CN102010337B - Method and equipment for decoloring dioctyl terephthalate raw ester - Google Patents
Method and equipment for decoloring dioctyl terephthalate raw ester Download PDFInfo
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Abstract
The invention discloses a method and equipment for decoloring raw ester, which belongs to the technical field of dioctyl terephthalate raw ester (DOTP raw ester) decoloring. The method comprises the following steps that: the DOTP raw ester is subjected to a membrane separation process to form DOTP penetrant; and the DOTP penetrant is subjected to a resin adsorption process to be further decolored. The equipment comprises a membrane separation device and at least two stages of controllable temperature resin adsorption devices, wherein the membrane separation device comprises a hollow fibrous membrane assembly, and the penetrant outlet of the hollow fibrous membrane assembly is connected in series with each stage of the controllable temperature resin adsorption device sequentially; the last stage of the controllable temperature resin adsorption device is connected with a finished product storage tank through an ester discharge valve; and temperature of the controllable temperature resin adsorption devices is controlled by a circulating water bath device. The method is in accordance with the requirement of an environmentally-friendly process by adopting membrane separation technology and resin adsorption technology, is simple, and is convenient to popularize practically; and the equipment has the advantages of low energy consumption, large operation elasticity, small floor area and low cost, and can be easily industrially applied.
Description
Technical field
The invention belongs to the thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP, lower with) decolouring technology field, particularly a kind of decoloring dioctyl terephthalate raw ester method and apparatus.The present invention is specially a kind of method and apparatus that makes the thick ester decoloration of DOTP by membrane sepn and resin absorption integrated technology (MS-RA method), realizes high yield, less energy-consumption decolouring.
Background technology
Terephthalic acid di-isooctyl (DOTP) is the softening agent of a kind of excellent property of growing up the beginning of the seventies, and it has good electrical insulating property, winter hardiness, anti-extractable, flexibility, and volatility is little simultaneously, plasticizing efficiency is high.DOTP also is considered to a kind of non-toxic plasticizer, as primary plasticizer, can replace dioctyl phthalate (DOP) (DOP).Generally use DOTP abroad in 70 ℃ of level CABLE MATERIALS, and DOP can only reach the requirement of 65 ℃ of level CABLE MATERIALS, can not satisfy 70 ℃ of level cable standards of International Electrotechnical Commission (IEC) regulation, for in line with international standards, China's cable industry IEC277-1979 standard of carrying out in an all-round way, thereby will promote production and the application of the high temperature plasticizers such as DOTP.
The production method of DOTP mainly contains (1), direct esterification: the direct esterification under catalyzer exists of crude terephthalic acid (TPA) and octanol forms.(2), ester-interchange method: dimethyl terephthalate (DMT) (DMT) or polyethylene terephthalate waste material and octanol carry out transesterification reaction under catalyzer exists.(3), alcoholysis of acyl chloride method: p-phthaloyl chloride and octanol carry out alcoholysis reaction, because the method cost is high, and be subjected to the impact of starting material source and price, make the development of this technique be restricted be of little use (" plastics manufacturing " (Plastics Manufacture) 2008, the 4th volume: 106-108).And be chocolate by the thick ester of DOTP that method (1) (2) makes, and can not satisfy the industrial application requirement, must decolour.
The decoloring method of DOTP has [" Speciality Petrochemicals " (Speciality Petrochemicals), 1999,3 volumes, 1-4 pages] such as conventional physical-chemical absorption method, oxidative bleaching method, distillation under vacuum.Wherein absorption method and dioxygen water law decolouring, DeGrain is applicable to the decolouring of light DOTP; Chlorine method and potassium permanganate are sent out decolouring, and DOTP colourity is obviously improved, but will drop to below 4# (iodine colorimetry), and is very difficult; Chlorine and hydrochloric acid are all serious to equipment corrosion, and three wastes treatment capacity is large; Distillation method decolouring: effective, few without the processing of the burn into three wastes, it is more rational decoloring method, the superheated vapour underpressure distillation can reduce distillation temperature greatly, and product color is slightly excellent than distillation under vacuum, so the superheated vapour distillation under vacuum is more satisfactory decoloring method.But in distillation method, energy consumption is high, has side reaction to occur, and product yield is low.
