CN111408330A - Ester exchange equipment and method for producing DOTP (dioctyl phthalate) by PET (polyethylene terephthalate) - Google Patents
Ester exchange equipment and method for producing DOTP (dioctyl phthalate) by PET (polyethylene terephthalate) Download PDFInfo
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- CN111408330A CN111408330A CN202010325128.0A CN202010325128A CN111408330A CN 111408330 A CN111408330 A CN 111408330A CN 202010325128 A CN202010325128 A CN 202010325128A CN 111408330 A CN111408330 A CN 111408330A
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Abstract
The invention provides ester exchange equipment and a method for producing DOTP by PET, wherein the equipment comprises an esterification kettle, a condenser, a primary absorption tank and a secondary absorption tank which are sequentially connected, and the primary absorption tank and the secondary absorption tank are arranged behind the condenser to carry out secondary absorption on glycol, so that the key point of esterification is easy to control, the concentration of the glycol is improved by about 2.4 times compared with that of the glycol adsorbed at the first time, and heat energy is saved for glycol refining. A pipeline between the condenser and the primary absorption tank is communicated with a front-stage water tank, PET is dehydrated before DOTP (dot over methyl terephthalate) production, and the dehydrated water enters the front-stage water tank and is not mixed with glycol water, so that the glycol water is recycled and balanced, and the esterification sewage discharge amount is reduced; the early-stage water tank is arranged to collect early-stage water, and the early-stage water is not mixed with other substances, so that the esterification end point is easy to master.
Description
Technical Field
The invention relates to DOTP production equipment and a process method, in particular to ester exchange equipment and a method for producing DOTP by taking PET as a raw material.
Background
Dioctyl terephthalate (DOTP for short) is a plasticizer with excellent performance, has good electric and thermal properties, has good acceleration effect and low volatility when being used on cable materials, is widely used for various products requiring heat resistance and high insulation, is an ideal plasticizer for producing cable materials with the temperature of 70 ℃ and other volatilization-resistant PVC products, has good cold resistance, and is an excellent environment-friendly plasticizer.
In the traditional DOTP production method, terephthalic acid and octanol are used as raw materials to directly carry out esterification reaction, but the price of the terephthalic acid raw materials is higher, so that the production cost is higher. In order to reduce the production cost, in recent years, the process for producing DOTP by using polyester (mainly comprising polyethylene terephthalate) waste as a raw material and performing ester exchange reaction with isooctanol has been industrialized.
The existing equipment for producing DOTP by taking PET as a raw material is shown in figure 1, PET, a catalyst and octanol are added into an esterification kettle 2 for esterification reaction, the whole esterification process is divided into two steps, namely alcoholysis and ester exchange, azeotropic distillation of ethylene glycol and octanol is carried out, and after condensation by a condenser 10, the ethylene glycol condensate is absorbed by an absorption tank 6. The PET ester exchange method produces DOTP, whether esterification is qualified is judged by testing glycol condensed in a condenser 10, if the glycol is detected to be not more than 2% after condensation, the existing production equipment uses an absorption tank 6 to carry out primary absorption, the glycol cannot be completely absorbed and returns to an esterification kettle, the detection is difficult to be qualified, the production difficulty is high, and the esterification end point is not well controlled.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides ester exchange equipment and method for producing DOTP by PET, so as to solve the technical problems.
The invention is realized by the following technical scheme that firstly, ester exchange equipment for producing DOTP by PET is provided, which comprises an esterification kettle, wherein the top of the esterification kettle is communicated with one end of a condenser, the other end of the condenser is communicated with the top of a primary absorption tank, the top of the primary absorption tank is communicated with a secondary absorption tank, the secondary absorption tank is also communicated with the esterification kettle, a front-stage water tank is communicated on a pipeline between the condenser and the primary absorption tank, the position of the condenser is higher than the positions of the primary absorption tank and the secondary absorption tank, and the position of the secondary absorption tank is higher than the position of the primary absorption tank.
Preferably, the charging opening of the esterification kettle is communicated with a bin, and a discharger is arranged between the bin and the charging opening of the esterification kettle;
the unloader includes the unloading chamber, unloading chamber top intercommunication the feed bin, unloading chamber bottom is through the valve intercommunication the charge door of esterification cauldron, unloading chamber outer wall is fixed with driving motor, driving motor's axis of rotation fixed connection pivot the pivot level set up in the unloading intracavity, just be provided with the blade in the pivot, the blade is "X" shape and distributes.
Preferably, be provided with the rapping device on the outer wall of feed bin, the rapping device includes vibrating motor, vibrating motor's base is fixed in on the outer wall of feed bin, be fixed with the eccentric wheel in vibrating motor's the axis of rotation.
Preferably, a vibration-proof device is arranged between the bin and the discharger.
Preferably, the discharge port of the esterification kettle is communicated with a filter, the filter comprises an outer cylinder and an inner cylinder, a stirring shaft is arranged in the inner cylinder, a scraper and a slag discharge auger are fixed on the stirring shaft, and the directions of the scraper and the slag discharge auger are opposite; the inner cylinder body is provided with a feed inlet and a slag discharge port communicated with the outside, and the outer cylinder body is provided with a filtrate outlet; the wall of the inner cylinder is of a screen mesh structure.
Preferably, the bottom of the filter is provided with at least one blowing and blocking opening.
Preferably, the earlier stage water tank is communicated with the ethylene glycol collection tank, the secondary absorption tank is communicated with the water tank, and the esterification kettle is communicated with the octanol tank.
The invention also provides an ester exchange method for producing DOTP by PET, in the esterification process, glycol and octanol are subjected to azeotropy, and after condensation by a condenser, glycol condensate is sequentially absorbed by the primary absorption tank and the secondary absorption tank for two times.
