge (M102) is connected with the charging aperture of reactor (F103), and the top of reactor (F103) goes out The charging aperture of liquid mouth and the first condenser (E101) is connected;The discharging opening of the first condenser (E101) enters with decanter (Q101's) Material mouth is connected, and the oil phase after water, oil phase layering is returned reactor (F103) by the liquid outlet of decanter (Q101);Reacted still (F103), after reaction, discharging opening and the second condenser (E102) charging aperture by reactor (F103) bottom are connected, and second is cold The charging aperture of condenser (E102) discharging opening and the 3rd centrifuge (M103) is connected, and two discharging openings of the 3rd centrifuge (M103) divide Lian Jie catalyst recycling can (V103) and collect the charging aperture of collecting tank (V104) of mixed ester.
Plasticizer of mixed ester pilot-plant the most according to claim 1, the liquid outlet of described decanter (Q101) by water, Oil phase after oil phase layering returns reactor (F103), it is characterised in that: the liquid outlet of decanter (Q101) and isooctanol basin (V101) charging aperture is connected, and the discharging opening of isooctanol basin (V101) is connected with the charging aperture of reactor (F103).
Plasticizer of mixed ester pilot-plant the most according to claim 1, it is characterised in that: also include the first pump (P101), The discharging opening of described defecator (G101) is connected through the charging aperture of the first pump (P101) with cooling tank (V102).
Plasticizer of mixed ester pilot-plant the most according to claim 2, it is characterised in that: also include the second pump (P102),
The discharging opening of described isooctanol basin (V101) is connected through the charging aperture of the second pump (P102) with reactor (F103).
Plasticizer of mixed ester pilot-plant the most according to claim 1, it is characterised in that: also include the 3rd pump (P103), Described the second condenser (E102) discharging opening is connected through the charging aperture of the second pump (P102) with the 3rd centrifuge (M103).
Plasticizer of mixed ester pilot-plant the most according to claim 1, it is characterised in that: described purification still (F101), Decolouring still (F102), the tank body of reactor (F103) use the sandwich being passed through water vapour.
Plasticizer of mixed ester pilot-plant the most according to claim 1, it is characterised in that: described purification still (F101) is also It is provided with and connects leakage fluid dram with wastewater treatment equipment.
Plasticizer of mixed ester pilot-plant the most according to claim 1, it is characterised in that: described defecator (G101) For active carbon filtering device.
Plasticizer of mixed ester pilot-plant the most according to claim 1, it is characterised in that: decanter (Q101) be additionally provided with by The discharge outlet that aqueous phase processes to wastewater treatment equipment.
CN201620543964.5U 2016-06-07 2016-06-07 Plasticizer of mixed ester pilot-plant Active CN205676397U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330448A (en) * 2019-06-19 2019-10-15 江阴长盛化工有限公司 A kind of heat-sensitive paper bisphenol S production system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330448A (en) * 2019-06-19 2019-10-15 江阴长盛化工有限公司 A kind of heat-sensitive paper bisphenol S production system

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