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Synthetic method of dipropylene glycol dibenzoate

A technology of dipropylene glycol dibenzoate and synthesis method, which is applied in the direction of carboxylate preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of using volatile solvents, slow reaction speed, high production cost, etc. Achieve the effect of reducing color number, short production cycle and small color number

Pending Publication Date: 2017-04-19
HUBEI GREENHOME MATERIALS TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of synthetic method of dipropylene glycol dibenzoate, has solved the low utilization rate of existing synthetic method, high production cost, slow reaction speed, long reaction time, use of volatile solvent, bigger environmental pollution and other technical issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Under the condition of nitrogen as the water-carrying agent, 134 parts (1 kg each, the same below) of dipropylene glycol, 243 parts of benzoic acid, 0.25 part of stannous oxalate, and 0.5 part of basic zirconium carbonate were added to the reaction kettle. Raise the temperature, start stirring after the material melts, control the temperature at 230-235°C, and continue to keep warm for 6 hours; cool down to 85°C, slowly add 10 parts of hydrogen peroxide into the reaction kettle, keep warm for 30min, then raise the temperature to 115°C, and keep warm at this temperature 15 minutes; cool down to 90°C, add 60 parts of 5% sodium carbonate solution and 50 parts of soft water, and stir for 30 minutes. During the process, you can add lye or soft water to adjust the pH of the system to about 9, otherwise it will not be easy to stratify; stand still Separated, drained phase; washed with 50 parts of soft water, the lower oil phase was dehydrated by vacuum distillation at 120°C to ...

Embodiment 2

[0019] Under the condition of nitrogen as the water-carrying agent, 134 parts of dipropylene glycol, 243 parts of benzoic acid, 0.5 part of stannous oxalate, and 0.5 part of basic zirconium carbonate were added to the reaction kettle. Raise the temperature, start stirring after the material melts, control the temperature at 230-235°C, and continue to keep warm for 6 hours; cool down to 85°C, slowly add 10 parts of hydrogen peroxide into the reaction kettle, keep warm for 30min, then raise the temperature to 115°C, and keep warm at this temperature 15 minutes; cool down to 90°C, add 60 parts of 5% sodium carbonate solution and 50 parts of soft water, and stir for 30 minutes. During the process, you can add lye or soft water to adjust the pH of the system to about 9, otherwise it will not be easy to stratify; stand still Separate the layers, drain the phase; wash with 50 parts of soft water, and dehydrate the lower oil phase at 120°C to obtain 320 parts of the finished product, t...

Embodiment 3

[0021] Under the condition of nitrogen as the water-carrying agent, 134 parts of dipropylene glycol, 243 parts of benzoic acid, 0.5 part of stannous oxalate, and 1.0 part of basic zirconium carbonate were added to the reaction kettle. Raise the temperature, start stirring after the material melts, control the temperature at 180-210°C, and continue to keep warm for 7 hours; cool down to 86-87°C, slowly add 12 parts of hydrogen peroxide into the reaction kettle, heat it up to 116°C after 38 minutes of heat preservation, and keep it at this temperature Keep warm for 18 minutes; cool down to 90°C, add 65 parts of 5% sodium carbonate solution and 50 parts of soft water, and stir for 30 minutes. During the process, add lye or soft water to adjust the pH of the system to about 9, otherwise it will not be easy to stratify; Stand to separate and separate, drain the phase; add 50 parts of soft water to wash, and the lower oil phase is dehydrated by vacuum distillation at 125°C to obtain ...

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PUM

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Abstract

A method for preparation of dipropylene glycol dibenzoate is disclosed. According to the method, a synthetic route of esterification-decoloration-washing-dehydration is adopted. benzoic acid and dipropylene glycol are used as raw materials; a stannous oxalate and basic zirconium carbonate binary complex catalyst is used; and an excessive amount of dipropylene glycol and nitrogen are used as a water carrying agent to reasonably control the temperature. Through decoloration, neutralization, washing and dehydration, the finished product dipropylene glycol dibenzoate is prepared. The synthetic method of the invention has advantages of simple process, short production period, high yield of the product, small colour number, etc. By the method, it is easy to realize industrialization.

Description

technical field [0001] The invention belongs to the field of dipropylene glycol dibenzoate production, in particular to a synthesis method of dipropylene glycol dibenzoate. Background technique [0002] As a plasticizer, dipropylene glycol dibenzoate (DPGDB) not only has the general properties of plasticizers, but also has its own characteristics: compatibility, antistatic, anti-staining and anti-volatility are remarkable. Widely used in polyurethane printing rubber rollers, coating rollers, printing seals and other plastic pressed products, as well as additives for synthetic leather, potting and packaging materials, etc., can make the products have ideal performance. In addition, it is also widely used in thermosetting plastics, coatings, rubber products, fillers, adhesives, etc., and the market demand is more urgent. [0003] The synthesis of dipropylene glycol dibenzoate (DPGDB) can be divided into esterification, transesterification and acid chloride condensation. At p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/78
CPCC07C67/08C07C69/78
Inventor 李鹏肖华青杨华
Owner HUBEI GREENHOME MATERIALS TECH INC
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