CN105198739B - The method and its device of tributyl 2-acetylcitrate semi-continuous production - Google Patents
The method and its device of tributyl 2-acetylcitrate semi-continuous production Download PDFInfo
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- CN105198739B CN105198739B CN201510547198.XA CN201510547198A CN105198739B CN 105198739 B CN105198739 B CN 105198739B CN 201510547198 A CN201510547198 A CN 201510547198A CN 105198739 B CN105198739 B CN 105198739B
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- 238000000034 method Methods 0.000 title claims abstract description 24
- PESZCXUNMKAYME-UHFFFAOYSA-N Citroflex A-4 Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)C(C(C)=O)C(=O)OCCCC PESZCXUNMKAYME-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000010924 continuous production Methods 0.000 title claims abstract description 10
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 35
- 150000002148 esters Chemical class 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 18
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000003860 storage Methods 0.000 claims abstract description 11
- 230000021736 acetylation Effects 0.000 claims abstract description 7
- 238000006640 acetylation reaction Methods 0.000 claims abstract description 7
- 239000012043 crude product Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- 238000002156 mixing Methods 0.000 claims description 33
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 24
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 24
- 239000004571 lime Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- 238000009833 condensation Methods 0.000 claims 2
- 230000005494 condensation Effects 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000009434 installation Methods 0.000 abstract description 3
- 229920001971 elastomer Polymers 0.000 abstract description 2
- 239000005060 rubber Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- 229910001948 sodium oxide Inorganic materials 0.000 description 2
- JBGDSVVIBTXYJD-UHFFFAOYSA-N 2-hydroxy-4-oxopentane-1,2,3-tricarboxylic acid Chemical compound CC(=O)C(C(O)=O)C(O)(C(O)=O)CC(O)=O JBGDSVVIBTXYJD-UHFFFAOYSA-N 0.000 description 1
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- -1 medical product Substances 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to rubber plastizing agent production technical field, and in particular to the method and its device of a kind of tributyl 2-acetylcitrate semi-continuous production.Device used in the present invention includes reactor, and reactor is sequentially connected by pipeline with surge tank, the first booster pump, heater, extracting tower, condenser, vavuum pump, fixed gas tank；Wherein, ATBC tank, acetic anhydride charging device and catalyst charging device have been also respectively connected with outside reactor；Condenser is also connected with acetic acid storage tank；Extracting tower bottom sets reboiler, and reboiler is also sequentially connected with thick ester tank, the second booster pump, continuous water cleaning device；Methods described is specifically：React after obtained acetylation crude product is flashed twice in the heater and washed into continuous water cleaning device.The present invention, which is solved in existing process, to yield poorly, the problem of utilization rate of equipment and installations is poor, production technology is heavy, and its apparatus structure is simple, easily operated.
Description
Technical field
The invention belongs to rubber plastizing agent production technical field, and in particular to a kind of tributyl 2-acetylcitrate is semicontinuous
The method and its device of production.
Background technology
Tributyl 2-acetylcitrate is nontoxic plasticizer, can be used as polyvinyl chloride, the increasing of celluosic resin and synthetic rubber
Mould agent.For nontoxic PVC granulations, food container, toy for children product, medical product, film, sheet material, cellulose paint
Deng product.Also stabilizer of polyvinylidene chloride etc. can be used as.
Traditional tributyl 2-acetylcitrate process units production capacity is all below 10,000 tons/year, between each set process is
Formula of having a rest is operated, and often covering process has reactor, and production technology is heavy, yields poorly, utilization rate of equipment and installations is poor.Tributyl 2-acetylcitrate
In production process, after acetylization reaction occurs, there is acetic acid and excessive acetic anhydride, traditional negative pressure separation method in material
So that poor product quality, side reaction is more.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of tributyl 2-acetylcitrate semi-continuous production
Method, solve in existing process and yield poorly, the problem of utilization rate of equipment and installations is poor, production technology is heavy, investment low with energy consumption
It is few, the characteristics of product yield is high, quality is high；Present invention simultaneously provides the device that it is used.
The method of tributyl 2-acetylcitrate semi-continuous production of the present invention is as follows：
Its used device is as follows：
Including reactor, reactor passes through pipeline and surge tank, the first booster pump, heater, extracting tower, condenser, true
Empty pump, fixed gas tank are sequentially connected；Wherein, ATBC tank, acetic anhydride have been also respectively connected with outside reactor to feed intake dress
Put and catalyst charging device；Condenser is also connected with acetic acid storage tank；Extracting tower bottom sets reboiler, reboiler also with thick ester
Tank, the second booster pump, continuous water cleaning device are sequentially connected；
Continuous water cleaning device includes sodium hydroxide cast feeder, blending tank, lime set tank, return water tank, supercentrifuge and ester
Holding vessel；Blending tank, supercentrifuge, return water tank are sequentially connected by pipeline, and hydrogen-oxygen has been also respectively connected with outside blending tank
Change sodium cast feeder and lime set tank；Supercentrifuge is also connected with ester holding vessel；
The method of described semi-continuous production comprises the following steps：
First, the ATBC in ATBC tank is squeezed into reactor, then, adds and urge into reactor
The catalyst and acetic anhydride of change amount are reacted, and reaction finishes to obtain acetylation crude product, is temporarily stored into surge tank；Then pass through
First booster pump is delivered to heater and heated, and thermal material enters extracting tower after being released at the top of heater, what tower top was steamed
Gas phase is condensed into condenser, and condensed fluid is stored into acetic acid storage tank, and fixed gas is drawn into fixed gas tank through vavuum pump；Depickling
Acetic acid and acetic anhydride are further backing out by the material of tower bottom of towe through reboiler secondary flash；Through the thing after reboiler secondary flash
Material enters thick ester tank, enters continuous water cleaning device after being pressurized through the second booster pump；In continuous water cleaning device, mixing is initially entered
Tank, sodium hydroxide is added into blending tank by sodium hydroxide cast feeder, and lime set is then passed through into blending tank from lime set tank mixes
Close, material is separated into supercentrifuge after mixing, and the water isolated enters return water tank, the acetyl tributyl citrate three isolated
Butyl ester enters ester holding vessel.
Wherein, preferably technical scheme is as follows：
Described catalyst is resin catalyst.
The speed of described addition acetic anhydride is 0.5-2 ton hours, and the time that adds is 2-3 hours.
Described ATBC and the mol ratio of acetic anhydride are 1:1.1-2.
Occur in described reactor for exothermic reaction, course of reaction is condensed using 5-12 DEG C of recirculation water, control
Reaction temperature is below 60 DEG C.
The speed that described acetylation crude product is delivered to heater is that the heating-up temperature in 2-6 ton hours, heater is
100-110℃。
The vacuum of described extracting tower is≤10kPa, and tower top temperature is controlled at 80-105 DEG C.
The column bottom temperature of secondary flash is 100-130 DEG C.
Device used in the method for described tributyl 2-acetylcitrate semi-continuous production, including reactor, reaction
Kettle is sequentially connected by pipeline with surge tank, the first booster pump, heater, extracting tower, condenser, vavuum pump, fixed gas tank；Its
In, ATBC tank, acetic anhydride charging device and catalyst charging device have been also respectively connected with outside reactor；Condenser
Also it is connected with acetic acid storage tank；Extracting tower bottom sets reboiler, reboiler also with thick ester tank, the second booster pump, continuous water cleaning device
It is sequentially connected；
Continuous water cleaning device includes sodium hydroxide cast feeder, blending tank, lime set tank, return water tank, supercentrifuge and ester
Holding vessel；Blending tank, supercentrifuge, return water tank are sequentially connected by pipeline, and hydrogen-oxygen has been also respectively connected with outside blending tank
Change sodium cast feeder and lime set tank；Supercentrifuge is also connected with ester holding vessel.
To improve water washing effect, described continuous water cleaning device is set to continuous 3.When washing for the first time, it is added to
The mixed mass concentration of sodium hydroxide and lime set in blending tank is 2%, during second of washing, is added to the hydrogen in blending tank
Sodium oxide molybdena and the mixed mass concentration of lime set are 1%, when third time is washed, do not add sodium hydroxide, only add lime set.
In summary, beneficial effects of the present invention are as follows：
The present invention by the improvement to deacidifying device and water washing device in tributyl 2-acetylcitrate production process, with reference to
The improvement of production technology, realizes the semi-continuous production of tributyl 2-acetylcitrate, substantially increases yield, improve equipment
Utilization rate, the automaticity of continuous operation is high, and product yield is big, and steady quality, the labor intensity of operative employee also has greatly
The reduction of amplitude；Apparatus structure used in the present invention is simple, easily operated.
