CN106674007A - Production method of triethylene glycol di-2-ethylhexoate - Google Patents
Production method of triethylene glycol di-2-ethylhexoate Download PDFInfo
- Publication number
- CN106674007A CN106674007A CN201611220377.3A CN201611220377A CN106674007A CN 106674007 A CN106674007 A CN 106674007A CN 201611220377 A CN201611220377 A CN 201611220377A CN 106674007 A CN106674007 A CN 106674007A
- Authority
- CN
- China
- Prior art keywords
- production method
- ethylenedioxybis
- ethanol
- tricaprylate
- pressure
- 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.)
- Pending
Links
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- -1 isooctyl Chemical group 0.000 claims description 14
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 8
- 239000001119 stannous chloride Substances 0.000 claims description 8
- 235000011150 stannous chloride Nutrition 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 239000004408 titanium dioxide Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000013517 stratification Methods 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 230000009471 action Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- 238000006356 dehydrogenation reaction Methods 0.000 abstract 2
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 239000000686 essence Substances 0.000 description 5
- 230000032050 esterification Effects 0.000 description 4
- 238000005886 esterification reaction Methods 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a production method of triethylene glycol di-2-ethylhexoate. The production method is characterized in that isocaprylic acid and triethylene glycol are taken as raw materials and sent into a stirring reaction kettle under the action of a catalyst for a negative-pressure and low-temperature reaction; after the reaction ends, an obtained reaction fluid is subjected to coarse filtration, filtrate is sent into a dehydrogenation kettle for dehydrogenation, and a triethylene glycol di-2-ethylhexoate crude product is prepared; finally, the crude product is neutralized, washed with water, dewatered and finely filtered, and a colorless, transparent and oily triethylene glycol di-2-ethylhexoate finished product is obtained. The novel catalyst is used, a negative-pressure and low-temperature process is adopted, the product is easy to produce, follow-up fine treatment is performed on the product, and accordingly, the production efficiency and the product purity are improved.
Description
Technical field
The present invention relates to a kind of production method of the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two.
Background technology
The tricaprylate of 2,2'-ethylenedioxybis(ethanol). two is a liquid kind colourless, slightly odorous, with good durability, UV resistant and anti-
Antistatic property, water insoluble and mineral oil dissolves in various organic solvents, is polyvinyl butyral resin and elastomeric specially good effect
Plasticizer, makes product produce low-temperature characteristics and low volatility feature, and its molecular structure can make machining object possess the good transparency
And colourity.The tricaprylate of 2,2'-ethylenedioxybis(ethanol). two can also be used for binding agent and encapsulant, be polrvinyl chloride, cellulosicss and styrene
Deng product plasticizer.It is indispensable in the film course of processing as the speciality plasticizer of polyvinyl butyral film
Raw material, thus be used widely in the field of polyvinyl butyral resin intermediate coat.
At present the domestic and international synthesis tricaprylate method of 2,2'-ethylenedioxybis(ethanol). two is broadly divided into two steps is carried out:The first step is the three of a molecule
The isooctyl acid of glycol and a molecule sloughs a molecular water under catalyst action, generates 2,2'-ethylenedioxybis(ethanol). list tricaprylate;And then enter
Row second step reacts, and a molecule 2,2'-ethylenedioxybis(ethanol). list tricaprylate and a molecule isooctyl acid slough again a molecule under catalyst action
Water, generates the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two.Reaction influence factor includes that catalyst type, response time, reaction temperature and three are sweet
Alcohol and isooctyl acid ratio etc., are typically to be esterified dehydration.
The major technique for producing the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two in the market is distinguished in the selection of catalyst, a part of factory
, with phosphoric acid mixed liquor as catalyst, a part of producer's selection solid acid or active hargil are used as catalysis for family's selection sulphuric acid
Agent, different catalysts affect very big on reaction, and existing catalyst system and catalyzing all has that low production efficiency, product purity are low.
The content of the invention
The present invention is to avoid the weak point existing for above-mentioned prior art, there is provided a kind of tricaprylate of 2,2'-ethylenedioxybis(ethanol). two
Production method, it is intended to new catalyst system and catalyzing, reach the purpose of improve production efficiency and product purity.
The present invention is adopted the following technical scheme that to solve technical problem:
The production method of the tricaprylate of 2,2'-ethylenedioxybis(ethanol). of the present invention two, its feature is:With isooctyl acid, 2,2'-ethylenedioxybis(ethanol). as raw material,
Sending in stirred autoclave under catalyst action carries out negative pressure, low-temp reaction;After reaction terminates, slightly mistake is carried out to gained reactant liquor
Filter, then will carry out taking off light in the de- light kettle of filtrate feeding, the tricaprylate crude product of 2,2'-ethylenedioxybis(ethanol). two is obtained;Finally crude product is neutralized,
Washing, dehydration, essence are filtered, that is, obtain the tricaprylate finished product of 2,2'-ethylenedioxybis(ethanol). two of water white transparency oily;
The catalyst is made up of major catalyst and promoter, the major catalyst be stannous chloride, the co-catalysis
Agent is made up of titanium dioxide with activated carbon;
Wherein:The mass ratio of 2,2'-ethylenedioxybis(ethanol)., isooctyl acid and stannous chloride is 1:2.2~2.4:0.3~0.5;The co-catalysis
Agent quality accounts for the 0.1%~0.5% of raw material gross mass.Titanium dioxide and the mass ratio of activated carbon are 1 in the promoter:1.
Specifically:
The material in reactor temperature is 65 DEG C~90 DEG C, and reactor pressure is 20KPa~60KPa, and the response time is 2
~4 hours.
The coarse filtration is to be removed solid particle filter pressing in reactant liquor using filter press.
Will filtrate send into take off carry out in light kettle de- light temperature be 150 DEG C~180 DEG C, pressure be 6KPa~10KPa.
The neutralization is to produce hydrochloric acid to stannous chloride hydrolysis to be neutralized, and it can be mass concentration to neutralize the reagent for using
Sodium hydroxide solution, or mass concentration for 5% is 5% potassium hydroxide solution, and preferred mass concentration is 5% hydrogen
Sodium hydroxide solution carries out Deca neutralization.
The washing be to wash away neutralization after ion in solution.
The method of the dehydration is:First stratification, then the tricaprylate of the oil reservoir 2,2'-ethylenedioxybis(ethanol). two employing decompression steaming to obtaining
Evaporate mode eliminating water;The pressure of the vacuum distillation is 30KPa~50Kpa, temperature is 110 DEG C~130 DEG C.
The essence is filtered to be filtered using quintessence oil plate oil-filter, filtering accuracy≤1~3 micron that essence is filtered.Essence
Purity >=99.5% of the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two is obtained after filtration.
Compared with existing technology, the beneficial effects are mainly as follows:
1st, the present invention produces the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two using novel catalyst system, can effectively suppress sending out for side reaction
It is raw, the generation of impurity is reduced, effectively improve the purity of product.
2nd, adopt negative pressure, low-temp reaction, the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two to be easy to produce in the present invention, production effect can be improved
Rate.
3rd, follow-up precision processing is carried out to the tricaprylate of esterification products 2,2'-ethylenedioxybis(ethanol). two in the present invention, makes the purity of product higher.
Specific embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following enforcements
Example.
Embodiment 1
The present embodiment produces as follows the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two:
2,2'-ethylenedioxybis(ethanol). 100Kg, isooctyl acid 220Kg, catalyst stannous chloride 30Kg, promoter titanium dioxide are weighed with activity
The common 0.5Kg of charcoal, adds reactor, starts reactor agitator, and reactor reaction pressure is evacuated to into 50KPa, then uses steam
Material is warming up to into 85 DEG C, after flowing back occurs in reactor, slows down programming rate, what is maintained the reflux for stablizes, esterification 4h.
After reaction terminates, reactant liquor is proceeded to into cooling coarse filtration groove, be cooled to carry out plate and frame filtration when less than 40 DEG C, with
Afterwards the filtrate collection for filtering is sent into into de- light component kettle, under the conditions of 6KPa, 150 DEG C, with steam heating excess in filtrate is steamed
Isooctyl acid, obtains the tricaprylate crude product of 2,2'-ethylenedioxybis(ethanol). two;Carried out being slowly added dropwise in neutralization crude product excessively with the aqueous slkali of 5% sodium hydroxide
Acid, then washed, water layer is released after stratification, oil reservoir is subtracted under the conditions of pressure is 50KPa, 130 DEG C of temperature
Pressure distillation dehydration, cooling is filtrated to get the tricaprylate finished product of water white transparency oily 2,2'-ethylenedioxybis(ethanol). two using quintessence oil plate oil-filter, surveys
It is 99.8% to obtain its purity.
Embodiment 2
The present embodiment produces as follows the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two:
2,2'-ethylenedioxybis(ethanol). 100Kg, isooctyl acid 240Kg, catalyst stannous chloride 40Kg, promoter titanium dioxide are weighed with activity
The common 0.7Kg of charcoal, adds reactor, starts reactor agitator, and reactor reaction pressure is evacuated to into 30KPa, then uses steam
Material is warming up to into 75 DEG C, after flowing back occurs in reactor, slows down programming rate, what is maintained the reflux for stablizes, esterification 3h.
After reaction terminates, reactant liquor is proceeded to into cooling coarse filtration groove, be cooled to carry out plate and frame filtration when less than 40 DEG C, with
Afterwards the filtrate collection for filtering is sent into into de- light component kettle, under the conditions of 8KPa, 160 DEG C, with steam heating excess in filtrate is steamed
Isooctyl acid, obtains the tricaprylate crude product of 2,2'-ethylenedioxybis(ethanol). two;Carried out being slowly added dropwise in neutralization crude product excessively with the aqueous slkali of 5% sodium hydroxide
Acid, then washed, water layer is released after stratification, oil reservoir is subtracted under the conditions of pressure is 30KPa, 110 DEG C of temperature
Pressure distillation dehydration, cooling is filtrated to get the tricaprylate finished product of water white transparency oily 2,2'-ethylenedioxybis(ethanol). two using quintessence oil plate oil-filter, surveys
It is 99.5% to obtain its purity.
Embodiment 3
The present embodiment produces as follows the tricaprylate of 2,2'-ethylenedioxybis(ethanol). two:
2,2'-ethylenedioxybis(ethanol). 100Kg, isooctyl acid 220Kg, catalyst stannous chloride 35Kg, promoter titanium dioxide are weighed with activity
The common 0.5Kg of charcoal, adds reactor, starts reactor agitator, and reactor reaction pressure is evacuated to into 40KPa, then uses steam
Material is warming up to into 80 DEG C, after flowing back occurs in reactor, slows down programming rate, what is maintained the reflux for stablizes, esterification 3h.