Preferably, the primary absorption tank is filled with water in advance, the secondary absorption tank is filled with water in advance to a preset liquid level, and the esterification is completed when the interface of the secondary absorption tank reaches a set height.
Preferably, in the esterification process, the glycol and the octanol are subjected to azeotropic distillation, and after the glycol and the octanol are condensed by a condenser, the octanol floats upwards and returns to the esterification kettle by potential difference, and the esterification is performed in a reciprocating cycle.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
the invention provides ester exchange equipment and a method for producing DOTP (dioctyl terephthalate) by PET (polyethylene terephthalate), wherein the equipment comprises an esterification kettle, the top of the esterification kettle is communicated with one end of a condenser, the other end of the condenser is communicated with the top of a primary absorption tank, the top of the primary absorption tank is communicated with the bottom of a secondary absorption tank, the secondary absorption tank is also communicated with the esterification kettle, a front-stage water tank is communicated on a pipeline between the condenser and the primary absorption tank, the position of the condenser is higher than the positions of the primary absorption tank and the secondary absorption tank, and the position of the secondary absorption tank is higher than the position of the primary absorption tank. The method comprises the steps that in the esterification process, glycol and octanol are subjected to azeotropic distillation, and after condensation through a condenser, glycol condensate sequentially passes through a primary absorption tank and a secondary absorption tank to be absorbed twice.
The ester exchange equipment for producing DOTP by PET provided by the invention is provided with the primary absorption tank and the secondary absorption tank, and is used for carrying out secondary absorption on glycol, the position of a condenser is required to be 3.5 meters higher than that of the secondary absorption tank, because the density of octanol is 0.83 and the density of glycol is 1.1, the pressure difference is calculated according to the specific gravity, when the liquid in a liquid pipeline behind the condenser is 1.8 meters higher than that of the secondary absorption tank, the liquid is balanced, and according to the siphon principle, the liquid can flow into the secondary absorption tank after being increased, namely the pressure in the liquid pipeline is larger than the water pressure resistance of the primary absorption tank. Before esterification, water is added in the secondary absorption tank in advance to a preset interface, most of glycol is dissolved in the water in the primary absorption tank after reaction, octanol and a small part of glycol are pressed into the secondary absorption tank by the difference of potential, and after the glycol is absorbed, the octanol returns to the esterification tank through an overflow port on the secondary absorption tank. And (3) all the increased liquid levels of all the produced glycol after being absorbed by water are embodied in the secondary absorption tank, and when the glycol is produced to a set boundary surface, the reaction end point is reached, and the reaction is finished. The two-stage adsorption designed by the invention enables the esterification key to be easily controlled, improves the concentration of the glycol by about 2.4 times compared with the glycol adsorbed once, and saves heat energy for glycol refining.
In the ester exchange equipment for producing DOTP by PET, a pipeline between a condenser and a primary absorption tank is communicated with a prophase water tank, when PET raw materials are waste materials, the PET waste materials need to be crushed in advance, and part of water needs to be added during crushing, so that an esterification kettle needs to be heated and dehydrated first before DOTP production, and a water inlet of the prophase water tank can be opened during dehydration to enable the dehydrated prophase water to enter the prophase water tank; the collected early-stage water is light-polluted condensate water which can be reused for the second time; meanwhile, the early-stage water tank is special for collecting early-stage water, so that the early-stage water is not mixed with other substances, the esterification end point is easy to master, and the esterification end point is reached when the liquid level gauge in the secondary absorption tank reaches a set height because the ethanol is generated in each kettle in a certain amount.
Drawings
For a clearer explanation of the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic diagram showing the structure of a transesterification apparatus for producing DOTP from PET in the prior art.
Fig. 2 is a schematic structural diagram of an ester exchange apparatus for producing DOTP from PET according to an embodiment of the present invention.
Fig. 3 is a schematic position structure diagram of a transesterification apparatus for producing DOTP from PET according to an embodiment of the present invention.
FIG. 4 is a schematic structural diagram of a secondary absorption tank of a transesterification apparatus for producing DOTP from PET according to an embodiment of the present invention.
FIG. 5 is a schematic structural diagram of a discharger of a transesterification apparatus for producing DOTP from PET according to an embodiment of the present invention.
FIG. 6 is a schematic diagram of an external structure of a discharger of a transesterification apparatus for producing DOTP from PET according to an embodiment of the present invention.
Fig. 7 is a schematic structural diagram of a rapper of a transesterification equipment for producing DOTP by PET according to an embodiment of the present invention.
FIG. 8 is a schematic structural diagram of the eccentric wheel of the rapper of the ester exchange equipment for producing DOTP by PET according to the embodiment of the invention.
FIG. 9 is a schematic structural diagram of a filter of a transesterification apparatus for producing DOTP from PET according to an embodiment of the present invention.
Shown in the figure:
1-a storage bin, 2-an esterification kettle, 3-a catalyst tank, 4-a secondary absorption tank, 41-an overflow port, 42-an observation window, 43-an interface meter, a 5-earlier stage water tank, 6-a primary absorption tank, 7-an ethylene glycol collection tank, 8-a water tank, 9-an octanol tank, 10-a condenser, 11-a discharger, 11.1-a discharge cavity and 11.2-a rotating shaft, 11.3-blade, 12-vibrator, 12.1-vibration motor, 12.2-eccentric wheel, 12.3-base, 13-filter, 13.1-outer cylinder, 13.2-inner cylinder, 13.3-stirring shaft, 13.4-scraper, 13.5-slag-out screw, 13.6-feed inlet, 13.7-slag-out port, 13.8-filtrate outlet, 13.9-blowing-blocking port and 14-cloth bag dust removal.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention, shall fall within the protection scope of the present invention.
