CN102952019A - Dioctyl phthalate production line and DOTP production method - Google Patents
Dioctyl phthalate production line and DOTP production method Download PDFInfo
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- CN102952019A CN102952019A CN2011102366521A CN201110236652A CN102952019A CN 102952019 A CN102952019 A CN 102952019A CN 2011102366521 A CN2011102366521 A CN 2011102366521A CN 201110236652 A CN201110236652 A CN 201110236652A CN 102952019 A CN102952019 A CN 102952019A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 38
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 title claims abstract description 18
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 title claims abstract description 18
- BJAJDJDODCWPNS-UHFFFAOYSA-N dotp Chemical compound O=C1N2CCOC2=NC2=C1SC=C2 BJAJDJDODCWPNS-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000005886 esterification reaction Methods 0.000 claims abstract description 77
- 230000032050 esterification Effects 0.000 claims abstract description 75
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 52
- 238000005406 washing Methods 0.000 claims abstract description 34
- 238000001914 filtration Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000010865 sewage Substances 0.000 claims abstract description 23
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 121
- 150000002148 esters Chemical class 0.000 claims description 116
- 239000007788 liquid Substances 0.000 claims description 59
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 238000011068 loading method Methods 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 15
- -1 alcohol ester Chemical class 0.000 claims description 13
- 238000012856 packing Methods 0.000 claims description 13
- 239000002351 wastewater Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005273 aeration Methods 0.000 claims description 7
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 6
- 238000005188 flotation Methods 0.000 claims description 6
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 239000003507 refrigerant Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 10
- OEIWPNWSDYFMIL-UHFFFAOYSA-N dioctyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C=C1 OEIWPNWSDYFMIL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- LERGDXJITDVDBZ-UHFFFAOYSA-N dioctyl benzene-1,3-dicarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=CC(C(=O)OCCCCCCCC)=C1 LERGDXJITDVDBZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 abstract 1
- 238000005457 optimization Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a dioctyl phthalate production line and a DOTP production method. Existing DOTP production methods have the defects of long esterification reaction time, large catalyst dosage, high octanol content in product, and slightly yellow color. The invention provides a dioctyl phthalate production line comprising an esterification system, a dealcoholization system, a neutralization/washing system, a stripping system, a filtering and decolorizing system, and a sewage purification and recovery system. All the systems are modified. The invention also relates to a DOTP production method, comprising a plurality of steps such as esterification, dealcoholization, neutralization/washing, stripping, filtering and decolorizing, sewage purification and recovery, and the like. All the steps are different from those of prior arts. When DOTP is produced with the method provided by the invention, the esterification reaction can be achieved in 4-5 hours; a catalyst dosage is low; the product is clean and colorless; alcohol content in finished product can be reduced to 20ppm; and quality is greatly improved. The production line and the method can be used for producing dioctyl terephthalate, dioctyl orthophthalate, and dioctyl isophthalate.
Description
Technical field
The method that the present invention relates to a kind of dioctyl phthalate production line and produce DOTP.
Background technology
Existing DOTP (dioctyl terephthalate) production line and production method reaction time of esterification are long, and catalyst levels is large, and octanol content is high in the product, the little Huang of color and luster.
Summary of the invention
The technical problem to be solved in the present invention is the defects that how to overcome prior art, the method that a kind of dioctyl phthalate production line is provided and produces DOTP.
For solving the problems of the technologies described above, dioctyl phthalate production line of the present invention comprises esterification system, dealcoholysis system, neutralization/water wash system, stripping system, filtration decolouring system and sewage water cleaning recovery system, it is characterized in that:
(1) esterification system comprises pure charging stock tank, reaction kettle of the esterification, packing tower, esterification system condenser and esterification system drainer, wherein be provided with feed-pipe bottom the pure charging stock tank, this feed-pipe is provided with valve, and passes into reaction kettle of the esterification, and the reaction kettle of the esterification bottom is provided with the discharge nozzle with valve; The reaction kettle of the esterification top is provided with escape pipe and with the loading hopper of valve, escape pipe emptying behind packing tower, esterification system condenser shell side, esterification system condenser tube side is walked recirculated water, the phlegma of esterification system condenser enters the esterification system drainer, esterification system drainer top also is provided with upflow tube, this upflow tube is back to reaction kettle of the esterification behind packing tower, esterification system drainer bottom discharge pipe leads to the wastewater collection tank of sewage recycling system.
