CN107286016B - Ester plasticizer production device and use method thereof - Google Patents
Ester plasticizer production device and use method thereof Download PDFInfo
- Publication number
- CN107286016B CN107286016B CN201610191841.4A CN201610191841A CN107286016B CN 107286016 B CN107286016 B CN 107286016B CN 201610191841 A CN201610191841 A CN 201610191841A CN 107286016 B CN107286016 B CN 107286016B
- Authority
- CN
- China
- Prior art keywords
- ester
- tank
- valve
- esterification
- scraper evaporator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 150000002148 esters Chemical class 0.000 title claims abstract description 119
- 239000004014 plasticizer Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005886 esterification reaction Methods 0.000 claims abstract description 59
- 238000001914 filtration Methods 0.000 claims abstract description 51
- 230000032050 esterification Effects 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003513 alkali Substances 0.000 claims abstract description 27
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000002351 wastewater Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 37
- 239000003054 catalyst Substances 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000013461 design Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- -1 n-propyl titanate Chemical compound 0.000 description 4
- HORIEOQXBKUKGQ-UHFFFAOYSA-N bis(7-methyloctyl) cyclohexane-1,2-dicarboxylate Chemical compound CC(C)CCCCCCOC(=O)C1CCCCC1C(=O)OCCCCCCC(C)C HORIEOQXBKUKGQ-UHFFFAOYSA-N 0.000 description 3
- BJAJDJDODCWPNS-UHFFFAOYSA-N dotp Chemical compound O=C1N2CCOC2=NC2=C1SC=C2 BJAJDJDODCWPNS-UHFFFAOYSA-N 0.000 description 3
- 239000004808 2-ethylhexylester Substances 0.000 description 2
- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 description 2
- SAOKZLXYCUGLFA-UHFFFAOYSA-N bis(2-ethylhexyl) adipate Chemical compound CCCCC(CC)COC(=O)CCCCC(=O)OCC(CC)CCCC SAOKZLXYCUGLFA-UHFFFAOYSA-N 0.000 description 2
- YKGYQYOQRGPFTO-UHFFFAOYSA-N bis(8-methylnonyl) hexanedioate Chemical compound CC(C)CCCCCCCOC(=O)CCCCC(=O)OCCCCCCCC(C)C YKGYQYOQRGPFTO-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000004806 diisononylester Substances 0.000 description 2
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ALKCLFLTXBBMMP-UHFFFAOYSA-N 3,7-dimethylocta-1,6-dien-3-yl hexanoate Chemical compound CCCCCC(=O)OC(C)(C=C)CCC=C(C)C ALKCLFLTXBBMMP-UHFFFAOYSA-N 0.000 description 1
- 239000004135 Bone phosphate Substances 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 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 description 1
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 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 description 1
- MIMDHDXOBDPUQW-UHFFFAOYSA-N dioctyl decanedioate Chemical compound CCCCCCCCOC(=O)CCCCCCCCC(=O)OCCCCCCCC MIMDHDXOBDPUQW-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- WDRCVXGINNJWPH-UHFFFAOYSA-N tris(6-methylheptyl) benzene-1,2,4-tricarboxylate Chemical compound CC(C)CCCCCOC(=O)C1=CC=C(C(=O)OCCCCCC(C)C)C(C(=O)OCCCCCC(C)C)=C1 WDRCVXGINNJWPH-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to an ester plasticizer production device and a using method thereof. The existing ester plasticizer production equipment and method have the disadvantages of large energy consumption, long time, complex operation and more wastewater generation. The novel ester plasticizer production device comprises an esterification system and a filtering system, wherein the esterification system comprises an esterification reaction kettle, a packed tower, an esterification condenser and an esterification condensing tank, the filtering system comprises a filtering crude ester tank, a filtering pump and a filter, the esterification system and a neutralization-stripping system are further arranged between the filtering systems, the neutralization-stripping system comprises a scraper evaporator, a stripping condenser, an alcohol-water separation tank and a water ring vacuum pump, the invention uses the scraper evaporator to replace a flash tower and a neutralization/water washing tank, introduces alkali liquor into the scraper evaporator by using steam, and performs neutralization and water washing while flashing, thereby greatly simplifying the whole subsequent process and equipment.
Description
Technical Field
The invention relates to an ester plasticizer production device and a using method thereof.