For industrial decoloration process, the past is continued to use the operating procedure of underpressure distillation filtration, activated carbon decolorizing, plate-and-frame filter press press filtration always, and this decoloration process equipment is numerous and jumbled, labour intensity is large, energy consumption is high.Membrane sepn-adsorption technology is expected to overcome above-mentioned decoloration process shortcoming, and the film decolouring technology just is being obtained extensive attention abroad, is a kind of novel decoloration process of efficient, energy-saving and environmental protection.Membrane separation technique possesses that cold operation, equipment are comparatively simple, treatment capacity is large, easy to operate, easily is automated; Typical physical separating process, without chemical reagent and additive, the characteristics such as product is not contaminated.Yet membrane separation technique is to utilize the pore size of film that target compound is separated, and the purity of separated product is relatively low.The resin absorption technology is to utilize aglucon in resin and the interaction of the foreign pigment in DOTP (aldehyde radical, carboxylic compound etc.) to carry out separation and purification, when feed liquid flows through resin with certain flow rate, coordinating group specific binding in foreign pigment and resin medium surface or resin hole and being retained down, qualified product flows out, by elutriant, target molecule is eluted again after pending end, thereby reach the purpose of decolouring.
Summary of the invention
The invention provides the decoloring method of the thick ester of a kind of terephthalic acid di-isooctyl (the thick ester of DOTP), be membrane sepn and resin absorption integrated technology (MS-RA method), the method comprises membrane sepn operation and resin absorption operation, and described membrane sepn operation adopts hollow-fibre membrane.The method specifically comprises the following steps: the thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) enters the membrane sepn operation and tentatively decolours, obtain terephthalic acid di-isooctyl (DOTP) penetrating fluid through after membrane filtration, terephthalic acid di-isooctyl (DOTP) penetrating fluid enters the resin absorption operation and further decolours.
Function and the feature of each operation are as follows:
The membrane sepn operation: the film decolouring technology just is being obtained extensive attention abroad, is a kind of novel decoloration process of efficient, energy-saving and environmental protection.Membrane separation technique possesses that cold operation, equipment are comparatively simple, treatment capacity is large, easy to operate, easily is automated; Typical physical separating process, without chemical reagent and additive, the characteristics such as product is not contaminated are to utilize the pore size of film that target compound is separated, and isolate the impurity such as colloid in the thick ester of DOTP and macrobead.The hollow-fibre membrane that uses be any one in polyvinylidene difluoride (PVDF) (PVDF), polysulfones (PS), polyethersulfone (PES), polyethylene (PE), polypropylene (PP) or polyvinyl chloride (PVC) etc., preferred polyvinylidene difluoride (PVDF) (PVDF) hollow-fibre membrane.The hollow-fibre membrane that uses be that 0.02～0.5 μ m, molecular weight cut-off are any one film in 2～80,000 scopes as the membranous wall mean pore size.The membrane module pressure versus flow is respectively 0.05～0.15MPa and 0.4～0.8m/s.The thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) obtains terephthalic acid di-isooctyl (DOTP) penetrating fluid through after membrane filtration, and terephthalic acid di-isooctyl (DOTP) penetrating fluid enters down one resin absorption technique and further decolours.
The thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) heating process can also be set before in the membrane sepn operation, the viscosity of the rear thick ester system of DOTP of heating is reduced greatly, mobility strengthens greatly, be convenient to the conveying of pipeline and strengthen the speed of carrying out of coarse filtration technique, the Heating temperature of described heating process is 30 ℃～80 ℃, and the thick ester of the DOTP after heating directly enters the membrane sepn operation.Thereby making hollow-fibre membrane membrane module entrance material temperature is 30 ℃～80 ℃.