(2) dealcoholysis system comprises the thick ester tank of dealcoholysis system, flashing tower, recycle alcohol condenser, water ring vacuum pump, thick ester surge tank and recycle alcohol tank, the entrance of the thick ester tank of dealcoholysis system connects the discharge nozzle of reaction kettle of the esterification bottom, the thick ester pot bottom discharging of dealcoholysis system is through the alcohol ester interchanger, enter and flashing tower, and in alcohol ester interchanger and the extremely octanol heat exchange of pure charging stock tank of recycle alcohol tank, the emptying behind the shell side of recycle alcohol condenser, water ring vacuum pump of flashing tower top escape pipe, the laggard recycle alcohol tank of the phlegma liquid seal can of recycle alcohol condenser; After flashing tower materials at bottom of tower liquid seal can advances thick ester surge tank, advance the neutralization/water washing tank of neutralization/water wash system through the thick ester pump of dealcoholysis system, the thick ester interchanger of dealcoholysis system.
(3) neutralization/water wash system comprises neutralization/water washing tank and the thick ester interchanger of neutralization/water wash system, wherein neutralization/water washing tank top is provided with loading hopper and the escape pipe with valve, the discharge nozzle of neutralization/water washing tank bottom send and filters the thick ester tank of decolouring system behind the thick ester pump of neutralization/water wash system, the thick ester interchanger of neutralization/water wash system.
(4) stripping system comprises the stripping system condenser, alcohol water separation tank and water ring vacuum pump, the escape pipe of neutralization/water washing tank communicates with stripping system condenser shell side inlet mouth, stripping system condenser shell side air outlet joins by pipeline and water ring vacuum pump suction opening, stripping system condenser bottom drain pipe passes into described pure water separation tank, refrigerant in the stripping system condenser is walked tube side, it is characterized in that: be provided with main road and bypass between described stripping system condenser and the water ring vacuum pump, be respectively equipped with switch valve in main road and the bypass, and also be provided with a secondary condenser and a Roots vaccum pump in the bypass, secondary condenser bottom drain pipe passes into described pure water separation tank.
(5) filter the decolouring system and comprise the thick ester tank of filtration decolouring system, coarse filter and fine filter, wherein filter decolouring system thick ester tank top and be provided with charging opening, filtering the thick ester pot bottom discharging of decolouring system decolours after the thick ester pump of system boosts after filtration, one the tunnel enters coarse filter from the bottom, then overflow back from coarse filter top and filter the thick ester tank of decolouring system, another road is after the bottom enters fine filter, then behind smart ester interchanger, send the finished product tank field, then divide to be filled to light transmission container, send uviolizing decolouring district.
(6) sewage water cleaning recovery system comprises that wastewater collection tank, air flotation slot, oil removal are except slag bath, aeration tank, neutralization precipitation pond, quartz filter and charcoal filter, aforesaid device is connected in turn, and the discharge nozzle of esterification system drainer and neutralization/water washing tank all communicates with the wastewater collection tank.
As optimization, loading hopper top, the bottom of reaction kettle of the esterification top band valve are equipped with valve, and are provided with a nitrogen pipeline, and nitrogen pipeline is provided with nitrogen pressurization valve.So design is convenient to add several times catalyzer.
The method that the aforesaid esterification production line of the present invention is produced DOTP comprises the steps:
(1) utilize esterification system to carry out esterification, get thick ester still liquid, it is characterized in that, the weight ratio that feeds intake of terephthalic acid and n-Octanol is 1: 2, use titanium ester four isopropyl esters to be catalyzer, the weight ratio of catalyzer and raw material summation is 11000: 9, and titanium ester four isopropyl esters are divided into 9 weight parts, add 5 weight parts during in still temperature rise to 70～85 ℃, add 3 weight parts during in still temperature rise to 90～100 ℃, add 1 weight part during in still temperature rise to 110～120 ℃, the 2nd, when adding catalyzer 3 times, open first the loading hopper upper valve, behind the adding catalyzer, close again the loading hopper upper valve, open nitrogen pressurization valve, then open loading hopper bottom valve, with nitrogen catalyzer is pressed into reaction kettle of the esterification, close at last loading hopper bottom valve and nitrogen pressurization valve.
(2) utilize the dealcoholysis system that the thick ester still of step (1) gained liquid is carried out thick dealcoholysis, it is characterized in that; The thick ester liquid of the thick ester pot bottom of dealcoholysis system and flashing tower and recycle alcohol tank are to pure liquid heat exchange in a plate-type heat exchanger of pure charging stock tank.
(3) utilize neutralization/water wash system that thick ester liquid is neutralized, washes, it is characterized in that:
Drop into weight content and be 5% buck and neutralize 1., first, stir half an hour after, left standstill 10 minutes, after the layering water in the thick ester liquid is emitted, for subsequent use as a washing water, wherein the volume feed ratio of thick ester liquid and buck is: 1000: 1.
2., in thick ester liquid, add entry, stir washing after 20 minutes, left standstill 10 minutes, after the layering water in the thick ester liquid is emitted, for subsequent use as the intermediate water wash water.
3., in thick ester liquid, add without dried up, thick ester liquid and be without dried up volume feed ratio: 1000: 1, stir washing after 20 minutes, left standstill 10 minutes, the water that layering is emitted in the thick ester liquid is done sewage disposal, remaining thick ester liquid send the filtration decolouring system of filtering the decolouring system thick ester tank after the heat exchange of the thick ester interchanger of neutralization/water wash system.
(4) utilize stripping system that thick ester liquid is carried out smart dealcoholysis, it is characterized in that: during dealcoholysis, open first main road, start water ring vacuum pump and vacuumize, the thick ester pot liquid of stripping system is carried out the low pressure flash vaporization, when vacuum tightness reaches 0.09 MPa (10-15 minute consuming time approximately), open bypass, start Roots vaccum pump, then close main road, finish the switching of main road and bypass, Roots vaccum pump and water ring vacuum pump are worked simultaneously and are vacuumized.
(5) utilize filtration decolouring system that thick ester liquid is filtered, decolours, it is characterized in that: during filtration, use first coarse filter, circulating filtration, after the filtrate cleaning to be seen, switch to fine filter filter, after smart ester interchanger cooling, send the finished product tank field, then packing penetrates light transmission container, send uviolizing decolouring district, carries out uviolizing decolouring 24 hours.
Prior art needs 10 hours usually, just can finish esterification, the little Huang of products obtained therefrom color and luster, and catalyst levels is large.Use production line of the present invention, according to the method for the invention, when producing DOTP, only needed 4-5 hour can finish esterification, catalyst levels is little, and the product cleaning is colourless, and pure content can be down to 20ppm in the finished product, and quality improves greatly.
As optimization, it comprises that also utilizing sewage water cleaning recovery system to purify reclaims sewage, is characterized in that: before the oil removal slagging-off, carry out air supporting slagging-off, aeration oxide treatment through air flotation slot first.So design when sewage still keeps comparatively high temps, is carried out air supporting slagging-off, aeration oxidation, can be as much as possible with the harmful chemical oxidation removal.
As optimization, (3) step the is 1. in the link: select washing water preparation buck in the production cycle; (3) step the is 2. in the link: select in the production cycle intermediate water wash water to wash.So design helps to shorten neutralization/washing operating time.
When utilizing the present invention to produce DOTP, can finish esterification in 4-5 hour, catalyst levels is little, and the product cleaning is colourless, and pure content can be down to 20ppm in the finished product, and quality improves greatly.Dioctyl phthalate production line of the present invention can be used for producing dioctyl terephthalate, dioctyl phthalate (DOP) and dioctyl isophthalate.
Description of drawings
Be described further below in conjunction with the method for accompanying drawing to dioctyl phthalate production line of the present invention and production DOTP:
Fig. 1 is the device structure synoptic diagram of this dioctyl phthalate production line.
Fig. 2 utilizes aforementioned dioctyl phthalate production line to produce the general flow chart of the method for DOTP.
Among Fig. 1: B101 is the recycle alcohol tank, B102 is pure charging stock tank, B103 is the esterification system drainer, B105 is the thick ester tank of dealcoholysis system, B107A is liquid seal can, B107B is thick ester surge tank, B108 is the phlegma liquid seal can, VB106A, VB106B is the waste collection tank, B108, B110 is respectively into water, advance the alkali device, B114 is pure water separation tank, B112A, B112B is waste water tank, B116 is the raw alcohol tank, B115A, B115B, B117A, B117B is finished pot, G102 is fine filter, G104 is coarse filter, K101 is packing tower, K102 is flashing tower, T101 is the wastewater collection tank, W101A, W101B is the esterification system condenser, W102A, W102B is the recycle alcohol condenser, W103 is the alcohol ester interchanger, W104 is the thick ester interchanger of dealcoholysis system, W105A is the stripping system condenser, W105B is secondary condenser, W106A, W106B is Water-ring vacuum pump seal water-to-water heat exchanger, and W107 is the thick ester interchanger of neutralization/water wash system, W108 is smart ester interchanger, P101A, B is the recycle alcohol pump, P102A, B is the thick ester pump of neutralization/water wash system, P103 is for filtering the thick ester pump of decolouring system, P106A, B, C is water ring vacuum pump, P107 is the thick ester pump of dealcoholysis system, P110 is Roots vaccum pump, P115A, B, P117A, B is discharge pump, P116 is the raw alcohol pump.
Among Fig. 2: 1 for utilizing esterification system esterification, 2 for utilizing the thick dealcoholysis of dealcoholysis system, 3 for utilizing neutralization/water wash system neutralization/washing, 4 to filter decolouring, 6 for utilizing sewage water cleaning recovery system purification recovery sewage for utilizing stripping system to carry out smart dealcoholysis, 5 for filtering the decolouring system.
Embodiment
Embodiment one: as shown in Figure 1, this dioctyl phthalate production line comprises esterification system, dealcoholysis system, neutralization/water wash system, stripping system, filtration decolouring system and sewage water cleaning recovery system, it is characterized in that:
(1) esterification system comprises pure charging stock tank B102, reaction kettle of the esterification R101, packing tower K101, esterification system condenser W101A, W101B and esterification system drainer B103, wherein be provided with feed-pipe bottom the pure charging stock tank B102, this feed-pipe is provided with valve, and passing into reaction kettle of the esterification R101, reaction kettle of the esterification R101 bottom is provided with the discharge nozzle with valve; Reaction kettle of the esterification R101 top is provided with escape pipe and with the loading hopper of valve, escape pipe emptying behind packing tower K101, esterification system condenser W101A, W101B shell side, esterification system condenser W101A, W101B tube side are walked recirculated water, the phlegma of esterification system condenser W101A, W101B enters esterification system drainer B103, esterification system drainer B103 top also is provided with upflow tube, this upflow tube is behind packing tower, be back to reaction kettle of the esterification R101, esterification system drainer B103 bottom discharge pipe leads to the wastewater collection tank T101 of sewage recycling system.
(2) dealcoholysis system comprises the thick ester tank B105 of dealcoholysis system, flashing tower K102, recycle alcohol condenser W102A, W102B, water ring vacuum pump P106A, B, C, thick ester surge tank B107B and recycle alcohol tank B101, the entrance of the thick ester tank B105 of dealcoholysis system connects the discharge nozzle of reaction kettle of the esterification R101 bottom, dealcoholysis system thick ester tank B105 bottom discharge is through alcohol ester interchanger W103, enter and flashing tower K102, and in alcohol ester interchanger W103 and the extremely octanol heat exchange of pure charging stock tank B102 of recycle alcohol tank B101, flashing tower K102 top escape pipe is through recycle alcohol condenser W102A, the shell side of W102B, water ring vacuum pump P106A, B, emptying behind the C, recycle alcohol condenser W102A, the laggard recycle alcohol tank of the phlegma liquid seal can B108 B101 of W102B; Flashing tower K102 materials at bottom of tower advances the neutralization of neutralization/water wash system/water washing tank R102 through the thick ester pump P107 of dealcoholysis system, the thick ester interchanger W104 of dealcoholysis system after liquid seal can B107A advances thick ester surge tank B107B.
