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Citrate plasticizer

A technology of citrate ester and plasticizer, which is applied in the field of plastic rubber plasticizer, can solve the problems of poor solvent extraction resistance and migration resistance, insufficient migration resistance and flame retardancy, and improper number ratio. Achieve good migration resistance, meet the requirements of industrial production, and achieve the effect of low volatility

Inactive Publication Date: 2021-05-14
马海社
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the small molecular weight, the ratio of the number of non-polar aliphatic carbon atoms to the number of polar ester groups (A P / A O ) and other reasons, the current citrate triester plasticizers still have shortcomings such as thermal stability, low temperature flexibility, solvent extraction resistance and migration resistance in actual use.
Scientific research workers have improved citrate triester plasticizers, such as octadecanoyl tributyl citrate (CN101255240A), oleoyl tributyl citrate (CN101255114A); developed two citrate triesters ( US3239555, CN1037350A) is to connect two citric acid triester molecules through fatty chains (the number of carbon atoms is usually 1 to 12) to form a double citrate triester molecule; Esterification (CN104163760B) has developed a highly branched citrate triester plasticizer; although this type of modified citrate triester molecule has improved the plasticizing effect to a certain extent, thermal stability, low temperature flexibility, resistance Solvent extractability, anti-migration and flame retardancy are still insufficient, which limits its application and cannot meet the actual needs

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation of tributyl citrate containing isocyanurate comprises the following steps:

[0029] 1) Preparation of tributyl citrate: add 100mol citric acid, 380mol butanols, p-benzenemethanesulfonic acid (mass fraction is 2% of the total mass of citric acid and alcohol) and 40L water-carrying agent cyclohexane in the reactor , heated to 120°C under stirring, refluxed for 4 hours, recovered excess alcohol by distillation under reduced pressure to obtain crude tributyl citrate, then washed the crude tributyl citrate with 2% sodium bicarbonate solution, removed the catalyst, and recovered the organic phase to obtain Tributyl Citrate.

[0030] 2) Preparation of carboxyl-containing tributyl citrate: add 100 mol carbon tetrachloride, 70 mol tributyl citrate and 70 mol succinic anhydride into the reaction kettle, feed nitrogen into the reaction kettle, stir and heat up to 70°C, react for 4 hours, After cooling, it was extracted and separated with ethyl acetate, and the org...

Embodiment 2

[0034] The preparation of tripentyl citrate containing isocyanurate comprises the following steps:

[0035]1) Preparation of tripentyl citrate: add 100mol citric acid, 400mol amyl alcohol, p-benzenemethanesulfonic acid (mass fraction is 2% of the total mass of citric acid and alcohol) and 40L water-carrying agent cyclohexane in the reactor , heated to 140°C under stirring, refluxed for 4 hours, and recovered excess alcohol by distillation under reduced pressure to obtain the crude product of tripentyl citrate, then washed the crude product of triamyl citrate with 2% sodium bicarbonate solution, removed the catalyst, and recovered the organic phase to obtain Tripentyl Citrate.

[0036] 2) Preparation of carboxyl-containing tripentyl citrate: add 100 mol carbon tetrachloride, 70 mol tripentyl citrate and 70 mol succinic anhydride into the reaction kettle, feed nitrogen into the reaction kettle, stir and heat up to 70° C., react for 4 hours, After cooling, it was extracted and s...

Embodiment 3

[0040] The preparation of trioctyl citrate containing isocyanurate comprises the following steps:

[0041] 1) Preparation of trioctyl citrate: add 100mol citric acid, 380mol octanol, p-benzenemethanesulfonic acid (mass fraction is 2% of the total mass of citric acid and alcohol) and 40L water-carrying agent cyclohexane in the reactor , heated to 150°C under stirring, refluxed for 4 hours, recovered excess alcohol by distillation under reduced pressure to obtain crude trioctyl citrate, then washed the crude trioctyl citrate with 2% sodium bicarbonate solution, removed the catalyst, and recovered the organic phase to obtain Trioctyl Citrate.

[0042] 2) Preparation of carboxyl-containing trioctyl citrate: add 100 mol carbon tetrachloride, 70 mol trioctyl citrate and 70 mol adipic anhydride into the reaction kettle, feed nitrogen into the reaction kettle, stir and heat up to 75 ° C, react for 5 hours, After cooling, it was extracted and separated with ethyl acetate, and the orga...

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Abstract

The invention discloses a citrate plasticizer and a preparation method thereof, and the preparation method of citrate comprises the following steps: firstly, citric acid and alcohol react to prepare citric acid triester, and then dianhydride acylation is carried out to prepare carboxyl-containing citric acid triester. After chlorination, the carboxyl-containing citric acid triester and the tris(2-ethoxyl) isocyanurate are subjected to esterification reaction to prepare triester citrate containing the isocyanurate. According to the present invention, the preparation method has characteristics of simple operation, wide raw material source and mild reaction condition, and meets the industrial production, the prepared triester citrate containing isocyanurate has a good plasticizing effect and excellent thermal stability, low-temperature flexibility, solvent extraction resistance, migration resistance and flame retardance, and can be widely applied to plastic rubber plasticizers.

Description

technical field [0001] The invention relates to a citrate plasticizer, which belongs to the technical field of plastic rubber plasticizers. Background technique [0002] Plasticizer is the category with the largest production capacity and consumption among plastic processing aids. Especially since the 1980s, with the continuous development of polyvinyl chloride (PVC) products, the plasticizer industry has shown a situation of rapid development. Citrate triester plasticizers are synthesized with citric acid as the main raw material. Due to its rich sources and low price, it has now become one of the plasticizers of choice in the plastics industry at home and abroad. Its main varieties are triethyl citrate ( TEC), acetyl triethyl citrate (ATEC), acetyl tri-n-butyl citrate (ATBC), tri-n-butyl citrate (TBC), tri-n-hexyl citrate (THC), acetyl tri-n-hexyl citrate ( ATHC) etc. However, due to the small molecular weight, the ratio of the number of non-polar aliphatic carbon atoms ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/30C08K5/3492
CPCC07D251/30C08K5/34924
Inventor 马海社
Owner 马海社
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