The resin absorption operation: the resin absorption technology is to utilize the physics and chemistry of aglucon in resin and the foreign pigment in DOTP (aldehyde radical, carboxylic compound etc.) to interact to carry out separation and purification, when feed liquid flows through resin with certain flow rate, coordinating group specific binding in foreign pigment and resin medium surface or resin hole and being retained down.Described resin absorption operation adopts macroporous adsorbent resin or ion exchange resin.Adopt following polymeric adsorbent in the resin absorption operation: H103T resin, ADS-22 resin, NKA-II resin or following ion exchange resin: any in 201*4 resin, D296R, D301T, D280, D072, D380, D261, NKC-9, D113 or any several mixed with resin decolouring.Making terephthalic acid di-isooctyl (DOTP) penetrating fluid during adsorption bleaching is that 30 ℃～50 ℃ and flow velocity are by being filled with the adsorption tower of polymeric adsorbent or ion exchange resin under the condition of 0.5～3BV/h in temperature.Temperature controllable resin absorption device is controlled the sorption and desorption temperature of resin at 30 ℃～50 ℃ by thermostatic circulation bath.
Described method can also contain hollow-fibre membrane backwash operation and resin regeneration operation.Function and the feature of each operation are as follows:
Hollow-fibre membrane backwash operation: for guaranteeing the efficient and life-time service of membrane separation unit, the present invention has designed back washing device for membrane separation unit, with in good time cleaning film assembly.Scavenging solution use toxicity little, to the good ethanol of DOTP impurity solvability, adopt the flow direction continuous wash 10～120min opposite with the thick ester of DOTP, the ethanol temperature is 30 ℃～45 ℃, pressure versus flow is respectively 0.05～0.15MPa and 0.4～0.8m/s.
Resin regeneration operation: according to the polymeric adsorbent that adopts and ion exchange resin, activate or regenerate according to production of resins producer's resin activation and renovation process, step.In order to guarantee the continuous, effective of operation, the present invention has designed resin regenerating device.
the thick ester of the DOTP that the inventive method is used can react the thick ester of DOTP that obtains by terephthalic acid tankage and isooctyl alcohol direct esterification, the colourity of the thick ester of DOTP is greater than 500# (platinum cobalt colorimetry), the colourity of the DOTP penetrating fluid that process membrane sepn operation obtains is 300～400# (platinum cobalt colorimetry), finished product colourity after in the resin absorption operation, one-level resin absorption device is processed is 150～260# (platinum cobalt colorimetry), if color is below standard, further process until the finished product colourity that obtains is up to state standards (HG/T2423-2008) with next stage resin absorption device.
The present invention also provides a cover decoloring equipment, and its technical process and desired result with locking is adapted.This equipment contains membrane separation unit and two-stage temperature controllable resin absorption device at least, described membrane separation unit contains hollow fiber film assembly, the penetrating fluid outlet of described hollow fiber film assembly is connected in series successively with every one-level temperature controllable resin absorption device, last step temperature controllable resin absorption device is connected with finished product storage tank through row's ester valve, and the temperature of described temperature controllable resin absorption device is controlled by the circulator bath device.Can detect after every one-level temperature controllable resin absorption device is processed, if arrive the colourity of national Specification, directly discharging to finished product storage tank, continues decolouring otherwise enter into next stage temperature controllable resin absorption device.
Described membrane separation unit comprises thick ester storage tank, the first defeated ester pump, tensimeter, the first defeated ester valve, described hollow fiber film assembly and the first check valve; Described thick ester storage tank, the first defeated ester pump, tensimeter, the first defeated ester valve and described hollow fiber film assembly are connected in series successively, and described hollow fiber film assembly is connected with described thick ester storage tank through the first check valve.
Described equipment also contains thick ester heating unit, and described thick ester heating unit is front well heater, and described front well heater is arranged between described thick ester storage tank and the described first defeated ester pump.
The penetrating fluid outlet of described hollow fiber film assembly is connected with first step temperature controllable resin absorption device through relay tank, post-heater, the second defeated ester pump, first flow meter and the check valve of being connected successively, all can be connected with under meter through defeated ester valve between every one-level temperature controllable resin absorption device.