Background
DOTP plasticizer (dioctyl terephthalate), DOA plasticizer (dioctyl adipate), DOS plasticizer (dioctyl sebacate), TOTM plasticizer (triisooctyl trimellitate), DINCH plasticizer (diisononyl cyclohexane 1, 2-dicarboxylate) and DIDA plasticizer (diisodecyl adipate) are all ester plasticizers. In the prior art, the plasticizers are prepared by esterification reaction of binary or ternary organic acid and corresponding alcohol, dealcoholization, neutralization, washing and filtration, and are prepared by heating esterification (the esterification reaction needs to be heated to 220 ℃), cooling neutralization (the traditional neutralization needs to be carried out at about 90 ℃), heating washing (neutralization leads the material to be cooled, the washing can be carried out after the temperature is firstly raised to 95 ℃, and the washing needs to be carried out for 2 times and is lifted twice), heating stripping (the temperature needs to be raised to 165 ℃), and finally cooling filtration (the temperature needs to be lowered to below 130 ℃), the whole process is repeatedly lifted, the number of equipment is large, the energy consumption is large, and the operation is complicated.
The invention discloses a dioctyl phthalate production line and a DOTP production method in Chinese patent with the publication number of CN102952019B and publication date of 2014, 07, 09, and by utilizing the production line and the method, corresponding alcohols and binary acid or tribasic acid raw materials are added, and DOTP, DOA, DOS, TOTM, DINCH, DIDA and other ester plasticizers can also be produced.
However, in the above method, dealcoholization, neutralization and washing need to be carried out in different equipment and at different times, and the crude ester material needs to be repeatedly heated and cooled, so that the energy consumption is high, the time is long, the operation is complicated, and more waste water is generated.
Disclosure of Invention
The technical problem to be solved by the invention is how to overcome the defects in the prior art, and an ester plasticizer production device and a use method thereof are provided.
In order to solve the technical problem, the ester plasticizer production device comprises an esterification system and a filtering system, wherein the esterification system comprises an esterification reaction kettle, a packing tower, an esterification condenser and an esterification condensing tank, and is characterized in that: a neutralization-stripping system is also arranged between the esterification system and the filtration system, the neutralization-stripping system comprises a scraper evaporator, a stripping condenser, an alcohol-water separation tank and a water ring vacuum pump, the top of the scraper evaporator is provided with a feed inlet and a flash vapor outlet, the bottom of the scraper evaporator is provided with a discharge outlet, a vapor pipe and a vapor feed valve, the outer wall of the scraper evaporator is provided with a jacket, the jacket is connected in series with an oil circuit of a heat conduction oil circulation system, a discharge pipe at the bottom of the esterification reaction kettle is communicated with the feed inlet at the top of the scraper evaporator through an esterification discharge valve and/or an esterification discharge pump, the flash vapor outlet at the top of the scraper evaporator is connected with the stripping condenser, the vapor pipe is also provided with an alkali liquor feed pipe and an alkali liquor valve, the discharge outlet at the bottom of the scraper evaporator is connected with a crude ester buffer tank through a liquid seal tank, the discharge pipe of the crude ester discharge pump is divided into a main path and a bypass path, the main path and the bypass path are respectively provided with a main path valve and a bypass valve, the main path is introduced into the filtering system through the crude ester heat exchanger, and the bypass path is introduced into the scraper evaporator from the top of the scraper evaporator through the bypass valve.
By adopting the design, the scraper evaporator is used for replacing a flash tower and a neutralization/water washing tank, alkali liquor is introduced into the scraper evaporator by using steam, neutralization and water washing are carried out during flash evaporation, no water is added in the whole process, only the steam is carried into the scraper evaporator and a small amount of water condensed in the scraper evaporator is used for water washing, the whole subsequent process and equipment are greatly simplified, the water is saved by 40 percent, the energy is saved by 30 percent, the production period is shortened by 6 hours, and the wastewater discharge is greatly reduced.
Preferably, a jet pump is arranged on the steam pipe, and a suction inlet of the jet pump is connected with the alkali liquor charging pipe and the alkali liquor charging valve. By the design, after the steam feed valve is opened, the alkali liquor feed valve is opened again, and the alkali liquor can be automatically sucked into the steam and fully mixed with the steam to enter the scraper evaporator together. High neutralization efficiency and good effect.