Brief description of the drawings
Fig. 1 is the structural representation of apparatus of the present invention；
In figure：1st, ATBC tank；2nd, acetic anhydride charging device；3rd, catalyst charging device；4th, reactor；5th, delay
Rush tank；6th, the first booster pump；7th, heater；8th, extracting tower；9th, reboiler；10th, condenser；11st, acetic acid storage tank；12nd, vavuum pump；
13rd, fixed gas tank；14th, thick ester tank；15th, the second booster pump；16th, sodium hydroxide cast feeder；17th, blending tank；18th, lime set tank；19、
Return water tank；20th, supercentrifuge；21st, ester holding vessel.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
As shown in figure 1, device used in the method for tributyl 2-acetylcitrate semi-continuous production of the present invention
Including reactor 4, it is characterised in that：Reactor 4 by pipeline and surge tank 5, the first booster pump 6, heater 7, extracting tower 8,
Condenser 10, vavuum pump 12, fixed gas tank 13 are sequentially connected；Wherein, ATBC has been also respectively connected with it outside reactor 4
Tank 1, acetic anhydride charging device 2 and catalyst charging device 3；Condenser 10 is also connected with acetic acid storage tank 11；The bottom of extracting tower 8 is set
Reboiler 9, reboiler 9 is also sequentially connected with thick ester tank 14, the second booster pump 15, continuous water cleaning device；
Continuous water cleaning device include sodium hydroxide cast feeder 16, blending tank 17, lime set tank 18, return water tank 19, at a high speed from
Scheming 20 and ester holding vessel 21；Blending tank 17, supercentrifuge 20, return water tank 19 are sequentially connected by pipeline, blending tank 17
Outside has been also respectively connected with sodium hydroxide cast feeder 16 and lime set tank 18；Supercentrifuge 20 is also connected with ester holding vessel 21.
Concrete operations are：
First, the ATBC in ATBC tank 1 is squeezed into reactor 4, then, added into reactor 4
The resin catalyst and acetic anhydride for entering catalytic amount are reacted, and reaction is finished, and obtain acetylation crude product, are temporarily stored up into surge tank
Deposit.Wherein, the speed that acetic anhydride is added is 0.5-2 ton hours, and the time that adds is 2-3 hours；ATBC and acetic anhydride
Mol ratio be 1:1.1-2.In course of reaction, condensed using 5-12 DEG C of recirculation water, controlling reaction temperature is below 60 DEG C.
Then, acetylation crude product is delivered to heater 7 through the first booster pump 6 and heated, transporting velocity be 2-6 tons/
Hour, heating-up temperature is 100-110 DEG C；Thermal material enters extracting tower 8, the vacuum of extracting tower 8 after being released from the top of heater 7
For≤10kPa, tower top temperature is controlled at 80-105 DEG C；The gas phase that tower top is steamed is condensed into condenser 10, and condensed fluid enters
Acetic acid storage tank 11 is stored, and fixed gas is drawn into fixed gas tank 13 through vavuum pump 12；The material of the bottom of towe of extracting tower 8 is through reboiler 9 two
Secondary flash distillation, acetic acid and acetic anhydride are further backing out；The column bottom temperature of secondary flash is 100-130 DEG C.
Material after the secondary flash of reboiler 9 enters thick ester tank 14, enters continuous water after being pressurized through the second booster pump 15
Cleaning device；In continuous water cleaning device, blending tank 17 is initially entered, is added by sodium hydroxide cast feeder 16 into blending tank 17
Sodium hydroxide, is then passed through lime set mixing into blending tank 17, material enters into supercentrifuge 20 after mixing from lime set tank 18
Row separation, the water isolated enters return water tank 19, and the tributyl 2-acetylcitrate isolated enters ester holding vessel 21.
To improve water washing effect, described continuous water cleaning device is set to continuous 3.When washing for the first time, it is added to
The mixed mass concentration of sodium hydroxide and lime set in blending tank is 2%, during second of washing, is added to the hydrogen in blending tank
Sodium oxide molybdena and the mixed mass concentration of lime set are 1%, when third time is washed, do not add sodium hydroxide, only add lime set.
The method of the invention compares with traditional handicraft：
(1) production capacity：The production capacity of traditional handicraft is 0.8 ten thousand tons/year；This method is 50,000 tons/year.
(2) acid number after deacidification process：Traditional handicraft reaches 20mgKOH/g；This method reaches 5mgKOH/g.
(3) purity of product：Traditional handicraft reaches 97.5%；This method reaches 98.5%.
(4) quantity of equipment：It is large scale equipment 21 in traditional handicraft；This method large scale equipment 10.