(3) neutralization/water wash system comprises neutralization/water washing tank R102 and the thick ester interchanger of neutralization/water wash system W107, wherein neutralization/water washing tank R102 top is provided with loading hopper and the escape pipe with valve, the discharge nozzle of neutralization/water washing tank R102 bottom send and filters the thick ester tank R103 of decolouring system behind neutralization/water wash system thick ester pump P102A or P102B, the thick ester interchanger of neutralization/water wash system W107.
(4) stripping system comprises stripping system condenser W105A, alcohol water separation tank B114 and water ring vacuum pump P106A, B, C, the escape pipe of neutralization/water washing tank R102 communicates with stripping system condenser W105A shell side inlet mouth, stripping system condenser W105A shell side air outlet is by pipeline and water ring vacuum pump P106A, B, the C suction opening joins, stripping system condenser W105A bottom drain pipe passes into described pure water separation tank B114, refrigerant among the stripping system condenser W105A is walked tube side, it is characterized in that: described stripping system condenser W105A and water ring vacuum pump P106A, B, be provided with main road and bypass between the C, be respectively equipped with switch valve in main road and the bypass, and also be provided with a secondary condenser W105B and a Roots vaccum pump P110 in the bypass, secondary condenser W105B, the bottom drain pipe passes into described pure water separation tank B114.
(5) filter the decolouring system and comprise the filtration thick ester tank R103 of decolouring system, coarse filter G104 and fine filter G102, wherein filter decolouring system thick ester tank R103 top and be provided with charging opening, filtering the thick ester tank R103 of decolouring system bottom discharge decolours after the thick ester pump P103 of system boosts after filtration, one the tunnel enters coarse filter G102 from the bottom, then overflow back from coarse filter G102 top and filter the thick ester tank R103 of decolouring system, another road is after the bottom enters fine filter G104, then behind smart ester interchanger G104, send finished pot B115A, the B115B district, then divide to be filled to light transmission container, send uviolizing decolouring district (Fig. 1 is not shown).
(6) sewage water cleaning recovery system comprises that wastewater collection tank T101, air flotation slot, oil removal are except slag bath, aeration tank, neutralization precipitation pond, quartz filter and charcoal filter, aforesaid device is connected in turn, and the discharge nozzle of esterification system drainer B103 and neutralization/water washing tank R103 all communicates with wastewater collection tank T101.
Loading hopper top, the bottom of reaction kettle of the esterification R101 top band valve are equipped with valve, and are provided with a nitrogen pipeline, and nitrogen pipeline is provided with nitrogen pressurization valve.
Waste liquid among VB106A, the VB106B is after W106A, W106B heat exchange, and the sealing water that can be used as water ring vacuum pump P106A, B, C uses.
As shown in Figure 2, the present invention utilizes the method for the production DOTP of aforementioned dioctyl phthalate production line, comprise the steps: that (1) utilizes esterification system to carry out esterification, get thick ester still liquid, it is characterized in that, the weight ratio that feeds intake of terephthalic acid and n-Octanol is 1: 2, use titanium ester four isopropyl esters to be catalyzer, the weight ratio of catalyzer and raw material summation is 11000: 9, and titanium ester four isopropyl esters are divided into 9 weight parts, add 5 weight parts during in still temperature rise to 70～85 ℃, add 3 weight parts during in still temperature rise to 90～100 ℃, add 1 weight part during in still temperature rise to 110～120 ℃, the 2nd, when adding catalyzer 3 times, open first the loading hopper upper valve, behind the adding catalyzer, close again the loading hopper upper valve, open nitrogen pressurization valve, then open loading hopper bottom valve, with nitrogen catalyzer is pressed into reaction kettle of the esterification, close at last loading hopper bottom valve and nitrogen pressurization valve;
When 2nd, adding catalyzer 3 times, open first the catalyst charging hole upper valve, after adding catalyzer, close again the catalyst charging hole upper valve, open nitrogen pressurization valve, then open catalyst charging hole bottom valve, with nitrogen catalyzer is pressed into reaction kettle of the esterification, close at last catalyst charging hole bottom valve and nitrogen pressurization valve.