Preferably, the filtering system comprises a filtering coarse ester tank, a coarse filter and a fine filter, wherein a coarse ester material from a coarse ester heat exchanger is added into the filtering coarse ester tank from a feeding port at the top of the filtering coarse ester tank, a discharge material at the bottom of the filtering coarse ester tank is boosted by a coarse ester filtering pump and enters the coarse filter from the lower part, one path of the discharge material overflows from the upper part of the coarse filter and returns to the filtering coarse ester tank, and the other path of the discharge material is subjected to heat exchange by the fine ester heat exchanger and then is sent to a finished product tank. So design, the filter effect is good.
The use method of the ester plasticizer production device comprises the following steps:
(1) carrying out esterification reaction by using an esterification system: respectively adding an acid raw material and an alcohol raw material according to a reaction ratio, and preparing a crude ester kettle solution by using a titanate catalyst;
(2) carrying out dealcoholization, neutralization and stripping treatment on the crude ester kettle liquid obtained in the step (1) by using a neutralization-stripping system:
starting a motor at the top of the scraper evaporator, starting a stripping condenser and a water ring vacuum pump to heat the scraper evaporator to 165-185 ℃, starting a heat conduction oil circulation system to heat if necessary, starting an esterification discharge valve and an esterification discharge pump, adding kettle liquid from an esterification reaction kettle from the top of the scraper evaporator, and simultaneously starting a steam feed valve and an alkali liquor feed valve, wherein the volume feed ratio of the kettle liquid to the alkali liquor of the esterification reaction kettle is as follows: 1000:1, wherein the alkali liquor is a sodium hydroxide aqueous solution with the weight content of 5%.
After steam at the top of the scraper evaporator is condensed by a stripping condenser, uncondensed gas is pumped out by a water ring vacuum pump, liquid enters an alcohol-water separation tank, and is separated by the alcohol-water separation tank, water is placed in a waste water tank, and alcohol materials are placed in a circulating alcohol tank;
the crude ester material at the bottom of the scraper evaporator enters a crude ester buffer tank through a liquid seal tank, sampling and testing are carried out to judge whether the crude ester material meets the requirements of finished product plasticizer on moisture and pH value, if the crude ester material is qualified, a crude ester discharging pump is started, and the crude ester material is sent to a filtering system through a main path valve and a crude ester heat exchanger; if the crude ester is not qualified, the crude ester discharge pump is started, the crude ester flows back to the scraper evaporator through the bypass valve, dealcoholization, neutralization and steam stripping are carried out until the crude ester at the bottom of the scraper evaporator is qualified, and then the crude ester is sent to the filtering system. By using the production device and the method, 90 percent of the obtained crude ester material is qualified at one time, and the method has obvious progress compared with the original neutralization water washing process.
(3) The crude ester material was filtered using a filtration system: and (3) after the crude ester material obtained in the step (2) is received, filtering out the catalyst and other impurities, and conveying the filtrate to a finished product tank after the filtrate is observed to be clean. The design completes dealcoholization, neutralization, water washing and steam stripping in one step, and is simple, convenient, economical and environment-friendly.
In the step (1), the weight ratio of the total amount of the raw materials to the catalyst is 11000:9, the titanate catalyst is added when the temperature of the kettle rises to 145 ℃, an upper valve of a catalyst feeding funnel is opened, the upper valve of the catalyst feeding funnel is closed after the catalyst is added, a nitrogen pressurizing valve is opened, a lower valve of the catalyst feeding funnel is opened, the catalyst is pressed into the esterification reaction kettle by nitrogen, and finally the lower valve of the catalyst feeding funnel and the nitrogen pressurizing valve are closed. By the design, the reaction effect is good.
The ester plasticizer production device and the use method thereof have the advantages of water saving, energy saving, high efficiency and high product quality, and are suitable for processing and preparing various ester plasticizers.
Drawings
The ester plasticizer production device and the use method thereof of the present invention are further described with reference to the accompanying drawings:
FIG. 1 is a schematic flow chart of the production apparatus of the ester plasticizer.