Referring to fig. 2, a schematic structural diagram of an ester exchange apparatus for producing DOTP from PET according to an embodiment of the present invention is shown.
As can be known from figure 2, the ester interchange equipment of PET production DOTP that this embodiment provided, including esterification kettle 2, esterification kettle 2's top intercommunication condenser 10's one end, the top of overhead tank 6 is once communicated to the other end of condenser 10, overhead tank 6's top intercommunication secondary absorption jar 4, secondary absorption jar 4 passes through overflow mouth 41 intercommunication esterification kettle 2, condenser 10 with intercommunication has earlier stage water pitcher 5 on the pipeline between the overhead tank 6, condenser 10's position is higher than the position of overhead tank 6 and secondary absorption jar 4, just the position of secondary absorption jar 4 is higher than the position of overhead tank 6.
Specifically, in this embodiment, the earlier-stage water tank 5 is communicated with an ethylene glycol collection tank 7, the secondary absorption tank 4 is communicated with a water tank 8, and the esterification kettle 2 is communicated with an octanol tank 9. The whole equipment adopts tertiary installation, as shown in figure 3, the lowest one deck is primary absorption tank 6 and various storage tanks, the middle two decks are earlier stage water tank 5, secondary absorption tank 4, esterification kettle 2, the highest three-layer is feed bin 1, condenser 10, the operation of whole system potential difference, simple process, energy saving, convenient operation, improvement production efficiency, product quality is stable, production is relatively safe, can realize the intermittent production automation.
The condenser 10 of the present embodiment sequentially communicates the primary absorption tank 6 and the secondary absorption tank 4, the condenser 10 is located higher than the primary absorption tank 6 and the secondary absorption tank 4, and the secondary absorption tank 4 is located higher than the primary absorption tank 6. The condenser 10 was located 3.5 m higher than the secondary absorption tank 4, the octanol density was 0.83, the ethylene glycol density was 1.1, the pressure difference was calculated by specific gravity, and when the liquid in the liquid pipe after the condenser 10 was 1.8 m higher than the secondary absorption tank 4, equilibrium was obtained. After the liquid is increased again, the pressure in the pipe is larger than the water pressure resistance of the primary absorption tank 6, and then the liquid can permeate into the secondary absorption tank 4 (siphon principle). The invention carries out secondary adsorption on the glycol through the primary absorption tank 6 and the secondary absorption tank 4, improves the concentration by about 2.4 times compared with the concentration of the primary adsorption, and saves heat energy for subsequent glycol refining.
According to the general design of the device: the ratio of the tank diameter to the height, i.e. the height of the primary absorption tank 6 and the secondary absorption tank 4, is at most 4 meters, which is sufficient for all production plants. In this embodiment, an octanol interface of 1 m is left on the upper part of the secondary absorption tank 4, the primary absorption tank 6 is totally ethylene glycol water, i.e. the height is 3.5 m, and the maximum height of the secondary absorption tank is 3.5 m, i.e. the sum of 3.5 m and 3.5 m is equal to 7 m. Octanol density 0.83, 0.83 × 7m ═ 5.81(5810 mmH)2O); the density of the ethylene glycol water is 1.075, the concentration of ethylene glycol is 60% at the maximum, 1.075 x 7 ═ 1.715(1715 mmH)2O), therefore, when the esterification reaches the end (when qualified), the head difference 1715mmH is reached when the ethanol water interface in the secondary absorption tank 4 reaches the maximum height2O, i.e., the system pressure differential is balanced when the differential is approximately 1800 mm. The whole esterification process in the esterification kettle 2 is at atmospheric pressure, and because a noncondensable gas discharge port is arranged behind the condenser 10, the potential difference is 3.5 meters, which is suitable for all devices with production capacity.
In the invention, the chemical reaction equation for producing DOTP by PET is as follows:
C18H8O4(PET)+C16H36O2(isooctyl alcohol) ═ C1 24H38O4(DOTP)+C1 2H6O2(ethylene glycol);
the molecular weight of PET is 192.1728, the molecular weight of isooctanol is 260.4586, the molecular weight of DOTP is 8.129, and the molecular weight of ethylene glycol is 62.069; assuming 4t of PET input per kettle, 5.4213t of ethylene glycol is required, yielding 8.129t of DOTP and 1.292t of ethylene glycol as by-product.
Designing a primary absorption tank 6:
the feed PET is known to be 4t, the ethylene glycol production is known to be 1.292t, ifThe glycol content in the primary absorption tank 6 is 60%, and then 0.86t of water should be added, and the glycol density is 1.1t/m3The total volume of the liquid after the reaction was 0.863(Water) +1.175m3(ethylene glycol), i.e., the total volume in the primary absorption tank 6 was 2.035m3。
The total volume of the primary absorption tank is 2.035m3The secondary absorption tank is added with water of 0.86m3(ii) a When the first kettle reacts (the content in the first kettle primary absorption tank 6 is less than 60 percent), the liquid level in the primary absorption tank 6 is discharged completely, and 2.035m is discharged3The dilute glycol aqueous solution in the secondary absorption tank 4 is put into the primary absorption tank and is put into the primary absorption tank for 2.035m3Adding water 0.86m into the secondary absorption tank3Adding octanol to the upper overflow port, thus adding 0.86m of water3Tapping 2.153t, and tapping concentration is calculated as:
2.153t (ethylene glycol aqueous solution) -0.86t (water) ═ 1.292t (ethylene glycol)/2.153 t (aqueous solution) ═ 0.6, i.e., 60%.
When the first kettle is esterified (originally started), water is added into the secondary absorption tank 4 to 0.86m3The upper part of the second absorption tank 4 is supplemented with octanol to an overflow port, when the first kettle is esterified qualified, the upper part of the second absorption tank 4 is already provided with octanol with the height of 1 meter, and when the second kettle is added with octanol later, the amount of octanol added into the kettle is added with glycol (1.292 tons, namely 1.175 m)3) I.e. 1.175m more octanol is added in each kettle3When the temperature rises, the back flow is generated, and when the back flow flows to an upper overflow port, the octanol in the kettle is the pumped octanol with the well-matched concentration, so that the octanol which is not compensated in the secondary absorption tank 4 is only added with water of 0.86m3And (4) finishing.
After the reaction is finished, the octanol in the secondary absorption tank 4 can not be completely returned to the esterification kettle, the octanol amount returned to the kettle is equal to the amount of ethylene glycol, when the liquid level in the primary absorption tank 6 is discharged, the liquid level in the secondary absorption tank 4 is filled, half of the octanol at the upper part of the secondary absorption tank 4 is remained in the primary absorption tank 6, and when 0.86m of water is added3When the octanol is floated, the octanol floats upwards. The octanol interface in the primary absorption tank 6 is different only by the amount of ethylene glycol to the overflow port. The secondary canister 4 may be designed to be larger than the primary canister 6. When esterification is qualified, the octanol keeps 1 half high liquid level, and the octanol is ensured to be thoroughly separated.
Designing a secondary absorption tank 4:
before esterification, water was added to interface B (1.175 m) in secondary absorption tank 43) And adding octanol to an overflow port 41 at the upper part, condensing ethylene glycol and octanol replaced by reaction through a condenser 10, then feeding the condensed ethylene glycol and octanol into a primary absorption tank 6, dissolving most of the ethylene glycol in water in the primary absorption tank 6, pressing the octanol and a small part of the ethylene glycol into a secondary absorption tank 4 by means of potential difference, and returning the octanol into the esterification kettle 2 through the overflow port 41 at the upper part of the secondary absorption tank 4 after the ethylene glycol is absorbed. The increased liquid level of all the produced glycol after water absorption is totally reflected in the secondary absorption tank 4, and when the glycol is produced to 1.175m3The reaction is terminated when the reaction reaches the interface A shown in FIG. 8, i.e., the end of the reaction is reached. The secondary absorption tank 4 is provided with two observation windows 42 for observing the liquid level, the two observation windows 42 are respectively arranged at the height positions of the interface A and the interface B, the observation windows 42 are circular, and the central lines of the two observation windows 42 are respectively at the height positions of the interface A and the interface B.
The secondary absorption tank 4 is provided with an interface meter 43, the interface meter 43 is a magnetic turning plate liquid level meter, the density is 0.9, and the density is between the density of water 1 and the density of octanol 0.83.
The PET ester exchange method is used for producing DOTP, whether esterification is qualified or not is glycol condensed by the chemical examination condenser 10, if the glycol is detected to be qualified when the glycol is not more than 2% after condensation, if the glycol is not completely adsorbed, the glycol returns to the esterification kettle 2, even if the reaction reaches the end point, the glycol content brought back exceeds the standard, the detection is difficult to be qualified, so that the glycol content absorbed once is up to 30% at most, and if the glycol content is more than 30%, the glycol content returned to the esterification kettle 2 is detected to be more than 2%, and the glycol can never be qualified. Moreover, the maximum content of the adsorbed glycol is 30% only once, and the energy consumption in the subsequent glycol dehydration refining process is large. According to the equipment provided by the invention, the primary adsorption tank 6 and the secondary adsorption tank 4 are designed to carry out two-stage adsorption, the content of ethylene glycol can reach 60%, the detection is qualified, the content of ethylene glycol is improved, and the energy consumption is reduced for the subsequent ethylene glycol refining process.
When one material adsorbs another (liquid to liquid), there is a direct relationship between the solubility and dissolution rate of the adsorbed liquid. Meanwhile, the concentration of the dissolving solution is related to the concentration of the absorbed solution, and when the concentration of the mixed solution is increased, the discharge concentration of the absorbed solution is in direct proportion, and is generally calculated according to the absorption rate of 93%. If the concentration in the secondary absorption tank 4 is 30%, then 0.3 × 0.93 ═ 0.279, then the absorption liquid content reaches 27.9%, and the absorbed liquid 0.3-0.279 × 0.021, i.e. 2.1%, then the ethylene glycol concentration after testing the condenser 10 is less than 2%, then the ethylene glycol concentration after testing the condenser 10 exceeds 2% if the concentration in the secondary absorption tank 4 reaches 30%, so the concentration in the secondary absorption tank 4 is set to 28%, then 0.28 × 0.93 ═ 0.26, 0.28-0.26 ═ 0.02, i.e. 2%, meets the pass requirement, and therefore, the concentration in the secondary absorption tank 4 should be less than or equal to 28%. In the embodiment, the concentration of the primary absorption tank 6 is 60%, and the concentration of the secondary absorption tank 4 is less than 28%.
The embodiment adopts two-stage adsorption, when esterification is qualified, all the ethylene glycol liquid in the primary adsorption tank 6 is discharged, all the mixed water liquid in the secondary adsorption tank 4 is placed in the primary adsorption tank 6, and 0.86m of water is added into the secondary adsorption tank 43Reciprocating and adding water 0.86m3Out of 2.035m3. The content of the ethylene glycol in the primary absorption tank 6 is 60 percent, and the content of the ethylene glycol in the secondary absorption tank 4 is 22.5 percent.
Each time 2.153t of ethylene glycol aqueous solution is put into the primary absorption tank 6, 1.292t of ethylene glycol is discharged from each reactor, 1.292/2.153 is 0.6, the absorption rate of the primary absorption tank is 85% (because the absorption rate is lower than that of the secondary absorption tank due to concentration relation), namely, the amount of ethylene glycol recovered by the primary absorption tank 6 is 1.292 x 0.85 x 1.0982t, the amount of ethylene glycol entering the secondary absorption tank 4 is 1.292t-1.0982t x 0.1983t, 0.1983t of ethylene glycol is absorbed by 0.86t of water in the secondary absorption tank 4, the ethylene glycol content in the secondary absorption tank 4 is 0.1983/0.86 x 0.225, namely 22.5%, therefore, the ethylene glycol content in the secondary absorption tank 4 is lower than 28%, the ethylene glycol in the secondary absorption tank is lower than 2% after absorption, and when the esterification is qualified, the ethylene glycol content is lower than 2% after a condenser is measured.
Water is added repeatedly for 0.86t, and 2.153t is discharged, wherein the glycol 1.292t is contained, and the content is 1.292/2.153-0.6, namely 60%.
The content in the secondary absorption tank is 22.5 percent;
if the single absorption is carried out, the concentration in the absorption tank is less than 30 percent; according to the general design, a factor of 1.2 is added for the stability, and the ratio of 30%/1.2 is 25%; calculating the concentration increase: the concentration of the secondary absorption ratio adopted by the invention is increased by 2.4 times compared with the primary absorption by only adopting the secondary absorption ratio calculated by theory, wherein the ratio of 60%/25% is 2.4 times.
This embodiment still communicates earlier stage water pitcher 5 on the pipeline between condenser 10 and the primary absorption jar 6, the raw materials PET that this embodiment PET production DOTP adopted is the waste material, the PET waste material needs to be smashed in advance, it needs to add part of water to remove dust during smashing, therefore PET production DOTP need heat earlier dehydration to esterification kettle 2 before esterifying, open the water inlet of water pitcher 5 in earlier stage during the dehydration, make the earlier stage water that deviates from get into water pitcher 5 in earlier stage, this embodiment sets up water pitcher 5 in earlier stage and collects the water that PET deviates from specially, this water does not mix with ethylene glycol water, make ethylene glycol water reuse balance, can alleviate esterification blow off water amount 100%; the collected early-stage water is light-polluted condensate water which can be reused for the second time; meanwhile, the early-stage water tank 5 is specially used for collecting early-stage water, so that the early-stage water is not mixed with other substances, the esterification end point is easy to master, and the esterification end point is reached when the liquid level meter in the secondary absorption tank 4 reaches a set height because the ethanol is generated in each kettle to a certain extent.
Further, in this embodiment, as shown in fig. 5 and fig. 6, a feed inlet of the esterification reactor 2 is communicated with a bin 1, and a discharger 11 is arranged between the bin 1 and the feed inlet of the esterification reactor 2;
The prior esterification kettle 2 is generally provided with one
A feed inlet, wherein during feeding, the screws of the manhole cover need to be loosened, and the manhole is opened for feedingThe feeding through the manhole is long in time, and the feeding is easy to be uneven, so that the stirrer of the esterification kettle 2 is stressed unevenly, and the stirring is easy to stop running and trip when the stirring load is overlarge. The feeding sequence of DOTP production by PET is that firstly octanol is added, the octanol is used as liquid, then PET is added, the PET raw material is crushed terylene wiredrawing leftovers or PET packaging bottles of beverage and food, the PET raw material is granular or powdery, and dust is easily raised and air is polluted when the PET raw material is added.
This embodiment communicates feed bin 1 on esterification reactor 2's charge door, and feed bin 1 seals alone with the material loading, leads to the purification treatment behind the sack dust removal 14 by the draught fan, avoids the raise dust, as shown in fig. 3. Unload feed bin 1 through tripper 11, flange connection feed bin 1's bottom is passed through at tripper 11's top, as shown in fig. 5 and fig. 6, fixed driving motor 11.4 on the chamber 11.1 outer wall of unloading, driving motor 11.4's transmission shaft and pivot 11.2 fixed connection, driving motor 11.4's transmission shaft rotates and drives pivot 11.2 and rotate, thereby it rotates to drive fixed blade 11.3 on the pivot 11.2, blade 11.3 is four, the side is "X" form, inside tripper 11, two opposite faces that use pivot 11.2 as the symmetry axis are spherical, in order to guarantee that blade 11.3 can revolute 11.2 rotations of axle.
When discharger 11 is in the closure state, blade 11.3 just can seal unloading chamber 11.1, feed bin 1 is reinforced the back, the material can not fall if discharger 11 does not start, when needing to throw the material in esterifying kettle 2, open the valve of discharger 11 bottom, start driving motor 11.4, driving motor 11.4 drives pivot 11.2 and rotates, thereby it is rotatory to drive blade 11.3, the material in feed bin 1 falls to between two adjacent blades 11.3, drive the material upset whereabouts by the rotation of blade 11.3, get into esterifying kettle 2 in, reinforced speed can be decided by driving motor 11.4's speed, driving motor 11.4 can set up to inverter motor.
Specifically, be provided with rapping device 12 on the outer wall of feed bin 1, rapping device 12 includes vibrating motor 12.1, vibrating motor 12.1's base 12.3 is fixed in on the outer wall of feed bin 1, be fixed with eccentric wheel 12.2 in vibrating motor 12.1's the axis of rotation.
