Method for preparing oleoyl tributyl citrate plasticizer

A technology of tributyl citrate and oleoyl citric acid, which is applied in the field of preparation of plastic plasticizers, can solve the problems of poor solvent resistance, poor thermal stability, poor migration resistance, etc.

Inactive Publication Date: 2008-09-03
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

At present, the product development of citric acid esters at home and abroad mainly contains triethyl citrate (TEC), acetyl triethyl citrate (ATEC), tri-n-butyl citrate (TBC), acetyl tri-n-butyl citrate ( ATBC), trioctyl citrate (TOC), acetyl trioctyl citrate (ATOC), tri-n-hexyl citrate (THC), acetyl tri-n-hexyl citrate (ATHC), butyryl tri-n-hexyl citrate (BTHC ) and other nine aspects, but these citric acid ester products generally have the defects of poor thermal stability, low plasticizer viscosity stability, insufficient low temperature flexibility, poor solvent extraction resistance and poor migration resistance in actual use. These deficiencies in performance limit the scope of use of existing citric acid ester products

Method used

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  • Method for preparing oleoyl tributyl citrate plasticizer
  • Method for preparing oleoyl tributyl citrate plasticizer
  • Method for preparing oleoyl tributyl citrate plasticizer

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preparation example Construction

[0016] The present invention is the preparation method of oleoyl tributyl citrate plasticizer, and its synthetic route is as follows:

[0017] Step 1: Synthesis of tributyl citrate

[0018]

[0019] Step 2: Synthesis of oleoyl chloride

[0020] 3CH 3 (CH 2 ) 7 CH=CH(CH 2 ) 7 COOH+PCl 3 →3CH 3 (CH 2 ) 7 CH=CH(CH 2 ) 7 COCl+H 3 PO 3

[0021] Step 3: Synthesis of oleoyl tributyl citrate

[0022]

[0023] Its specific synthetic steps are as follows:

[0024] Step 1: Synthesis of tributyl citrate. Add citric acid, n-butanol, water-carrying agent, and catalyst into a reactor equipped with electric stirring, electric heating cap heating, oil-water separation, reflux condenser, and temperature measurement system, start stirring and raise the temperature, and control the temperature at 96°C to Until anhydrous is generated, tributyl citrate is obtained;

[0025] Step 2: Synthesis of oleoyl chloride. In the reactor equipped with electric stirring, water bath heat...

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Abstract

The invention provides a method for preparing oleoyl tributyl citrate plasticizer, comprises: adding citric acid, n-butanol, water-carrying agent and catalytic agent into a reactor, stirring and heating up, controlling the temperature for reaction at 96 degree C until no water is generated again, and obtaining tributyl citrate; adding oleate into the reactor, stirring and heating up, dropping phosphorus trichloride into the reactor, reacting for 3h at 60 degree C, cooling to room temperature, standing for 2h, and separating to obtain; and a step 3, synthesizing oleoyl tributyl citrate; adding tributyl citrate and a catalytic agent into the reactor, stirring and heating up to 70 degree C, dropping oleoyl chloride, absorbing the generated hydrogen chloride by introducing the drier into base, stopping the reaction until the pH value of base has no change, and obtaining oleoyl tributyl citrate by neutralizing with sodium carbonate solution, water washing, and vacuum filtrating.

Description

technical field [0001] The invention relates to a preparation method of a plastic plasticizer. Background technique [0002] Phthalate esters, plasticizers used in polymer materials such as food packaging and children's toys, can induce cancer. Foreign countries have legislated to restrict their use and are actively looking for non-toxic plasticizers that can replace phthalates. Citrate plasticizers are a kind of promising non-toxic plasticizers with broad development prospects. At present, the product development of citric acid esters at home and abroad mainly contains triethyl citrate (TEC), acetyl triethyl citrate (ATEC), tri-n-butyl citrate (TBC), acetyl tri-n-butyl citrate ( ATBC), trioctyl citrate (TOC), acetyl trioctyl citrate (ATOC), tri-n-hexyl citrate (THC), acetyl tri-n-hexyl citrate (ATHC), butyryl tri-n-hexyl citrate (BTHC ) and other nine aspects, but these citric acid ester products generally have the defects of poor thermal stability, low plasticizer viscos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08C07C67/30C08K5/11
Inventor 崔锦峰姚向民杨保平周应萍张建强寇丹
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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