CN103664617A - New production process for diethylene glycol dibenzoate - Google Patents
New production process for diethylene glycol dibenzoate Download PDFInfo
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- CN103664617A CN103664617A CN201310608079.1A CN201310608079A CN103664617A CN 103664617 A CN103664617 A CN 103664617A CN 201310608079 A CN201310608079 A CN 201310608079A CN 103664617 A CN103664617 A CN 103664617A
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- Prior art keywords
- diethylene glycol
- glycol dibenzoate
- production process
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- new production
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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
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a new production process for diethylene glycol dibenzoate. The new production process comprises the following steps: taking and pouring benzoic acid and diethylene glycol into a reactor at the molar ratio of (1.2-1.4):1, stirring while raising the temperature; adding a compound non-acid catalyst, and performing heat preservation to achieve complete reaction; adding butanol into the product of the reaction to allow the benzoic acid in the raw materials to fully react so as to obtain a crude product of the diethylene glycol dibenzoate; allowing the crude product to be subjected to water washing, dealcoholization, bleaching and pressure filtration so as to obtain the diethylene glycol dibenzoate. The new production process improves the production processing safety for eliminating the toluene, reduces the energy consumption, not only ensures shortened esterification reaction time, but also saves a great amount of alkali materials and water for washing due to the compound non-acid catalyst, and meets the environment-friendly and energy-saving requirements. Moreover, the equipment is not easy to corrode.
Description
Technical field
The invention belongs to vitochemical technical field, more specifically relate to a kind of synthesis technique of ester compound.
Background technology:
Diethylene glycol dibenzoate is the various kinds of resin softening agent such as polyvinyl chloride, polyvinyl acetate (PVA), it is good that it has solvability, consistency is good, volatilize low, the features such as oil resistant, water-fast, fast light, stain resistance is good, are applicable to process polyvinyl chloride (PVC) flooring material, plastipaste, polyester acetoacetic ester tackiness agent and synthetic rubber etc.
In current existing art production process, conventionally adopt toluene as band aqua, and toluene is Class A dangerization product, using and storing of it all has danger significantly; In addition, the synthetic basic principles of chemistry of diethylene glycol dibenzoate are esterifications, esterification generally need to could complete smoothly under the existence of catalyzer, in existing technique, mostly use sulfuric acid as catalyzer, sulfuric acid is efficient as the advantage of catalyzer, but also there is serious problem: the one, sulfuric acid can severe corrosion equipment, the 2nd, can bring a large amount of in and waste water, be unfavorable for environmental protection and energy saving.
Summary of the invention:
For above-mentioned deficiency, the object of the invention is to provide a kind of safer and new production process of the diethylene glycol dibenzoate of environmental protection and energy saving more.
To achieve these goals, processing step of the present invention is:
(1), by benzene raw materials formic acid: the mol ratio of glycol ether is that 1.2-1.4:1 gets, benzene feedstock formic acid and glycol ether are dropped in reactor to warming while stirring;
(2) add compound non-catalysis with acid agent, insulation, carries out completely reaction; The mixture that described compound non-catalysis with acid agent is tetrabutyl titanate and tetracol phenixin, wherein the add-on of tetrabutyl titanate is the 1.5%-1.7% of reaction raw materials total mass, tetracol phenixin enter the 0.7%-0.9% that amount is reaction raw materials total mass;
(3) to adding mass percent in reacted product, be the butanols of 0.1-0.4%, make the phenylformic acid complete reaction in raw material, obtain the thick product of diethylene glycol dibenzoate;
(4) the thick product of diethylene glycol dibenzoate is washed, dealcoholysis, decolouring, press filtration obtain diethylene glycol dibenzoate.
Current original technical recipe is phenylformic acid: the mol ratio of glycol ether is 1:1; in adding catalyst reaction process, add again toluene as band aqua; but toluene is Class A dangerization product; it uses and stores all more dangerous; therefore, in the present invention, phenylformic acid: the mol ratio of glycol ether is improved to 1.2-1.4:1; later stage in reaction adds butanols that unreacted benzoic acid is complete, the use of so just having omitted toluene.