As shown in fig. 7 and 8, an eccentric wheel 12.2 is fixed on a rotating shaft of a vibration motor 12.1, the structure of the eccentric wheel 12.2 is as shown in fig. 8, the vibration motor 12.1 rotates to drive the eccentric wheel 12.2 to rotate, the vibration motor 12.1 is fixed on the outer wall of the storage bin 1, and the eccentric wheel 12.2 strikes the outer wall of the storage bin 1 to vibrate materials in the storage bin 1, so that the materials can fall down more smoothly. Meanwhile, the eccentric wheel 12.2 rotates to generate centrifugal force, so that the vibration motor 12.1 generates vibration, and the vibration motor 12.1 is fixed on the outer wall of the storage bin 1 to drive the storage bin 1 to vibrate, so that the material falls smoothly.
More specifically, in this embodiment, a vibration-proof device is disposed between the bin 1 and the discharger 11 to prevent the discharger 11 from vibrating. The vibration isolation device can be a rubber pad or a spring, and the structure of the vibration isolation device is not limited by the invention and can play a role in vibration attenuation.
Furthermore, in this embodiment, as shown in fig. 9, the discharge port of the esterification reactor 2 is communicated with a filter 13, the filter 13 includes an outer cylinder 13.1 and an inner cylinder 13.2, a stirring shaft 13.3 is disposed in the inner cylinder 13.2, a scraper 13.4 and a slag discharge auger 13.5 are fixed on the stirring shaft 13.3, and the directions of the scraper 13.4 and the slag discharge auger 13.5 are opposite; the inner cylinder body 13.2 is provided with a feed inlet 13.6 and a slag discharge port 13.7 which are communicated with the outside, and the outer cylinder body is provided with a filtrate outlet 13.8; the section of thick bamboo wall of interior barrel 13.2 is the screen cloth structure, and this embodiment is the steel sheet screen cloth.
The esterified material contains partial particulate matter impurities, the filter 13 is arranged for filtering in the embodiment, the esterified material enters the inner cylinder 13.2 from the feed inlet 13.6, liquid is filtered through the steel plate screen, filter residues are left in the screen, namely the inner cylinder 13.2, the liquid enters the outer cylinder 13.1 through the screen and flows out from the filtrate outlet 13.8, and the discharged liquid can be sent to a distillation still by an impeller pump for subsequent distillation; the left-handed scraper 13.4 and the right-handed slag discharge auger 13.5 are arranged on the stirring shaft 13.3 in the inner cylinder body 13.2, the filter residue left in the inner cylinder body 13.2 is scraped by the scraper 13.4 under the stirring of the stirring shaft 13.3, and is discharged from the slag discharge port 13.7 under the driving of the slag discharge auger 13.5.
Specifically, in the embodiment, two blowing and blocking ports 13.9 are arranged at the bottom of the filter 13, as shown in fig. 9, one blowing and blocking button 13.9 is positioned at the lower part of the outer cylinder 13.1, and the other blowing and blocking button is positioned at the slag discharge port 13.7, and nitrogen can be blown in through the blowing and blocking port 13.9. The blowing blockage opening 13.9 positioned at the lower part of the outer cylinder body 13.1 is used for preventing the screen mesh from being blocked, and the blowing blockage opening 13.9 positioned at the slag discharge opening 13.7 is used for preventing the slag discharge opening 13.7 from being blocked.
The embodiment of the invention provides an ester exchange method for producing DOTP by PET, which comprises the following steps:
feeding: sequentially adding octanol and PET prepared in advance into an esterification kettle 2 according to the amount:
(1) adding octanol, pumping a prepared octanol tank 9 into the esterification kettle 2 according to the scale;
(2) adding PET, and after finishing adding octanol, uniformly adding the PET prepared in the stock bin 1 into the esterification kettle 2 through a discharger 11 under the action of a vibrator 12.
And (3) heating and dehydrating: stirring in the esterification kettle 2, raising the temperature to 170 ℃ for dehydration, and leading the dehydrated water to enter the early-stage water tank 5.
Raw materials PET that this embodiment PET production DOTP adopted is the waste material, the PET waste material need be smashed in advance, it needs to add part of water to remove dust during crushing, consequently PET production DOTP esterify preceding need to esterify 2 interior PET raw materials heat earlier and dewater, open the water inlet of earlier stage water pitcher 5 during the dehydration, make the earlier stage water of deviating from get into earlier stage water pitcher 5, this embodiment dewaters before esterifying earlier, and set up earlier stage water pitcher 5 and collect the water that PET deviates from specially, make the earlier stage water that PET deviates from not mix with ethylene glycol water, make ethylene glycol water reuse balance, can alleviate esterification blow off 100%; the collected early-stage water is light-polluted condensate water which can be reused for the second time; meanwhile, the early-stage water tank 5 is specially used for collecting early-stage water, so that the early-stage water is not mixed with other substances, the esterification end point is easy to master, and the esterification end point is reached when the liquid level meter in the secondary absorption tank 4 reaches a set height because the ethanol is generated in each kettle to a certain extent.
Adding a catalyst: the temperature in the esterification kettle 2 is raised to 183 ℃, and the catalyst metered in the catalyst tank 3 is added into the esterification kettle 2.
Esterification: the whole esterification process is divided into two steps, namely alcoholysis and ester exchange, and the glycol and octanol are subjected to azeotropic distillation, and are condensed by a condenser 10, the glycol condensate sequentially passes through a primary absorption tank 6 and a secondary absorption tank 4, water is filled in the primary absorption tank 6 in advance, water is filled in the secondary absorption tank 4 in advance to a preset liquid level interface B, the octanol floats upwards, the octanol returns to the esterification kettle by virtue of potential difference pressure, and the esterification is circulated repeatedly, and when the interface of the secondary absorption tank 4 reaches a set height interface A, the esterification is carried out to the end point, and the esterification is completed without chemical analysis.