In fig. 1: b101 is a circulating alcohol tank, B102 is an alcohol feeding tank, B103 is an esterification condensing tank, B105 is an esterification crude ester buffer tank, B106 is a water ring vacuum pump sealed water collecting tank, B107A is a liquid seal tank, B107B is a crude ester buffer tank, B109 is an alkali liquor tank, B114 is an alcohol-water separation tank, B115 is a finished product tank, B116 is a raw material alcohol tank, F1 is a steam feeding valve, F2 is an alkali liquor feeding valve, F3 is an esterification discharging valve, F4 is a main way valve, F5 is a bypass way valve, G102 is a fine filter, G104 is a crude filter, G105 is a scraper evaporator, K101 is a packed tower, L1 is a main way of a crude ester discharging pump discharging pipe, L2 is a bypass way of a crude ester discharging pipe pump, P101 is a circulating alcohol pump, P102 is a filtering crude ester pump, P103 is a filtering crude ester pump, P106 is a water ring vacuum pump, P115 is a crude ester discharging pump, P115 is a finished product pump, R116 is a filtering tank, R101 is a waste material collecting tank, and R101 is a waste alcohol tank, W101A and W101B are esterification condensers, W102A and W102B are stripping condensers, W104 is a crude ester heat exchanger, and W108 is a refined ester heat exchanger.
Detailed Description
The first implementation mode comprises the following steps: as shown in fig. 1, the ester plasticizer production apparatus of the present invention comprises an esterification system and a filtration system, wherein the esterification system comprises an esterification reaction kettle R101, a packed tower K101, esterification condensers W102A, W102B, and an esterification condensation tank B103, and is characterized in that: a neutralization-stripping system is also arranged between the esterification system and the filtration system, the neutralization-stripping system comprises a scraper evaporator G105, stripping condensers W102A and W102B, an alcohol-water separation tank B114 and a water ring vacuum pump P106, the top of the scraper evaporator G105 is provided with a feed inlet and a flash steam outlet, the bottom of the scraper evaporator G105 is provided with a discharge outlet, a steam pipe and a steam feed valve F1, the outer wall of the scraper evaporator G105 is provided with a jacket, the jacket is connected in series on an oil circuit of a heat conduction oil circulation system, and a discharge pipe at the bottom of the esterification reaction kettle R101 is communicated with the feed inlet of the top of the scraper evaporator G105 through an esterification discharge valve F3 and an esterification discharge pump P102 (certainly, the esterification discharge pump P102 can be omitted due to enough height difference, and the process is.
The flash evaporation gas outlet at the top of the scraper evaporator G105 is connected with stripping condensers W102A and W102B, an alkali liquor feeding pipe and an alkali liquor feeding valve F2 are further arranged on the steam pipe, a discharge port at the bottom of the scraper evaporator G105 is connected with a crude ester buffer tank B107B through a liquid seal tank B107A, a crude ester discharge pump P107 is connected below the crude ester buffer tank B107B, discharge pipes of the crude ester discharge pump P107 are divided into a main path L1 and a bypass L2, and are respectively provided with a main path valve F4 and a bypass valve F5, the main path is introduced into a filtering system through the main path valve F4 and the crude ester heat exchanger W104, and the bypass is introduced into the scraper evaporator G105 through the bypass valve F5 and the scraper evaporator top G105.
A jet pump (not shown in the figure) is arranged on the steam pipe, and a suction inlet of the jet pump is connected with the alkali liquor feeding pipe and the alkali liquor feeding valve F2.
The filtering system comprises a filtering crude ester tank R103, a crude filter G104 and a fine filter G102, wherein crude ester materials from a crude ester heat exchanger W104 are added into the filtering crude ester tank R103 from a feed inlet at the top of the filtering crude ester tank R103, the discharge material at the bottom of the filtering crude ester tank R103 enters the crude filter G104 from the lower part after being boosted by a filtering crude ester pump P103, then one path of the discharge material overflows from the upper part of the crude filter G104 and returns to the filtering crude ester tank R103, and the other path of the discharge material is sent to a finished product tank B115 after being subjected to heat exchange by a fine ester heat exchanger W108.
The using method of the ester plasticizer production device comprises the following steps:
(1) carrying out esterification reaction by using an esterification system: respectively adding an acid raw material and an alcohol raw material according to a reaction ratio, and preparing a crude ester kettle solution by using a titanate catalyst (n-butyl titanate, n-propyl titanate, n-octyl titanate or a mixture of the n-butyl titanate, the n-propyl titanate and the n-octyl titanate);
(2) carrying out dealcoholization, neutralization and stripping treatment on the crude ester kettle liquid obtained in the step (1) by using a neutralization-stripping system:
starting a motor at the top of a scraper evaporator G105, starting stripping condensers W102A, W102B and a water ring vacuum pump P106 to heat the scraper evaporator G105 to 165-185 ℃, starting a heat conduction oil circulating system to heat if necessary, starting an esterification discharge valve F3 and an esterification discharge pump P102, adding kettle liquid from an esterification reaction kettle R101 from the top G105 of the scraper evaporator, and simultaneously starting a steam feed valve F1 and an alkali liquor feed valve F2, wherein the volume feed ratio of the kettle liquid to the alkali liquor of the esterification reaction kettle R101 is as follows: 1000:1, wherein the alkali liquor is a sodium hydroxide aqueous solution with the weight content of 5%.
After steam at the top G105 of the scraper evaporator is condensed by stripping condensers W102A and W102B, uncondensed gas is pumped out by a water ring vacuum pump P106, liquid enters an alcohol-water separation tank B114, and is separated by the alcohol-water separation tank B114, water is put into a waste water tank T101, and alcohol materials are put into a circulating alcohol tank B101;
the crude ester material at the bottom of the scraper evaporator G105 enters a crude ester buffer tank B107B through a liquid seal tank B107A, sampling and testing are carried out to judge whether the crude ester material meets the requirements of finished product plasticizer on moisture and pH value, if the crude ester material is qualified, a crude ester discharge pump P107 is started, and the crude ester material is sent to a filtering system through a main path valve F4 and a crude ester heat exchanger W104; if the crude ester is not qualified, the crude ester discharge pump P107 is started, the crude ester flows back to the scraper evaporator G105 through a bypass valve F5, dealcoholization, neutralization and stripping are carried out until the crude ester at the bottom of the scraper evaporator G105 is qualified, and then the crude ester is sent to a filtering system.
The discharge temperature of the crude ester material at the bottom of the scraper evaporator G105 is controlled to be 130 +/-5 ℃, a heat-conducting oil heating system is started when the temperature is low, and a heat exchanger is started when the temperature is high.
(3) The crude ester material was filtered using a filtration system: after the crude ester material obtained in the step (2) is received, the catalyst and other impurities are filtered, and after the filtrate is observed to be clean, the filtrate is sent to a finished product tank B115.
In the step (1), the weight ratio of the total amount of the raw materials to the catalyst is 11000:9, the titanate catalyst is added when the temperature of the kettle rises to 145 ℃, the upper valve of the catalyst feeding funnel is opened, the upper valve of the catalyst feeding funnel is closed after the catalyst is added, the nitrogen pressurization valve is opened, the lower valve of the catalyst feeding funnel is opened, the catalyst is pressed into the esterification reaction kettle by nitrogen, and finally the lower valve of the catalyst feeding funnel and the nitrogen pressurization valve are closed.
Claims (5)
1. The utility model provides an ester plasticizer apparatus for producing, is including system and the filtration system of esterifying, and the system of esterifying is including esterification reaction cauldron, packed tower, esterification condenser and the condensing tank of esterifying, its characterized in that: a neutralization-stripping system is also arranged between the esterification system and the filtration system, the neutralization-stripping system comprises a scraper evaporator, a stripping condenser, an alcohol-water separation tank and a water ring vacuum pump, the top of the scraper evaporator is provided with a feed inlet and a flash vapor outlet, the bottom of the scraper evaporator is provided with a discharge outlet, a vapor pipe and a vapor feed valve, the outer wall of the scraper evaporator is provided with a jacket, the jacket is connected in series with an oil circuit of a heat conduction oil circulation system, a discharge pipe at the bottom of the esterification reaction kettle is communicated with the feed inlet at the top of the scraper evaporator through an esterification discharge valve and/or an esterification discharge pump, the flash vapor outlet at the top of the scraper evaporator is connected with the stripping condenser, the vapor pipe is also provided with an alkali liquor feed pipe and an alkali liquor valve, the discharge outlet at the bottom of the scraper evaporator is connected with a crude ester buffer tank through a liquid seal tank, the discharge pipe of the crude ester discharge pump is divided into a main path and a bypass path, the main path and the bypass path are respectively provided with a main path valve and a bypass valve, the main path is introduced into the filtering system through the crude ester heat exchanger, and the bypass path is introduced into the scraper evaporator from the top of the scraper evaporator through the bypass valve.
2. The ester plasticizer production apparatus according to claim 1, wherein: the steam pipe is provided with a jet pump, and a suction inlet of the jet pump is connected with the alkali liquor charging pipe and the alkali liquor charging valve.
3. The ester plasticizer production apparatus according to claim 1, wherein: the filtering system comprises a filtering coarse ester tank, a coarse filter and a fine filter, wherein a coarse ester material from a coarse ester heat exchanger is added into the filtering coarse ester tank from a feed inlet at the top of the filtering coarse ester tank, the discharge material at the bottom of the filtering coarse ester tank is boosted by a filtering coarse ester pump and enters the coarse filter from the lower part, one path of the discharge material overflows from the upper part of the coarse filter and returns to the filtering coarse ester tank, and the other path of the discharge material is subjected to heat exchange by the fine ester heat exchanger and then is sent to a finished product tank.
4. A method for using the ester plasticizer production apparatus as set forth in claim 1, 2 or 3, comprising the steps of:
(1) carrying out esterification reaction by using an esterification system: respectively adding an acid raw material and an alcohol raw material according to a reaction ratio, and preparing a crude ester kettle solution by using a titanate catalyst;
(2) carrying out dealcoholization, neutralization and stripping treatment on the crude ester kettle liquid obtained in the step (1) by using a neutralization-stripping system:
starting a motor at the top of the scraper evaporator, starting a stripping condenser and a water ring vacuum pump to heat the scraper evaporator to 165-185 ℃, starting a heat conduction oil circulation system to heat if necessary, starting an esterification discharge valve and an esterification discharge pump, adding kettle liquid from an esterification reaction kettle from the top of the scraper evaporator, and simultaneously starting a steam feed valve and an alkali liquor feed valve, wherein the volume feed ratio of the kettle liquid to the alkali liquor of the esterification reaction kettle is as follows: 1000:1, wherein the alkali liquor is a sodium hydroxide aqueous solution with the weight content of 5 percent,
after steam at the top of the scraper evaporator is condensed by a stripping condenser, uncondensed gas is pumped out by a water ring vacuum pump, liquid enters an alcohol-water separation tank, and is separated by the alcohol-water separation tank, water is placed in a waste water tank, and alcohol materials are placed in a circulating alcohol tank;
the crude ester material at the bottom of the scraper evaporator enters a crude ester buffer tank through a liquid seal tank, sampling and testing are carried out to judge whether the crude ester material meets the requirements of finished product plasticizer on moisture and pH value, if the crude ester material is qualified, a crude ester discharging pump is started, and the crude ester material is sent to a filtering system through a main path valve and a crude ester heat exchanger; if the crude ester is not qualified, starting a crude ester discharge pump, refluxing to the scraper evaporator through a bypass valve, performing dealcoholization, neutralization and steam stripping treatment until the crude ester at the bottom of the scraper evaporator is qualified, and then sending into a filtering system;
(3) the crude ester material was filtered using a filtration system: and (3) after the crude ester material obtained in the step (2) is received, filtering out the catalyst and other impurities, and conveying the filtrate to a finished product tank after the filtrate is observed to be clean.
5. The use method of an ester plasticizer production apparatus according to claim 4, characterized in that: the weight ratio of the total raw materials and the catalyst in the step (1) is 11000:9, the titanate catalyst is added when the temperature of the kettle rises to 145 ℃, the upper valve of the catalyst feeding funnel is opened, the upper valve of the catalyst feeding funnel is closed after the catalyst is added, the nitrogen pressurization valve is opened, the lower valve of the catalyst feeding funnel is opened, the catalyst is pressed into the esterification reaction kettle by nitrogen, and finally the lower valve of the catalyst feeding funnel and the nitrogen pressurization valve are closed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610191841.4A CN107286016B (en) | 2016-03-30 | 2016-03-30 | Ester plasticizer production device and use method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610191841.4A CN107286016B (en) | 2016-03-30 | 2016-03-30 | Ester plasticizer production device and use method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107286016A CN107286016A (en) | 2017-10-24 |
| CN107286016B true CN107286016B (en) | 2020-04-03 |
Family
ID=60087077
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610191841.4A Active CN107286016B (en) | 2016-03-30 | 2016-03-30 | Ester plasticizer production device and use method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107286016B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4241216A (en) * | 1979-01-02 | 1980-12-23 | Basf Wyandotte Corporation | Phthalic acid diester preparation with waste stream purification and recycle |
| CN101486923A (en) * | 2009-02-05 | 2009-07-22 | 迟洪军 | Environment friendly process for biodiesel |
| CN102952019A (en) * | 2011-08-17 | 2013-03-06 | 张炜海 | Dioctyl phthalate production line and DOTP production method |
| CN105330539A (en) * | 2015-11-26 | 2016-02-17 | 山东蓝帆化工有限公司 | Production process of dibutyl phthalate plasticizer |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050059837A1 (en) * | 2003-09-15 | 2005-03-17 | Cooper Cynthia Kiest | Method for producing butyl acrylate |
-
2016
- 2016-03-30 CN CN201610191841.4A patent/CN107286016B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4241216A (en) * | 1979-01-02 | 1980-12-23 | Basf Wyandotte Corporation | Phthalic acid diester preparation with waste stream purification and recycle |
| CN101486923A (en) * | 2009-02-05 | 2009-07-22 | 迟洪军 | Environment friendly process for biodiesel |
| CN102952019A (en) * | 2011-08-17 | 2013-03-06 | 张炜海 | Dioctyl phthalate production line and DOTP production method |
| CN105330539A (en) * | 2015-11-26 | 2016-02-17 | 山东蓝帆化工有限公司 | Production process of dibutyl phthalate plasticizer |
Non-Patent Citations (2)
| Title |
|---|
| 100kt/a邻苯二甲酸二辛酯生产装置国产化设计;罗文聆;《化工设计》;20051231;第15卷(第1期);第11-14页 * |
| DOP装置汽提工序的研究;张健春 等;《精细石油化工进展》;20021031;第3卷(第10期);第45-47页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107286016A (en) | 2017-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102952019B (en) | Dioctyl phthalate production line and DOTP production method | |
| CN103359736B (en) | A kind of method from crystalline silicon cutting waste mortar synthesis silicon carbide powder | |
| CN105330539B (en) | Plasticized with Dibutyl Phthalate agent producing process | |
| CN102911036A (en) | Method for obtaining high pure dicarboxylic acid | |
| CN108558644B (en) | Production process and device of industrial oleic acid | |
| CN101870648B (en) | Method for recovering benzoic acid from PTA oxidation residue | |
| CN105130804A (en) | Production method of environmental friendly plasticizer DOTP and production system | |
| CN105695104B (en) | In-tower pumping type high-vacuum rectification method and device for precisely separating C16-C22 fatty acids | |
| CN112876357A (en) | Production process for producing plasticizer from PTA oxidation residues | |
| CN107286016B (en) | Ester plasticizer production device and use method thereof | |
| KR101623864B1 (en) | Method and apparatus for purifying glycerin generated in the preparing of bio diesel | |
| CN102371078B (en) | Recovery method for ionic liquid solvent generated from homogeneous acylation reaction of cellulose | |
| CN105524712B (en) | The degreasing plant of a kind of Oleum Brassicae campestris and technique thereof | |
| CN103772186A (en) | Refining method of fermented organic acid | |
| CN107216253A (en) | A kind of utilization enzyme-chemically United Technologies extract the production method of VE, sterol from soybean oil deodorizer distillate | |
| CN210261601U (en) | Continuous production device of dioctyl adipate | |
| CN109879760B (en) | Method for preparing dioctyl terephthalate by alcoholysis esterification of polyester waste | |
| CN109503361B (en) | Method and device for extracting organic tin from sodium acetate as byproduct of sucralose | |
| CN104743694B (en) | Recycling processing method and device of heavy metal ion-containing organic acid wastewater | |
| CN105315149B (en) | A kind of method for preparing sodium citrate | |
| CN109970688B (en) | Method for preparing epoxy plasticizer from waste grease and product | |
| CN103752075B (en) | Method for removing and separating residual solid impurities out of reaction products in production of aluminum alkyl | |
| CN101659684B (en) | Method for recovering lincomycin from waste active carbon decolorized by lincomycin | |
| CN102616969A (en) | Pure terephthalic acid (PTA) mother liquor recycling system and recycling method thereof | |
| CN214781579U (en) | Device for recovering hexamethylcyclotrisiloxane in vented hot gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240109 Address after: 256300 West Side of East Ring Road, Economic Development Zone, Gaoqing County, Zibo City, Shandong Province Patentee after: Shandong Meisheng Energy Technology Co.,Ltd. Address before: No. 36, Liujia North Living Area, Wenshao Road, Linzi District, Zibo City, Shandong Province, 255400 Patentee before: Zhang Kaiyi |