Described equipment can comprise that also (washing lotion storage tank, lotion pumps and washing lotion valve consist of back washing device to the hollow-fibre membrane back washing device, back washing device is connected with hollow fiber film assembly) and resin regenerating device (washing lotion storage tank, lotion pumps and washing lotion valve consist of the resin regeneration back washing device, and the resin regeneration back washing device is connected with temperature controllable resin absorption device).
Beneficial effect of the present invention is: compare with the DOTP decolouring technology under traditional sense, the present invention holds back the colloid in the thick ester of DOTP and tentatively decolours by membrane separation technique, again penetrating fluid is further decoloured through resin absorption, the DOTP finished product that the product performance that obtain after two kinds of techniques are integrated reach or are near the mark, whole process has not related to a large amount of energy consumptions, and by the cleaning of hollow fiber film assembly and the reclaiming process of resin, whole decolouring integrated technique can recycle, thereby reaches the purpose that reduces energy consumption, reduces costs.
Method of the present invention is introduced membrane separation technique and resin absorption technology, walk the environment-friendly type technique route, and technique is simple, is convenient to actual popularization; This equipment energy consumption is low, and turndown ratio is large, and floor space is little, and cost is low, is easy to industrial applications.The finished product conformance with standard (HG/T2423-2008) of gained after the thick ester decoloration of DOTP.
Description of drawings
Fig. 1. be the decoloring method of the thick ester of DOTP of the present invention and technological principle and the device structure schematic diagram of equipment;
Fig. 2. be membrane flux time history plot when adopting polyvinylidene difluoride (PVDF) (PVDF) hollow-fibre membrane to process the thick ester of DOTP;
The thick ester storage tank of number in the figure: 1-; Well heater before 2-; The defeated ester pump of 3-first; The 4-tensimeter; The defeated ester valve of 5-first; The 6-hollow fiber film assembly; 7-the first check valve; The 8-relay tank; 9-washing lotion storage tank; The 10-lotion pumps; 11-washing lotion valve; The 12-post-heater; The defeated ester pump of 13-second, 14-first flow meter; 15-the second check valve; 16-first step temperature controllable resin absorption device; The defeated ester valve of 17-second; 18-the second under meter; 19-second stage temperature controllable resin absorption device; 20-row ester valve; The 21-finished product storage tank; 22-washing lotion storage tank; The 23-lotion pumps; 24-washing lotion valve, 25-washing lotion valve; The 26-lotion pumps; 27-washing lotion storage tank.
Embodiment
The invention will be further described below in conjunction with drawings and Examples, and the present invention never only limits to following examples:
Embodiment 1 decoloring equipment and technique
a kind of decoloring equipment, its structural representation as shown in Figure 1, this equipment contains membrane separation unit and two-stage temperature controllable resin absorption device: first step temperature controllable resin absorption device 16 and second stage temperature controllable resin absorption device 19, described membrane separation unit contains hollow fiber film assembly 6, the penetrating fluid outlet of described hollow fiber film assembly 6 is connected in series successively with every one-level temperature controllable resin absorption device, last step temperature controllable resin absorption device is connected with finished product storage tank 21 through row's ester valve 20, the temperature of described temperature controllable resin absorption device is controlled by circulator bath device 28, keep column temperature stable.
Described membrane separation unit comprises thick ester storage tank 1, the first defeated ester pump 3, tensimeter 4, the first defeated ester valve 5, hollow fiber film assembly 6 and the first check valve 7; Described thick ester storage tank 1, the first defeated ester pump 3, tensimeter 4, the first defeated ester valve 5 are connected in series successively with hollow fiber film assembly 6, and described hollow fiber film assembly 6 is connected with described thick ester storage tank 1 through the first check valve 7.Be that the recirculation after the first defeated ester pump 3 input hollow fiber film assemblies 6 are processed of thick ester is returned in thick ester storage tank 1, by changing the first defeated ester valve 5 and the first check valve 7 sizes, regulate seepage water pressure and the infiltration capacity of hollow fiber film assembly 6, tensimeter 4 is used to refer to the pipeline driving pressure.
Described equipment also can contain thick ester heating unit, described thick ester heating unit is front well heater 2, described front well heater 2 is arranged between described thick ester storage tank 1 and the described first defeated ester pump 3, be that described thick ester storage tank 1, front well heater 2, the first defeated ester pump 3, tensimeter 4, the first defeated ester valve 5 and hollow fiber film assembly 6 are connected in series successively, described hollow fiber film assembly 6 is connected with described thick ester storage tank 1 through the first check valve 7 again.
The outlet of the penetrating fluid of described hollow fiber film assembly 6 is connected with first step temperature controllable resin absorption device 16 through relay tank 8, post-heater 12, the second defeated ester pump 13, first flow meter 14 and the check valve 15 of being connected successively, between first step temperature controllable resin absorption device 16 and second stage temperature controllable resin absorption device 19 through the second defeated ester valve 17 be connected under meter 18 and be connected.
Described equipment also can comprise the hollow-fibre membrane back washing device, and (washing lotion storage tank, lotion pumps and washing lotion valve consist of back washing device, back washing device is connected with hollow fiber film assembly) and resin regenerating device (washing lotion storage tank, lotion pumps and washing lotion valve consist of the resin regeneration back washing device, and the resin regeneration back washing device is connected with temperature controllable resin absorption device).
The hollow-fibre membrane back washing device is a cover supplementary unit of rinsing membrane module 6, to guarantee the efficient and life-time service of membrane separation unit.Comprise washing lotion storage tank 9, lotion pumps 10 and the several parts of washing lotion valve 11, in washing lotion storage tank 9, washing lotion is connected with the washing lotion valve through lotion pumps 10 and is connected with hollow fiber film assembly 6, forms back washing device.For guaranteeing cleaning performance, can improve the alcohol immersion time and adopt pulsed to clean.
Resin regenerating device is the supplementary unit that resin is regenerated, and for easy to operate, has designed washing lotion storage tank 22,27, lotion pumps 23,26, washing lotion valve 24,25, be conducive to the resin regeneration process continuously, convenient, can operate.
A kind of decoloration process: comprise membrane sepn operation and resin absorption operation, described membrane sepn operation adopts hollow-fibre membrane; Specifically comprise the following steps: the thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) enters the membrane sepn operation and tentatively decolours, obtain terephthalic acid di-isooctyl (DOTP) penetrating fluid through after membrane filtration, terephthalic acid di-isooctyl (DOTP) penetrating fluid enters the resin absorption operation and further decolours.
The thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) heating process is set before described membrane sepn operation, makes hollow-fibre membrane membrane module entrance material temperature reach design temperature, can adopt the electric mantle heating, the thick ester of the DOTP after heating directly enters membrane separation process.
Temporarily be stored in relay tank 8 from membrane separation unit DOTP penetrating fluid out, be heated to as required the temperature of technique initialization with post-heater 12, then by the second defeated ester pump 13, the DOTP penetrating fluid is squeezed into first step temperature controllable resin absorption device 16 from the bottom of first step temperature controllable resin absorption device 16, controlled column temperature and flow velocity and decolour.DOTP from first step temperature controllable adsorption unit 16 tops out after, detect, if to the colourity of national Specification, directly discharging to finished product storage tank 21, continues to decolour otherwise enter into next stage temperature controllable resin absorption device.
The thick ester decoloration technique of embodiment 2.DOTP
The present embodiment decoloring equipment used contains front well heater 2, and has two-stage temperature controllable adsorption unit as described in Example 1.
The thick ester of the described DOTP of the embodiment of the present invention is the thick ester of DOTP (lower same) that is obtained by terephthalic acid tankage and isooctyl alcohol direct esterification reaction, and the colourity of the thick ester of DOTP is greater than 500# (platinum cobalt colorimetry).
