Maleic acid tributyl citrate diester compound and preparation method thereof

A technology of butenedioic acid citric acid and tributyl citrate, which is applied in the field of plastic plasticizers, can solve problems such as thermal stability and poor volatility, and achieve improved anti-aging performance, high yield, and good anti-bleeding sexual effect

Inactive Publication Date: 2010-07-21
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

because A p / P o The value has a great influence on the performance of the plasticizer, the smaller the value, the better the compatibility, plasticizing efficiency, oil resistance, low temperature flexibility, but the worse the thermal stability and volatility

Method used

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  • Maleic acid tributyl citrate diester compound and preparation method thereof
  • Maleic acid tributyl citrate diester compound and preparation method thereof
  • Maleic acid tributyl citrate diester compound and preparation method thereof

Examples

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preparation example Construction

[0031] see Figure 1~3 , the preparation method of butenedioic acid tributyl citrate diester, comprises the following steps:

[0032] 1) Synthesis of tributyl citrate: add citric acid (2) and excess n-butanol (3) in the reaction kettle, then add iron trichloride hexahydrate (FeCl 3 ·6H 2 O) as a catalyst, stir and heat up to 108-115° C., reflux reaction until anhydrous is generated, and recover the residual n-butanol (3) by distillation to obtain tributyl citrate (4);

[0033] 2) Synthesis of fumaric acid: Add maleic anhydride (5) and water 2 to 2.5 times its mass in the reaction kettle, stir until the solution is clear and carry out hydrolysis reaction to generate maleic anhydride (6 ), then add thiourea (7) with 2% maleic anhydride mass as a catalyst, stir and heat to 70°C and keep it for 0.5-0.8h, cool to room temperature, filter, wash the solid with distilled water, and obtain trans Butenedioic acid (8);

[0034] 3) Synthesis of trans-butene dichloride: add fumaric aci...

Embodiment 1

[0037] The preparation of butenedioic acid tributyl citrate diester comprises the following steps:

[0038] 1) Synthesis of tributyl citrate: in parts by mass, add 35 parts of citric acid and 58 parts of n-butanol (excessive) in the reactor, then add citric acid quality 4% (1.4 parts) of six Ferric trichloride hydrate is used as a catalyst for esterification reaction, stirred and heated to 108 ° C, and refluxed with a serpentine condenser tube, reacted to anhydrous (H 2 O) generate, after distillation reclaims excess n-butanol remaining, obtain tributyl citrate;

[0039] 2) Synthesis of fumaric acid: in parts by mass, add 95 parts of maleic anhydride and 190 parts of water in the reactor, stir and carry out hydrolysis reaction until the solution is clear without separation, and then Add 1.8 parts of thiourea directly to the system as a catalyst (2% of the mass of maleic anhydride), stir and heat to 70°C, the system quickly becomes cloudy, keep the reaction at 70°C for 0.5h, coo...

Embodiment 2

[0043] The preparation of butenedioic acid tributyl citrate diester comprises the following steps:

[0044] 1) Synthesis of tributyl citrate: in parts by mass, add 38.6 parts of citric acid and 59.4 parts of n-butanol (excessive) in the reactor, then add citric acid quality 5.1% (2.0 parts) of six Ferric trichloride hydrate is used as a catalyst for esterification reaction, stirred and heated to 115 ° C, and refluxed with a serpentine condenser tube, reacted to anhydrous (H 2 O) generate, after distillation reclaims excess n-butanol remaining, obtain tributyl citrate;

[0045] 2) Synthesis of fumaric acid: in parts by mass, add 98 parts of maleic anhydride and 200 parts of water in the reactor, stir and carry out hydrolysis until the solution is clear without separation, and then Add 2.0 parts of thiourea directly to the system as a catalyst (2% of the mass of maleic anhydride), stir and heat to 70°C, the system quickly becomes cloudy, keep the reaction at 70°C for 0.5h, cool...

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Abstract

The invention discloses a new type green environmental protection type plastic plasticizer, which belongs to the technical field of plastic plasticizers and has the chemical name of maleic acid tributyl citrate diester. The invention also discloses a preparation method of the compound. Tributyl citrate and trans-maleic acid chloride are synthesized into a whole by a converging method, thereby effectively preparing a final product of the maleic acid tributyl citrate diester. The Maleic acid tributyl citrate diester as the plastic plasticizer has the advantages of small volatility, high stability, good anti-migration, good anti-extraction performance, good low-temperature flexibility, safety and no toxicity.

Description

technical field [0001] The invention belongs to the technical field of plastic plasticizers, and relates to a green and environment-friendly plastic plasticizer, in particular to butenedioic acid tributyl citrate diester and a preparation method thereof. Background technique [0002] The traditional plastic plasticizer is a phthalate (DOP) type structure containing an aromatic skeleton. This type of plastic plasticizer has carcinogenic toxicity, can cause anemia, hematuria, affect liver cells and white blood cells, and is harmful to the human body. Especially infants and young children have certain toxic and side effects. Therefore, developed countries such as Europe and the United States have strictly requested to limit the use of such plasticizers in infant toys. [0003] Citrate plastic plasticizer is a green and environment-friendly replacement product that can replace phthalate plasticizer. As a new type of non-toxic, low-toxic or biodegradable plastic additives, this...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/14
Inventor 孟歌杨涛师建华郑美林王梅赵桂兰
Owner XI AN JIAOTONG UNIV
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