Before esterification, water is added into the secondary absorption tank 4 until the interface B1.175m3And adding octanol to an overflow port 41 at the upper part, condensing ethylene glycol and octanol replaced by reaction through a condenser 10, then feeding the condensed ethylene glycol and octanol into a primary absorption tank 6, dissolving most of the ethylene glycol in water in the primary absorption tank 6, pressing the octanol and a small part of the ethylene glycol into a secondary absorption tank 4 by means of potential difference, and returning the octanol into the esterification kettle 2 through the overflow port 41 at the upper part of the secondary absorption tank 4 after the ethylene glycol is absorbed. The increased liquid level of all the produced glycol after water absorption is totally reflected in the secondary absorption tank 4, and when the glycol is produced to 1.175m3When the reaction reaches the interface A shown in FIG. 8, that is, the end point of the reaction is reached, the reaction is completed, that is, the esterification is completed.
The boiling point of octanol is 183 ℃, the reaction time of glycol boiling point 190 ℃ is more than or equal to 190 ℃ DOTP boiling point 400 ℃, the ester exchange reaction formula is adopted, if the reaction condition is reached, the reaction temperature is more than 190 ℃, so a great deal of octanol is evaporated during the reaction, if the octanol is not condensed and then returns to the esterification kettle 2, namely, the octanol in the esterification kettle 2 is completely evaporated, only PET solid is remained, when the temperature is less than 190 ℃, the glycol cannot be brought out, and side reaction occurs, therefore, the glycol is dissolved in water, the octanol is not dissolved in water, after the glycol is extracted, the octanol returns to the esterification kettle 2, when DOTP is continuously generated, the DOTP content is continuously increased, the temperature is immediately increased, when the temperature is increased to 200-210 ℃, the reaction is fastest, when the molar concentration is 1:3, 210-215 ℃ is used, namely, the reaction end point is reached, namely, all PET is completely reacted, and.
Discharging: after the esterification is qualified, the mixed liquid is filtered by a filter 13, and then the liquid material is sent to distillation by a transfer pump, and the residue is discharged after the material is sent.
Adding ethylene glycol water: when the esterification is qualified, the content of the ethylene glycol in the primary absorption tank 6 is 60%, the volume of the equipment and the water adding amount are designed, and no test analysis is needed. Completely discharging the ethylene glycol aqueous solution in the primary absorption tank 6, completely discharging the ethylene glycol aqueous solution in the secondary absorption tank 4 into the primary absorption tank 6, adding water into the secondary absorption tank 4 again, wherein the added water can be water distilled from the rectification of the ethylene glycol, and adding water into the secondary absorption tank 4 again to a set scale value (interface B) to prepare for the esterification of the next kettle.
When the first kettle is qualified, the water content of the discharged glycol is slightly lower than 60 percent, the glycol content in the second kettle fluctuates slightly up and down at 60 percent, and the analysis in the problem 3 picture shows that the water is added into the secondary absorption tank 4 to 0.86m3Adding octanol into the upper part, increasing ethylene glycol, and decreasing octanol in the tank with increasing ethylene glycol when the ethylene glycol rises to 1.175m3After the reaction, the total volume of the primary absorption tank 6 was 2.035m3Therefore, the liquid in the secondary absorption tank 4 is substantially filled in the primary absorption tank 6.
Of course, the above description is not limited to the above examples, and the undescribed technical features of the present invention can be implemented by or using the prior art, and will not be described herein again; the above embodiments are merely for illustrating the technical solutions of the present invention and not for limiting the present invention, and the present invention has been described in detail with reference to the preferred embodiments, and those skilled in the art should understand that changes, modifications, additions or substitutions which are made by those skilled in the art within the spirit of the present invention are also within the scope of the claims of the present invention.
Claims (10)
1. The utility model provides a PET production DOTP's ester exchange equipment, includes esterification kettle (2), the top of esterification kettle (2) communicates the one end of condenser (10), its characterized in that, the top of another end intercommunication primary absorption jar (6) of condenser (10), the top of primary absorption jar (6) communicates secondary absorption jar (4), secondary absorption jar (4) still communicate esterification kettle (2), condenser (10) with intercommunication has earlier stage water pitcher (5) on the pipeline between primary absorption jar (6), the position of condenser (10) is higher than the position of primary absorption jar (6) and secondary absorption jar (4), the position of secondary absorption jar (4) is higher than the position of primary absorption jar (6).
2. The transesterification apparatus for producing DOTP by PET according to claim 1, wherein a feed port of the esterification reactor (2) is communicated with a bin (1), and a discharger (11) is arranged between the bin (1) and the feed port of the esterification reactor (2);
discharger (11) is including unloading chamber (11.1), unloading chamber (11.1) top intercommunication feed bin (1), unloading chamber (11.1) bottom is through the valve intercommunication the charge door of esterification kettle (2), unloading chamber (11.1) outer wall is fixed with driving motor (11.4), axis of rotation fixed connection pivot (11.2) of driving motor (11.4) pivot (11.2) level set up in unloading chamber (11.1), just be provided with blade (11.3) on pivot (11.2), blade (11.3) are "X" shape and distribute.
3. Transesterification apparatus for the production of DOTP by PET according to claim 2, characterized in that a vibrator (12) is provided on the outer wall of the silo (1), the vibrator (12) comprises a vibration motor (12.1), the base (12.3) of the vibration motor (12.1) is fixed on the outer wall of the silo (1), and an eccentric wheel (12.2) is fixed on the rotation shaft of the vibration motor (12.1).
4. Transesterification plant for the production of DOTP according to claim 3, characterised in that between the silo (1) and the discharger (11) there are provided anti-vibration means.