(2) utilize the dealcoholysis system that the thick ester still of step (1) gained liquid is carried out thick dealcoholysis, it is characterized in that; The thick ester tank B105 of dealcoholysis system is to thick ester liquid and the extremely pure liquid heat exchange in a plate-type heat exchanger W103 of pure charging stock tank B103 of recycle alcohol tank of flashing tower K102.
(3) utilize neutralization/water wash system that thick ester liquid is neutralized, washes,
Drop into weight content and be 5% buck and neutralize 1., first, stir half an hour after, left standstill 10 minutes, after the layering water in the thick ester liquid is emitted, for subsequent use as a washing water, wherein the volume feed ratio of thick ester liquid and buck is: 1000: 1; Except first production, select washing water preparation buck in the production cycle.(get thick ester liquid acid number for being generally 0.6 by this technique gained, as in producing as thick ester liquid acid number change, scale up or reduce the buck consumption)
2., in thick ester liquid, add entry, stir washing after 20 minutes, left standstill 10 minutes, after the layering water in the thick ester liquid is emitted, for subsequent use as the intermediate water wash water, except first production, select in the production cycle intermediate water wash water to wash.
3., in thick ester liquid, add without dried up, thick ester liquid and be without dried up volume feed ratio: 1000: 1, stir washing after 20 minutes, left standstill 10 minutes, the water that layering is emitted in the thick ester liquid is done sewage disposal, remaining thick ester liquid send the filtration decolouring system of filtering the decolouring system thick ester tank after the thick ester interchanger of neutralization/water wash system W107 heat exchange.
(4) utilize stripping system that thick ester liquid is carried out smart dealcoholysis, it is characterized in that: during dealcoholysis, open first main road, starting water ring vacuum pump P106 (A, B or C) vacuumizes, liquid in the flashing tower K102 is carried out the low pressure flash vaporization, when vacuum tightness reaches 0.09 MPa (10-15 minute consuming time approximately), open bypass, start Roots vaccum pump P110, then close main road, finish the switching of main road and bypass, Roots vaccum pump P110 and water ring vacuum pump P106 (A, B or C) work simultaneously and vacuumize.
(5) utilize filtration decolouring system that thick ester liquid is filtered, decolours, it is characterized in that: during filtration, use first coarse filter G104 circulating filtration, after the filtrate cleaning to be seen, switch to fine filter G102 filter, after smart ester interchanger W108 cooling, send finished pot B115A, B district, then packing penetrates light transmission container, send uviolizing decolouring district, carry out uviolizing decolouring 24 hours.
(6) utilize sewage water cleaning recovery system to purify and reclaim sewage, it is characterized in that: before the oil removal slagging-off, carry out air supporting slagging-off, aeration oxide treatment through air flotation slot first.