After reaction terminates, reactant liquor is proceeded to into cooling coarse filtration groove, be cooled to carry out plate and frame filtration when less than 40 DEG C, with
Afterwards the filtrate collection for filtering is sent into into de- light component kettle, under the conditions of 10KPa, 180 DEG C, with steam heating excess in filtrate is steamed
Isooctyl acid, obtains the tricaprylate crude product of 2,2'-ethylenedioxybis(ethanol). two;Carried out being slowly added dropwise in neutralization crude product excessively with the aqueous slkali of 5% sodium hydroxide
Acid, then washed, water layer is released after stratification, to oil reservoir pressure be 40KPa, temperature be to carry out under the conditions of 120 DEG C
Decompression dehydration, cooling, using quintessence oil plate oil-filter the tricaprylate finished product of water white transparency oily 2,2'-ethylenedioxybis(ethanol). two is filtrated to get, and is measured
Its purity is 99.7%.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. the production method of the tricaprylate of a kind of 2,2'-ethylenedioxybis(ethanol). two, it is characterised in that:With isooctyl acid, 2,2'-ethylenedioxybis(ethanol). as raw material, in catalysis
The lower feeding in stirred autoclave of agent effect carries out negative pressure, low-temp reaction;After reaction terminates, coarse filtration is carried out to gained reactant liquor,
Filtrate is sent into again take off and carry out in light kettle de- light, the tricaprylate crude product of 2,2'-ethylenedioxybis(ethanol). two is obtained;Finally crude product is neutralized, water
Wash, be dehydrated, essence is filtered, that is, obtain the tricaprylate finished product of 2,2'-ethylenedioxybis(ethanol). two of water white transparency oily;
The catalyst is made up of major catalyst and promoter, the major catalyst be stannous chloride, the promoter by
Titanium dioxide is constituted with activated carbon;
Wherein:The mass ratio of 2,2'-ethylenedioxybis(ethanol)., isooctyl acid and stannous chloride is 1:2.2~2.4:0.3~0.5;The promoter matter
Amount accounts for the 0.1%~0.5% of raw material gross mass.
2. production method according to claim 1, it is characterised in that:Titanium dioxide and activated carbon in the promoter
Mass ratio is 1:1.
3. production method according to claim 1, it is characterised in that:The material in reactor temperature is 65 DEG C~90
DEG C, reactor pressure is 20KPa~60KPa, and the response time is 2~4 hours.
4. production method according to claim 1, it is characterised in that:The coarse filtration will be reacted using filter press
Filtering residue filter pressing in liquid is removed.
5. production method according to claim 1, it is characterised in that:Filtrate is sent into take off and carry out in light kettle de- light temperature
It is 6KPa~10KPa for 150 DEG C~180 DEG C, pressure.
6. production method according to claim 1, it is characterised in that:The used reagent of the neutralization is mass concentration
5% sodium hydroxide solution or the potassium hydroxide solution of mass concentration 5%.
7. production method according to claim 1, it is characterised in that:The washing be to wash away neutralization after in solution from
Son.
8. production method according to claim 1, it is characterised in that:The method of the dehydration is:First stratification, then it is right
The oil reservoir for obtaining adopts vacuum distillation mode eliminating water;The pressure of the vacuum distillation be 30KPa~50Kpa, temperature be 110 DEG C~
130℃。
9. production method according to claim 1, it is characterised in that:The essence is filtered to be entered using quintessence oil plate oil-filter
Row is filtered, filtering accuracy≤1~3 micron that essence is filtered.
10. production method according to claim 1, it is characterised in that:Essence filters the obtained tricaprylate of 2,2'-ethylenedioxybis(ethanol). two
Purity >=99.5%.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611220377.3A CN106674007A (en) | 2016-12-26 | 2016-12-26 | Production method of triethylene glycol di-2-ethylhexoate |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201611220377.3A CN106674007A (en) | 2016-12-26 | 2016-12-26 | Production method of triethylene glycol di-2-ethylhexoate |
Publications (1)
Publication Number | Publication Date |
---|---|
CN106674007A true CN106674007A (en) | 2017-05-17 |
Family
ID=58870463
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201611220377.3A Pending CN106674007A (en) | 2016-12-26 | 2016-12-26 | Production method of triethylene glycol di-2-ethylhexoate |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106674007A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111393294A (en) * | 2020-04-13 | 2020-07-10 | 盘锦洪鼎化工有限公司 | Method for refining triethylene glycol diisocaprylate rectifying still residual liquid |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102108050A (en) * | 2010-12-17 | 2011-06-29 | 上海博康精细化工有限公司 | Synthesis method of diphenylcarbinol decanoate |
CN104529760A (en) * | 2014-12-03 | 2015-04-22 | 营口天元化工研究所股份有限公司 | Preparation method of triethylene glycol di-2-ethylhexoate |
-
2016
- 2016-12-26 CN CN201611220377.3A patent/CN106674007A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102108050A (en) * | 2010-12-17 | 2011-06-29 | 上海博康精细化工有限公司 | Synthesis method of diphenylcarbinol decanoate |
CN104529760A (en) * | 2014-12-03 | 2015-04-22 | 营口天元化工研究所股份有限公司 | Preparation method of triethylene glycol di-2-ethylhexoate |
Non-Patent Citations (3)
Title |
---|
牛梅菊: "氯化亚锡催化剂在酯化反应中的应用", 《化学与粘合》 * |
牛梅菊等: "无水氯化亚锡催化合成苯甲酸乙酯", 《聊城师院学报(自然科学版)》 * |
高燕萍: "氯化亚锡催化合成肉桂酸环己酯的研究", 《化工时刊》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111393294A (en) * | 2020-04-13 | 2020-07-10 | 盘锦洪鼎化工有限公司 | Method for refining triethylene glycol diisocaprylate rectifying still residual liquid |
CN111393294B (en) * | 2020-04-13 | 2022-09-02 | 盘锦洪鼎化工有限公司 | Method for refining triethylene glycol diisocaprylate rectifying still residual liquid |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP2732921B2 (en) | Method for producing polyglycerin | |
CN109485568B (en) | Preparation method of high-optical indoxacarb intermediate | |
CN101058526A (en) | Method of increasing quality of glycol | |
CN100395243C (en) | Improved systhesizing process for dicyclohexyl-18-crown-6 | |
CN108997419A (en) | A method of palladium (0) or platinum (0) complex chemical compound are prepared using triphenylphosphine | |
CN108129316A (en) | A kind of nylon acid two(2- ethyls)The preparation method of own ester | |
CN101289395B (en) | Method for preparing methyl ethyl carbonate | |
CN102875332B (en) | Process for synthesizing 3-hexyne-2,5-diol through slurry bed based on low pressure method | |
CN106674007A (en) | Production method of triethylene glycol di-2-ethylhexoate | |
CN102417445B (en) | Method for synthesizing succinic acid from maleic acid | |
CN110713439A (en) | Preparation method of cyclohexane-1, 2-dicarboxylate environment-friendly plasticizer | |
CN107501212B (en) | Synthetic method of 3-hydroxymethyl tetrahydrofuran | |
CN111187152A (en) | Method for synthesizing pseudo ionone under catalysis of alkaline immobilized ionic liquid | |
CN104650013B (en) | A kind of high selective (S)-beta-hydroxy-gamma-butyrolactone simple and convenient process for preparing | |
CN106928057B (en) | Method for synthesizing maleic acid di (2-ethylhexyl) ester | |
CN101092360B (en) | Method for catalyzing and synthesizing tri-butyl citrate from methylal naphthalene sulfonic acid | |
CN105860052A (en) | Method for improving colors of polyether polyol | |
CN103702987B (en) | The manufacture method of alkyl diol list glycidyl ether | |
CN112495360B (en) | Solid composite catalyst for continuously preparing 3-hydroxybutyraldehyde, and preparation method and application thereof | |
CN1225919A (en) | Synthesizing method for dimethyl ester of mixed acid of butane diacid, glutaric acid and hexane diacid | |
CN114409574A (en) | Preparation method of allyl benzenesulfonate | |
CN1528799A (en) | Improved polyvinyl alcohol-beta-cyanoethyl ether preparing method | |
CN110776419A (en) | Green and clean production process for preparing dibutyl phthalate | |
CN111704527B (en) | Method and device system for producing 1, 2-hexanediol | |
CN105061143B (en) | The technique that slurry bed acidity Control method synthesizes 3 hexin 2,5 glycol |
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 | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170517 |