Claims (1)
1. a kind of method of tributyl 2-acetylcitrate semi-continuous production, its used device includes reactor（4）, it is special
Levy and be：Reactor（4）Pass through pipeline and surge tank（5）, the first booster pump（6）, heater（7）, extracting tower（8）, condenser
（10）, vavuum pump（12）, fixed gas tank（13）It is sequentially connected；Wherein, reactor（4）Outside has been also respectively connected with the fourth of citric acid three
Ester tank（1）, acetic anhydride charging device（2）With catalyst charging device（3）；Condenser（10）Also with acetic acid storage tank（11）It is connected；
Extracting tower（8）Bottom sets reboiler（9）, reboiler（9）Also with thick ester tank（14）, the second booster pump（15）, continuous water cleaning device
It is sequentially connected；
Continuous water cleaning device includes sodium hydroxide cast feeder（16）, blending tank（17）, lime set tank（18）, return water tank（19）, it is high
Fast centrifuge（20）With ester holding vessel（21）；Blending tank（17）, supercentrifuge（20）, return water tank（19）By pipeline successively
It is connected, blending tank（17）Outside has been also respectively connected with sodium hydroxide cast feeder（16）With lime set tank（18）；Supercentrifuge（20）
Also with ester holding vessel（21）It is connected；
Concrete operations are：
First, by ATBC tank（1）In ATBC squeeze into reactor（4）, then, to reactor（4）It is interior
The resin catalyst and acetic anhydride for adding catalytic amount are reacted, and reaction is finished, and obtains acetylation crude product, into surge tank（5）
Temporarily storage；Wherein, the speed that acetic anhydride is added is 0.5-2 ton hours, and the time that adds is 2-3 hours；ATBC with
The mol ratio of acetic anhydride is 1:1.1-2；In course of reaction, condensed using 5-12 DEG C of recirculation water, controlling reaction temperature is 60
Below DEG C；
Then, acetylation crude product is through the first booster pump（6）It is delivered to heater（7）Heated, transporting velocity be 2-6 tons/
Hour, heating-up temperature is 100-110 DEG C；Thermal material is from heater（7）Top enters extracting tower after releasing（8）, extracting tower（8）'s
Vacuum is≤10kPa, and tower top temperature is controlled at 80-105 DEG C；The gas phase that tower top is steamed enters condenser（10）Condensation, condensation
Liquid enters acetic acid storage tank（11）Storage, fixed gas is through vavuum pump（12）It is drawn into fixed gas tank（13）；Extracting tower（8）Bottom of towe
Material is through reboiler（9）Secondary flash, acetic acid and acetic anhydride are further backing out；The column bottom temperature of secondary flash is 100-130
℃；
Through reboiler（9）Material after secondary flash enters thick ester tank（14）, through the second booster pump（15）Enter after supercharging continuous
Water washing device；In continuous water cleaning device, blending tank is initially entered（17）, pass through sodium hydroxide cast feeder（16）To blending tank
（17）Sodium hydroxide is inside added, then by lime set tank（18）To blending tank（17）Lime set mixing is inside passed through, material enters after mixing
Supercentrifuge（20）Separated, the water isolated enters return water tank（19）, the tributyl 2-acetylcitrate entrance isolated
Ester holding vessel（21）；
Described continuous water cleaning device is continuous 3；
When washing for the first time, blending tank is added to（17）The interior mixed mass concentration of sodium hydroxide and lime set is 2%, second
During secondary washing, blending tank is added to（17）The interior mixed mass concentration of sodium hydroxide and lime set is 1%, when third time is washed,
Sodium hydroxide is not added, lime set is only added；
The production capacity of methods described is 50,000 tons/year；Acid number after deacidification process is 5mgKOH/g；Product purity reaches 98.5%；Adopt
The quantity of large scale equipment is 10.
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| CN201510547198.XA CN105198739B (en) | 2015-08-31 | 2015-08-31 | The method and its device of tributyl 2-acetylcitrate semi-continuous production |
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|---|---|---|---|
| CN201510547198.XA CN105198739B (en) | 2015-08-31 | 2015-08-31 | The method and its device of tributyl 2-acetylcitrate semi-continuous production |
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| CN105198739B true CN105198739B (en) | 2017-09-29 |
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| CN110305013A (en) * | 2019-08-05 | 2019-10-08 | 江苏开来医药科技有限公司 | The preparation method of acetyl tributyl citrate |
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Effective date of registration: 20201015 Address after: 255400 Jinshan Economic Development Zone, Linzi District, Shandong, Zibo Patentee after: Shandong Langhui Grand Pacific Petrochemical Co. Address before: 255400 Qilu Chemical Industry Zone, Linzi District, Shandong, Zibo Patentee before: ZIBO BLUE SAIL CHEMICAL Co.,Ltd. |
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Denomination of invention: Method and device for semi continuous production of acetyl tributyl citrate Effective date of registration: 20211129 Granted publication date: 20170929 Pledgee: Qi commercial bank Limited by Share Ltd. Linzi branch Pledgor: Shandong Langhui Grand Pacific Petrochemical Co. Registration number: Y2021980013506 |
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Date of cancellation: 20220818 Granted publication date: 20170929 Pledgee: Qi commercial bank Limited by Share Ltd. Linzi branch Pledgor: Shandong Langhui Grand Pacific Petrochemical Co. Registration number: Y2021980013506 |
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Denomination of invention: Method and device for semi continuous production of tributyl acetylcitrate Effective date of registration: 20231207 Granted publication date: 20170929 Pledgee: Qi commercial bank Limited by Share Ltd. Linzi branch Pledgor: Shandong Langhui Grand Pacific Petrochemical Co. Registration number: Y2023980069984 |