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A method for preparing bis(2-propylheptyl) phthalate

A technology of diphthalate and phthalic acid, which is applied in the field of preparation of bis(2-propylheptyl)phthalate, and can solve problems such as large environmental pollution, poor safety, and catalyst corrosion

Active Publication Date: 2016-08-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the serious problems of severe catalyst corrosion, heavy environmental pollution, and use of phthalic anhydride as raw material in the current DPHP preparation process, the raw material consumption, high energy consumption and poor safety of the phthalic anhydride preparation process, the purpose of the invention is to develop a phthalic anhydride The method for preparing DPHP from formic acid has outstanding advantages such as mild reaction conditions, simple and convenient operation, etc.

Method used

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  • A method for preparing bis(2-propylheptyl) phthalate
  • A method for preparing bis(2-propylheptyl) phthalate
  • A method for preparing bis(2-propylheptyl) phthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 16.6 grams of phthalic acid (0.1mol), 33.2 grams of 2-propylheptanol (2-PH, 0.21mol), 8.3 grams of xylene and 0.332 grams of carbon sulfonic acid into 100ml of two-port round bottom equipped with a water separator In the flask, fill the water separator with toluene and connect the condenser, stir evenly, heat up to 140°C and react for 6 hours; distill and recover xylene and excess 2-propylheptanol; take 2ml of the residual liquid after distillation, and use 0.05mol / l NaOH solution titration; the calculated esterification rate of phthalic acid is 99%. The product was qualitatively analyzed by gas chromatography-mass spectrometry.

Embodiment 2～14

[0016] The specific method of Examples 2-14 is similar to that of Example 1, and the specific reaction conditions and results are shown in Table 1.

Embodiment 15

[0018] Add 16.6 grams of phthalic acid (0.1mol) and 39.6 grams of 2-propylheptanol (2-PH, 0.25mol) into a 100ml two-necked round-bottomed flask equipped with a water separator, which is filled with 2- Propyl heptanol was connected to the condenser, stirred evenly, and heated to 230°C for 6 hours; excess 2-propyl heptanol was recovered by distillation; 2ml of residual liquid after distillation was titrated with 0.05mol / l NaOH solution; The esterification rate of phthalic acid is 99%. The product was qualitatively analyzed by gas chromatography-mass spectrometry.

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Abstract

The invention relates to a method for preparation of phthalate di(2-propyl heptyl) ester(DPHP). Phthalic acid and 2-propylheptanol as raw materials are used for preparation of the DPHP, and the reaction is performed in the following two ways: (1) using toluene, xylene or a toluene and xylene mixture as a water-carrying agent, using one or more substance of char sulfonic acid, SO3H functionalized ionic liquid, sulfonic acid resin, phenylsulfonic acid, naphthalene sulfonic acid, trifluoromethanesulfonic acid, phosphotungstic heteropoly acid, heterpoly tungstosilicate, phospho-molybdic heteropolyacid, SO4<2-> / MxOy or S2O8<2-> / MxOy solid super acid as a catalyst, reacting for 2 to 6 hours at 110 to 140 DEG C; and (2) reacting for 4 to 6 hours at 220 to 240 DEG C without external addition of the water carrying agent and the catalyst. By the two ways, the esterification rates of the phthalic acid both can reach above 99% to the highest degree. The method has the advantages of mild reaction conditions, and simple and convenient operation, and the like.

Description

technical field [0001] The invention relates to a method for preparing bis(2-propylheptyl) phthalate. Background technique [0002] Plasticizers must be used in the production of high molecular polymers such as plastics and rubber to weaken the intermolecular forces of polymers, increase the mobility of molecular chains, and reduce the crystallinity of molecular chains, thereby improving the plasticity, flexibility, and tension of polymers. The purpose of extensibility and processability. At present, dioctyl phthalate (DOP) is mainly used as plasticizer in China. Due to the great harm to the human body and the environment, in the United States and other developed countries, the production and use of DOP has been restricted, and has been replaced by new high-end plasticizers such as bis(2-propylheptyl) phthalate (DPHP) . DPHP is safe and non-toxic, has excellent comprehensive performance, good compatibility with plastics, and is not easy to precipitate. The surface of term...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/80C07C67/08
CPCC07C67/08C07C69/80
Inventor 黄义争徐杰高进苗虹孙颖
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI