CN104592020A - Preparation method of rubber plasticizer dioctyl adipate - Google Patents
Preparation method of rubber plasticizer dioctyl adipate Download PDFInfo
- Publication number
- CN104592020A CN104592020A CN201310525489.XA CN201310525489A CN104592020A CN 104592020 A CN104592020 A CN 104592020A CN 201310525489 A CN201310525489 A CN 201310525489A CN 104592020 A CN104592020 A CN 104592020A
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- CN
- China
- Prior art keywords
- preparation
- octanol
- dioctyl adipate
- reaction
- catalyst
- 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.)
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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- 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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/40—Substitution reactions at carbon centres, e.g. C-C or C-X, i.e. carbon-hetero atom, cross-coupling, C-H activation or ring-opening reactions
- B01J2231/49—Esterification or transesterification
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- 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)
Abstract
The invention discloses a preparation method of a rubber plasticizer dioctyl adipate. The method includes the following steps: 1, adding adipic acid and octanol into a four-neck flask equipped with a stirrer, a thermometer, a water separator and a reflux condensing tube, heating while stirring the solid until complete dissolution, adding a solid superacid resin catalyst, and conducting reflux reaction for 140 min; and 2, after the reaction, cooling and separating the catalyst and an ester layer, conducting reduced pressure distillation to recycle the excessive amount of octanol and cyclohexane, washing the remaining reaction liquid with saturated NaHCO3 and brine, conducting reduced pressure distillation on an oil layer, and collecting fraction to obtain colorless and transparent dioctyl adipate liquid. The preparation method provided by the invention employs a novel solid superacid resin to substitute concentrated sulfuric acid as the catalyst in the synthesis of dioctyl adipate, and the solid superacid resin has the advantages of high esterification rate, good selectivity, easy separation from the product, repeated use, simple posttreatment, no corrosion to equipment, no environmental pollution, green and environment-friendliness.
Description
Technical field
The present invention relates to a kind of preparation method of rubber plastizing agent, be specifically related to a kind of preparation method of Octyl adipate.
Background technology
Octyl adipate is a kind of cold-resistant plasticizer, can improve low-temperature pliability and the shock-resistance of polymkeric substance, be widely used in the softening agent of agricultural film, leatheroid, Frozen Food Packaging, synthetic rubber etc.By hexanodioic acid and n-Octanol, direct esterification under acid catalysis obtains usual Octyl adipate, current is catalyzer mainly with the vitriol oil and tosic acid, but this technique exists the problems such as poor product quality, serious to equipment corrosion, side reaction is many, aftertreatment is complicated, environmental pollution is serious.
Summary of the invention
The object of the invention is to, a kind of preparation method of rubber plastizing agent Octyl adipate is provided, replace the vitriol oil to do catalyzer synthesizing adipic acid dioctyl ester with novel solid super-strong acid resin, esterification yield is high, and selectivity is good, easily separated with product, can repeatedly use, aftertreatment is simple, not etching apparatus, free from environmental pollution, environmental protection.
The preparation method of described rubber plastizing agent Octyl adipate, it comprises the following steps:
One, hexanodioic acid, octanol are added in the four-hole boiling flask with agitator, thermometer, water trap, reflux condensing tube, be heated with stirring to solid and dissolve completely, add superpower solid acid resin catalyst, carry out back flow reaction 140min;
Two, reaction terminates, and cool and isolate catalyzer and ester layer, excessive octanol and hexanaphthene are reclaimed in underpressure distillation, residual reaction liquid saturated sodium bicarbonate and salt water washing, and oil reservoir carries out underpressure distillation, collects cut, obtains water white transparency Octyl adipate liquid.
The preparation method of rubber plastizing agent Octyl adipate provided by the invention, its beneficial effect is, replace the vitriol oil to do catalyzer synthesizing adipic acid dioctyl ester with novel solid super-strong acid resin, esterification yield is high, and selectivity is good, easily separated with product, can repeatedly use, aftertreatment is simple, not etching apparatus, free from environmental pollution, environmental protection.
Embodiment
Below in conjunction with an embodiment, the preparation method of rubber plastizing agent Octyl adipate provided by the invention is described in detail.
Embodiment
One, hexanodioic acid, octanol are added in the four-hole boiling flask with agitator, thermometer, water trap, reflux condensing tube, be heated with stirring to solid and dissolve completely, add superpower solid acid resin catalyst, carry out back flow reaction 140min;
Two, reaction terminates, and cool and isolate catalyzer and ester layer, excessive octanol and hexanaphthene are reclaimed in underpressure distillation, residual reaction liquid saturated sodium bicarbonate and salt water washing, and oil reservoir carries out underpressure distillation, collects cut, obtains water white transparency Octyl adipate liquid.
Claims (1)
1. a preparation method for rubber plastizing agent Octyl adipate, is characterized in that: it comprises the following steps:
One, hexanodioic acid, octanol are added in the four-hole boiling flask with agitator, thermometer, water trap, reflux condensing tube, be heated with stirring to solid and dissolve completely, add superpower solid acid resin catalyst, carry out back flow reaction 140min;
Two, reaction terminates, and cool and isolate catalyzer and ester layer, excessive octanol and hexanaphthene are reclaimed in underpressure distillation, residual reaction liquid saturated sodium bicarbonate and salt water washing, and oil reservoir carries out underpressure distillation, collects cut, obtains water white transparency Octyl adipate liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525489.XA CN104592020A (en) | 2013-10-31 | 2013-10-31 | Preparation method of rubber plasticizer dioctyl adipate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525489.XA CN104592020A (en) | 2013-10-31 | 2013-10-31 | Preparation method of rubber plasticizer dioctyl adipate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104592020A true CN104592020A (en) | 2015-05-06 |
Family
ID=53118128
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310525489.XA Pending CN104592020A (en) | 2013-10-31 | 2013-10-31 | Preparation method of rubber plasticizer dioctyl adipate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104592020A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966906A (en) * | 2017-05-19 | 2017-07-21 | 佛山市高明晟俊塑料助剂有限公司 | A kind of preparation method of dioctyl adipate |
-
2013
- 2013-10-31 CN CN201310525489.XA patent/CN104592020A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966906A (en) * | 2017-05-19 | 2017-07-21 | 佛山市高明晟俊塑料助剂有限公司 | A kind of preparation method of dioctyl adipate |
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Legal Events
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150506 |