Beneficial effect:
(1) the present invention has adjusted the ratio of phenylformic acid and glycol ether in original technique, strengthened benzoic usage quantity, later stage in reaction adds butanols, the benzoic acid that unreacted is complete is complete, cancelled the use of Class A dangerization product toluene in original technique, improve the security in production process, also saved energy consumption simultaneously;
(2) catalyzer that the present invention uses is compound non-catalysis with acid agent, replace an acidic catalyst using in original technique, can not only guarantee to shorten the reaction times of esterification, and saved a large amount of washing soda materials and water, also be not easy etching apparatus, the requirement that composite environmental-friendly is energy-conservation.
Embodiment:
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
Get 146.4 kilograms, phenylformic acid, 106 kilograms of glycol ethers, put into reactor, warming while stirring, is warming up to 190-210 ℃, adds compound non-catalysis with acid agent: tetrabutyl titanate and tetracol phenixin, tetrabutyl titanate quality is 3.79 kilograms, tetracol phenixin quality is 1.78 kilograms, is incubated 8 hours, and reaction is carried out completely; To the butanols that adds 0.26 kilogram in reaction product, the benzoic acid that unreacted in reaction product is complete is complete, obtain the thick product of diethylene glycol dibenzoate; By the thick product of diethylene glycol dibenzoate wash, dealcoholysis, decolouring, press filtration obtain diethylene glycol dibenzoate.
Embodiment 2:
Get 170.8 kilograms, phenylformic acid, 106 kilograms of glycol ethers, put into reactor, warming while stirring, is warming up to 180-200 ℃, adds compound non-catalysis with acid agent: tetrabutyl titanate and tetracol phenixin, tetrabutyl titanate quality is 4.71 kilograms, tetracol phenixin quality is 2.22 kilograms, is incubated 6 hours, and reaction is carried out completely; To the butanols that adds 0.53 kilogram in reaction product, the benzoic acid that unreacted in reaction product is complete is complete, obtain the thick product of diethylene glycol dibenzoate; By the thick product of diethylene glycol dibenzoate wash, dealcoholysis, decolouring, press filtration obtain diethylene glycol dibenzoate.
Claims (1)
1. a new production process for diethylene glycol dibenzoate, is characterized in that: processing step is,
(1), by benzene raw materials formic acid: the mol ratio of glycol ether is that 1.2-1.4:1 gets, benzene feedstock formic acid and glycol ether are dropped in reactor to warming while stirring;
(2) add compound non-catalysis with acid agent, insulation, carries out completely reaction; The mixture that described compound non-catalysis with acid agent is tetrabutyl titanate and tetracol phenixin, wherein the add-on of tetrabutyl titanate is the 1.5%-1.7% of reaction raw materials total mass, tetracol phenixin enter the 0.7%-0.9% that amount is reaction raw materials total mass;
(3) to adding mass percent in reacted product, be the butanols of 0.1-0.4%, make the phenylformic acid complete reaction in raw material, obtain the thick product of diethylene glycol dibenzoate;
(4) the thick product of diethylene glycol dibenzoate is washed, dealcoholysis, decolouring, press filtration obtain diethylene glycol dibenzoate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310608079.1A CN103664617A (en) | 2013-11-27 | 2013-11-27 | New production process for diethylene glycol dibenzoate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310608079.1A CN103664617A (en) | 2013-11-27 | 2013-11-27 | New production process for diethylene glycol dibenzoate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103664617A true CN103664617A (en) | 2014-03-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310608079.1A Pending CN103664617A (en) | 2013-11-27 | 2013-11-27 | New production process for diethylene glycol dibenzoate |
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| CN (1) | CN103664617A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776316A (en) * | 2019-03-06 | 2019-05-21 | 杭州多向流化学科技有限公司 | A kind of production method of environment-friendly plasticizer dibenzoic diglycol laurate |
| CN114085144A (en) * | 2021-12-09 | 2022-02-25 | 上海汇得科技股份有限公司 | Method for synthesizing plasticizer |
-
2013
- 2013-11-27 CN CN201310608079.1A patent/CN103664617A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776316A (en) * | 2019-03-06 | 2019-05-21 | 杭州多向流化学科技有限公司 | A kind of production method of environment-friendly plasticizer dibenzoic diglycol laurate |
| CN114085144A (en) * | 2021-12-09 | 2022-02-25 | 上海汇得科技股份有限公司 | Method for synthesizing plasticizer |
| CN114085144B (en) * | 2021-12-09 | 2023-12-29 | 上海汇得科技股份有限公司 | Synthetic method of plasticizer |
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Application publication date: 20140326 |
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