Claims (5)
1. a dioctyl phthalate production line comprises esterification system, dealcoholysis system, neutralization/water wash system, stripping system, filtration decolouring system and sewage water cleaning recovery system, it is characterized in that:
(1) esterification system comprises pure charging stock tank, reaction kettle of the esterification, packing tower, esterification system condenser and esterification system drainer, wherein be provided with feed-pipe bottom the pure charging stock tank, this feed-pipe is provided with valve, and passes into reaction kettle of the esterification, and the reaction kettle of the esterification bottom is provided with the discharge nozzle with valve; The reaction kettle of the esterification top is provided with escape pipe and with the loading hopper of valve, escape pipe emptying behind packing tower, esterification system condenser shell side, esterification system condenser tube side is walked recirculated water, the phlegma of esterification system condenser enters the esterification system drainer, esterification system drainer top also is provided with upflow tube, this upflow tube is back to reaction kettle of the esterification behind packing tower, esterification system drainer bottom discharge pipe leads to the wastewater collection tank of sewage recycling system;
(2) dealcoholysis system comprises the thick ester tank of dealcoholysis system, flashing tower, recycle alcohol condenser, water ring vacuum pump, thick ester surge tank and recycle alcohol tank, the entrance of the thick ester tank of dealcoholysis system connects the discharge nozzle of reaction kettle of the esterification bottom, the thick ester pot bottom discharging of dealcoholysis system is through the alcohol ester interchanger, enter and flashing tower, and in alcohol ester interchanger and the extremely octanol heat exchange of pure charging stock tank of recycle alcohol tank, the emptying behind the shell side of recycle alcohol condenser, water ring vacuum pump of flashing tower top escape pipe, the laggard recycle alcohol tank of the phlegma liquid seal can of recycle alcohol condenser; The flashing tower materials at bottom of tower advances the neutralization/water washing tank of neutralization/water wash system through the thick ester pump of dealcoholysis system, the thick ester interchanger of dealcoholysis system after liquid seal can advances thick ester surge tank;
(3) neutralization/water wash system comprises neutralization/water washing tank and the thick ester interchanger of neutralization/water wash system, wherein neutralization/water washing tank top is provided with loading hopper and the escape pipe with valve, the discharge nozzle of neutralization/water washing tank bottom send and filters the thick ester tank of decolouring system behind the thick ester pump of neutralization/water wash system, the thick ester interchanger of neutralization/water wash system;
(4) stripping system comprises the stripping system condenser, alcohol water separation tank and water ring vacuum pump, the escape pipe of neutralization/water washing tank communicates with stripping system condenser shell side inlet mouth, stripping system condenser shell side air outlet joins by pipeline and water ring vacuum pump suction opening, stripping system condenser bottom drain pipe passes into described pure water separation tank, refrigerant in the stripping system condenser is walked tube side, it is characterized in that: be provided with main road and bypass between described stripping system condenser and the water ring vacuum pump, be respectively equipped with switch valve in main road and the bypass, and also be provided with a secondary condenser and a Roots vaccum pump in the bypass, secondary condenser bottom drain pipe passes into described pure water separation tank;
(5) filter the decolouring system and comprise the thick ester tank of filtration decolouring system, coarse filter and fine filter, wherein filter decolouring system thick ester tank top and be provided with charging opening, filtering the thick ester pot bottom discharging of decolouring system decolours after the thick ester pump of system boosts after filtration, one the tunnel enters coarse filter from the bottom, then overflow back from coarse filter top and filter the thick ester tank of decolouring system, another road is after the bottom enters fine filter, then behind smart ester interchanger, send the finished product tank field, then divide to be filled to light transmission container, send uviolizing decolouring district;
(6) sewage water cleaning recovery system comprises that wastewater collection tank, air flotation slot, oil removal are except slag bath, aeration tank, neutralization precipitation pond, quartz filter and charcoal filter, aforesaid device is connected in turn, and the discharge nozzle of esterification system drainer and neutralization/water washing tank all communicates with the wastewater collection tank.
2. dioctyl phthalate production line according to claim 1, it is characterized in that: loading hopper top, the bottom of reaction kettle of the esterification top band valve are equipped with valve, and are provided with a nitrogen pipeline, and nitrogen pipeline is provided with nitrogen pressurization valve.