the thick ester of DOTP is inputted after front well heater 2 is heated to 30 ℃ in hollow fiber film assembly 6, and it is resistant to elevated temperatures polyvinylidene difluoride (PVDF) (PVDF) the hollow fiber film assembly filtration of 0.02 μ m that hollow fiber film assembly adopts mean pore size, working pressure 0.15MPa, the permeate collection that hollow-fibre membrane obtains after the large particulate matter in thick ester is held back is in relay tank 8, ester product in relay tank 8 are again after post-heater 12 is heated to 50 ℃, pumped in the first step temperature controllable resin absorption device 16 and second stage temperature controllable resin absorption device 19 of series connection through the second check valve 15 by the second defeated ester pump 13, in temperature controllable resin absorption device 16 and 19 the resin that uses all be H103T, thermostatic circulation bath 28 is used for controlling the temperature of temperature controllable resin absorption device 16 and 19 at 40 ℃, it is 0.5BV/h that the second defeated ester pump 13 is controlled the DOTP flow velocity, DOTP finished product after the two-stage resin adsorption bleaching is collected in finished product storage tank 21, this finished product conformance with standard (HG/T2423-2008).
The thick ester decoloration technique of embodiment 3.DOTP
Decoloration process and equipment are with embodiment 1, but processing condition are: thick ester temperature is heated under 50 ℃, working pressure 0.08MPa, adopt polysulfones (PS) hollow-fibre membrane, this membranous wall mean pore size 0.5 μ m, the thick ester of DOTP is carried out membrane sepn purify, can get as clear as crystal brown decolouring DOTP penetrating fluid.In first step temperature controllable resin absorption device 16 and second stage temperature controllable resin absorption device 19 the resin that uses all be D280, thermostatic circulation bath 28 is used for controlling the temperature of temperature controllable resin absorption device 16 and 19 at 30 ℃, it is 1BV/h that the second defeated ester pump 13 is controlled DOTP flow velocity in adsorption unit, DOTP finished product after the two-stage resin adsorption bleaching is collected in finished product storage tank 21, this finished product conformance with standard (HG/T2423-2008)
The thick ester decoloration technique of embodiment 4.DOTP
Decoloration process and equipment are with embodiment 1, but processing condition are: thick ester pretreatment temperature is 80 ℃, adopt polyvinylidene difluoride (PVDF) (PVDF) membrane module, tubular fibre membranous wall mean pore size is 0.1 μ m, working pressure 0.08MPa, in first step temperature controllable resin absorption device 16, potting resin is by being used resin to be D280 in D301T and second stage temperature controllable resin absorption device 19, the temperature that thermostatic circulation bath 28 is used for controlling temperature controllable resin absorption device 16 and 19 is at 35 ℃, and the second defeated ester pump 13 is controlled the flow velocity 2BV/h of DOTP in adsorption unit.DOTP finished product after the two-stage resin adsorption bleaching is collected in finished product storage tank 21, this finished product conformance with standard (HG/T2423-2008).
The thick ester decoloration equipment of embodiment 5.DOTP and technique
The present embodiment equipment increases third stage temperature controllable resin absorption device on the basis of embodiment 1 equipment used, and second stage temperature controllable resin absorption device is connected with third stage temperature controllable resin absorption device with under meter through defeated ester valve, and third stage temperature controllable resin absorption device is connected with finished product storage tank through row's ester valve.
The decoloring method of the present embodiment:
the thick ester of DOTP is inputted after front well heater 2 is heated to 60 ℃ in hollow fiber film assembly 6, and it is resistant to elevated temperatures polyvinylidene difluoride (PVDF) (PVDF) the hollow fiber film assembly filtration of 0.06 μ m that hollow fiber film assembly adopts mean pore size, working pressure 0.1MPa, the permeate collection that hollow-fibre membrane obtains after the large particulate matter in thick ester is held back is in relay tank 8, ester product in relay tank 8 are again after post-heater 12 is heated to 40 ℃, pumped into the first step temperature controllable resin absorption device 16 of series connection through the second check valve 15 by the second defeated ester pump 13, in second stage temperature controllable resin absorption device 19 and third stage temperature controllable resin absorption device, the first step, in the second stage and third stage temperature controllable resin absorption device, the resin that uses is respectively D072, D113, D296R, thermostatic circulation bath 28 is used for controlling the first step, the temperature of the second stage and third stage temperature controllable resin absorption device is at 40 ℃, it is 3BV/h that the second defeated ester pump 13 is controlled the DOTP flow velocity, DOTP finished product after three grade resins adsorption bleachings is collected in finished product storage tank 21, this finished product conformance with standard (HG/T2423-2008).