5. The transesterification equipment for producing DOTP by PET according to claim 4, wherein the discharge hole of the esterification kettle (2) is communicated with a filter (13), the filter (13) comprises an outer cylinder (13.1) and an inner cylinder (13.2), a stirring shaft (13.3) is arranged in the inner cylinder (13.2), a scraper (13.4) and a slag discharge auger (13.5) are fixed on the stirring shaft (13.3), and the directions of the scraper (13.4) and the slag discharge auger (13.5) are opposite; a feed inlet (13.6) and a slag discharge port (13.7) which are communicated with the outside are arranged on the inner cylinder body (13.2), and a filtrate outlet (13.8) is arranged on the outer cylinder body; the wall of the inner cylinder (13.2) is of a screen structure.
6. Transesterification apparatus for the production of DOTP by PET according to claim 5, characterized in that the bottom of the filter (13) is provided with at least one blow-plug (13.9).
7. A transesterification apparatus for DOTP production according to any one of claims 1 to 6, wherein the pre-water tank (5) is connected to a glycol collection tank (7), the secondary absorption tank (4) is connected to a water tank (8), and the esterification tank (2) is connected to an octanol tank (9).
8. An ester exchange method for producing DOTP by PET is characterized in that in the esterification process, glycol and octanol are subjected to azeotropic distillation and condensed by a condenser (10), and glycol condensate passes through a primary absorption tank (6) and a secondary absorption tank (4) in turn to be absorbed twice.
9. A transesterification method of producing DOTP by PET according to claim 8, wherein the primary absorption tank (6) is filled with water in advance, the secondary absorption tank (4) is filled with water in advance to a preset liquid level, and esterification is completed when the interface of the secondary absorption tank (4) reaches a set height.
10. A transesterification method of PET to produce DOTP according to claim 9, wherein during the esterification process, glycol and octanol are azeotroped, condensed by the condenser (10), and floated up, pressed back to the esterification kettle by a potential difference, and circulated in a reciprocating manner.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010325128.0A CN111408330A (en) | 2020-04-23 | 2020-04-23 | Ester exchange equipment and method for producing DOTP (dioctyl phthalate) by PET (polyethylene terephthalate) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010325128.0A CN111408330A (en) | 2020-04-23 | 2020-04-23 | Ester exchange equipment and method for producing DOTP (dioctyl phthalate) by PET (polyethylene terephthalate) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111889059A (en) * | 2020-08-29 | 2020-11-06 | 浙江工业大学 | Reaction device and process for preparing DOTP |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB246526A (en) * | 1925-01-26 | 1927-04-26 | Us Ind Alcohol Co | Process of esterification |
| CN101260201A (en) * | 2008-04-16 | 2008-09-10 | 李勇 | Method for preparing plasticity agent containing quantitative dioctyl terephthalate |
| CN103044257A (en) * | 2012-12-29 | 2013-04-17 | 南京化工职业技术学院 | Alcoholysis method and device system for producing dioctyl terephthalate by polyester wastes |
| CN104528291A (en) * | 2014-12-27 | 2015-04-22 | 蚌埠玻璃工业设计研究院 | Rotary blanking valve |
| CN204589035U (en) * | 2014-10-16 | 2015-08-26 | 杭州宇田科技有限公司 | DOTP esterification compressive reaction system |
| CN106117053A (en) * | 2016-08-24 | 2016-11-16 | 成都米特瑞新材料科技有限公司 | A kind of plasticizer production esterification process units |
| CN207722769U (en) * | 2017-11-20 | 2018-08-14 | 佛山市顺德区汉马粘胶实业有限公司 | A kind of reaction kettle feeding device |
| CN209619241U (en) * | 2019-03-01 | 2019-11-12 | 山东同源环保新材料有限公司 | A kind of collection system of ethylene glycol |
| CN209985023U (en) * | 2019-04-04 | 2020-01-24 | 山东润林新材料科技有限公司 | Production DOTP is with filtering agitating unit |
-
2020
- 2020-04-23 CN CN202010325128.0A patent/CN111408330A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB246526A (en) * | 1925-01-26 | 1927-04-26 | Us Ind Alcohol Co | Process of esterification |
| CN101260201A (en) * | 2008-04-16 | 2008-09-10 | 李勇 | Method for preparing plasticity agent containing quantitative dioctyl terephthalate |
| CN103044257A (en) * | 2012-12-29 | 2013-04-17 | 南京化工职业技术学院 | Alcoholysis method and device system for producing dioctyl terephthalate by polyester wastes |
| CN204589035U (en) * | 2014-10-16 | 2015-08-26 | 杭州宇田科技有限公司 | DOTP esterification compressive reaction system |
| CN104528291A (en) * | 2014-12-27 | 2015-04-22 | 蚌埠玻璃工业设计研究院 | Rotary blanking valve |
| CN106117053A (en) * | 2016-08-24 | 2016-11-16 | 成都米特瑞新材料科技有限公司 | A kind of plasticizer production esterification process units |
| CN207722769U (en) * | 2017-11-20 | 2018-08-14 | 佛山市顺德区汉马粘胶实业有限公司 | A kind of reaction kettle feeding device |
| CN209619241U (en) * | 2019-03-01 | 2019-11-12 | 山东同源环保新材料有限公司 | A kind of collection system of ethylene glycol |
| CN209985023U (en) * | 2019-04-04 | 2020-01-24 | 山东润林新材料科技有限公司 | Production DOTP is with filtering agitating unit |
Non-Patent Citations (3)
| Title |
|---|
| 曾人泉: "《塑料加工助剂》", 30 September 1997, 中国物资出版社 * |
| 涂国材: "《中等专业学校轻工专业教材 食品工厂设备》", 30 April 1991, 中国轻工业出版社 * |
| 蒋恩臣: "《畜牧业机械化》", 31 December 2005, 中国农业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111889059A (en) * | 2020-08-29 | 2020-11-06 | 浙江工业大学 | Reaction device and process for preparing DOTP |
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