3. a method of utilizing dioctyl phthalate production line claimed in claim 2 to produce DOTP comprises the steps:
(1) utilize esterification system to carry out esterification, get thick ester still liquid, it is characterized in that, the weight ratio that feeds intake of terephthalic acid and n-Octanol is 1: 2, use titanium ester four isopropyl esters to be catalyzer, the weight ratio of catalyzer and raw material summation is 11000: 9, and titanium ester four isopropyl esters are divided into 9 weight parts, when still temperature rise to 120 ℃, add 5 weight parts, when still temperature rise to 160 ℃, add 2 weight parts, when still temperature rise to 180 ℃, add 2 weight parts, the 2nd, when adding catalyzer 3 times, open first the loading hopper upper valve, behind the adding catalyzer, close again the loading hopper upper valve, open nitrogen pressurization valve, then open loading hopper bottom valve, with nitrogen catalyzer is pressed into reaction kettle of the esterification, close at last loading hopper bottom valve and nitrogen pressurization valve;
(2) utilize the dealcoholysis system that the thick ester still of step (1) gained liquid is carried out thick dealcoholysis, it is characterized in that; The thick ester liquid of the thick ester pot bottom of dealcoholysis system and flashing tower and recycle alcohol tank are to pure liquid heat exchange in a plate-type heat exchanger of pure charging stock tank;
(3) utilize neutralization/water wash system that thick ester liquid is neutralized, washes, it is characterized in that:
Drop into weight content and be 5% buck and neutralize 1., first, stir half an hour after, left standstill 10 minutes, after the layering water in the thick ester liquid is emitted, for subsequent use as a washing water, wherein the volume feed ratio of thick ester liquid and buck is: 1000: 1;
2., in thick ester liquid, add entry, stir washing after 20 minutes, left standstill 10 minutes, after the layering water in the thick ester liquid is emitted, for subsequent use as the intermediate water wash water;
3., in thick ester liquid, add without dried up, thick ester liquid and be without dried up volume feed ratio: 1000: 1, stir washing after 20 minutes, left standstill 10 minutes, the water that layering is emitted in the thick ester liquid is done sewage disposal, remaining thick ester liquid send the filtration decolouring system of filtering the decolouring system thick ester tank after the heat exchange of the thick ester interchanger of neutralization/water wash system;
(4) utilize stripping system that thick ester liquid is carried out smart dealcoholysis, it is characterized in that: during dealcoholysis, open first main road, start water ring vacuum pump and vacuumize, liquid in the flashing tower is carried out the low pressure flash vaporization, when vacuum tightness reaches 0.09 MPa, open bypass, start Roots vaccum pump, then close main road, finish the switching of main road and bypass, Roots vaccum pump and water ring vacuum pump are worked simultaneously and are vacuumized;
(5) utilize filtration decolouring system that thick ester liquid is filtered, decolours, it is characterized in that: during filtration, use first coarse filter, circulating filtration, after the filtrate cleaning to be seen, switch to fine filter filter, after smart ester interchanger cooling, send the finished product tank field, then packing penetrates light transmission container, send uviolizing decolouring district, carries out uviolizing decolouring 24 hours.
4. the method for production according to claim 3 DOTP, it is characterized in that: it comprises that also utilizing sewage water cleaning recovery system to purify reclaims sewage, is characterized in that: before the oil removal slagging-off, carry out air supporting slagging-off, aeration oxide treatment through air flotation slot first.
5. the method for production according to claim 3 DOTP is characterized in that: (3) step the is 1. in the link: select washing water preparation buck in the production cycle; (3) step the is 2. in the link: select in the production cycle intermediate water wash water to wash.
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| CN104610063A (en) * | 2015-01-08 | 2015-05-13 | 宜兴市阳洋塑料助剂有限公司 | Novel preparation method of dioctyl terephthalate |
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| CN106278884A (en) * | 2016-08-22 | 2017-01-04 | 浙江弘博新材料科技有限公司 | The processing technique of DOTP |
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| CN107286016A (en) * | 2016-03-30 | 2017-10-24 | 张开益 | New ester plasticizer production line and its application method |
| CN107286016B (en) * | 2016-03-30 | 2020-04-03 | 张开益 | Ester plasticizer production device and use method thereof |
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| CN106278884A (en) * | 2016-08-22 | 2017-01-04 | 浙江弘博新材料科技有限公司 | The processing technique of DOTP |
| CN109678712A (en) * | 2019-01-29 | 2019-04-26 | 安徽力天环保科技股份有限公司 | A kind of dioctyl phthalate preparation facilities and preparation method thereof |
| CN117486716A (en) * | 2023-12-28 | 2024-02-02 | 天津渤化澳佳永利化工有限责任公司 | DOA production method |
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