It is finished product (distillation method DOTP) performance comparison after finished product (MS-RA method DOTP) and the distillation method decolouring after embodiment 2, embodiment 3, embodiment 4, embodiment 5 decolourings in table 1.
The DOTP product performance contrast of table 1 different methods preparation
Embodiment 6. hollow-fibre membrane backwash operations and resin regeneration operation
Adopt toxicity little, be scavenging solution to the good ethanol of DOTP impurity solvability, adopt the flow direction continuous wash 30min opposite with the thick ester of DOTP, the ethanol temperature is 45 ℃, and pressure versus flow is respectively 0.1MPa and 0.8m/s, more than can making membrane module flux recovery to 95%, reach cleaning performance.
Resin regeneration operation: according to the polymeric adsorbent that adopts and ion exchange resin, activate or regenerate according to production of resins producer's resin activation and renovation process, step.
Claims (5)
1. the decoloring method of the thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP), is characterized in that, the method comprises membrane sepn operation and resin absorption operation, and described membrane sepn operation adopts hollow-fibre membrane; Specifically comprise the following steps: the thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) enters the membrane sepn operation and tentatively decolours, and enters the resin absorption operation through terephthalic acid di-isooctyl (DOTP) penetrating fluid that obtains after membrane filtration and further decolours.
2. the decoloring method of the thick ester of terephthalic acid di-isooctyl according to claim 1 (the thick ester of DOTP), it is characterized in that, the thick ester of terephthalic acid di-isooctyl (the thick ester of DOTP) heating process is set before described membrane sepn operation, and making hollow-fibre membrane membrane module entrance material temperature is 30 ℃～80 ℃.
3. the decoloring method of the thick ester of terephthalic acid di-isooctyl according to claim 1 (the thick ester of DOTP), it is characterized in that, described hollow-fibre membrane is that the membranous wall mean pore size is that 0.02～0.5 μ m, molecular weight cut-off are any one film in 2～80,000 scopes, and its material is any one in polyvinylidene difluoride (PVDF) (PVDF), polysulfones (PS), polyethersulfone (PES), polyethylene (PE), polypropylene (PP) or polyvinyl chloride (PVC);
Adopt following polymeric adsorbent in the resin absorption operation: H103T resin, ADS-22 resin, NKA-II resin or following ion exchange resin: any in 201*4 resin, D296R, D301T, D280, D072, D380, D261, NKC-9, D113 or any several mixed with resin decolouring.
4. the decoloring method of the thick ester of terephthalic acid di-isooctyl according to claim 1 (the thick ester of DOTP), is characterized in that, in the membrane sepn operation, the membrane module pressure versus flow is respectively 0.05～0.15MPa and 0.4～0.8m/s; Making terephthalic acid di-isooctyl (DOTP) penetrating fluid in the resin absorption operation during adsorption bleaching is that 30 ℃～50 ℃ and flow velocity are by being filled with the adsorption tower of resin under the condition of 0.5～3BV/h in temperature.
5. the decoloring method of the thick ester of terephthalic acid di-isooctyl according to claim 1 (the thick ester of DOTP), is characterized in that, described method also contains hollow-fibre membrane backwash operation and resin regeneration operation.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1563159A (en) * | 2004-03-18 | 2005-01-12 | 杨家勇 | Technique for preparing plasticizer of dioctyl terephthalate from terephthalic acid and capryl alcohol |
| CN1789228A (en) * | 2004-12-13 | 2006-06-21 | 上海市农药研究所 | Method for purifying hydroxy acetic acid produced by biological catalysis |
| CN101081810A (en) * | 2006-05-30 | 2007-12-05 | 上海市农药研究所 | Purification method of propenoic acid produced by biology catalysis |
| CN101245009A (en) * | 2008-03-14 | 2008-08-20 | 李勇 | Production method for p-benzene dioctyl dicarboxylic acid elasticizer |
| CN101659457A (en) * | 2009-09-15 | 2010-03-03 | 南京大学 | Recovering and treating method for treating biochemical tail water resin desorption liquid |
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