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A kind of preparation method of acetyl citrate tri(stearyl alcohol) ester

A technology of octadecanol and acetyl chloride, applied in the field of acetyl citrate triester and its synthesis, and the catalytic synthesis of medicinal acetyl citrate triester with mesoporous molecular sieve supported heteropoly acid, can solve the problem of poor catalyst reusability and anti-migration. It can improve the extraction resistance and migration resistance, increase the molecular weight, and have strong thermal stability.

Active Publication Date: 2018-01-05
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the production process of citrate plasticizers has the disadvantages of low yield, poor reusability of catalysts, and complicated impurity removal. At the same time, its products also have poor thermal stability, poor extractability, and poor migration resistance in actual use. Shortcomings

Method used

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  • A kind of preparation method of acetyl citrate tri(stearyl alcohol) ester
  • A kind of preparation method of acetyl citrate tri(stearyl alcohol) ester
  • A kind of preparation method of acetyl citrate tri(stearyl alcohol) ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Phosphotungstic heteropolyacid is dissolved in twice-distilled water, injected into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, weighs the molecular sieve MCM-41 carrier that has been baked, and pours it into the heteropolyacid solution, Add 4% molecular sieve quality sodium carbonate solid, stir to form a thick pack, treat in an oven at 110°C for 20h, filter after cooling, heat and dry to obtain the required supported heteropolyacid catalyst;

[0026] (2) Add a quantitative amount of 200g stearyl alcohol and 20g citric acid to a reactor equipped with a mechanical stirrer, a thermometer, and an oil-water separator, heat to melt the raw materials, add 0.5g catalyst and continue to heat up to 60°C, add 300ml n-Butanol, heated to reflux until the reaction is complete, and the excess stearyl alcohol is evaporated under reduced pressure;

[0027] (3) Add 10g of acetyl chloride in step (2), filter after fully reacting, reclaim the cata...

Embodiment 2

[0030] (1) Silicon-tungsten-molybdenum heteropolyacid is dissolved in double distilled water, injected into a stainless steel high-pressure autoclave with PTFE lining, weighed the baked molecular sieve MCM-41 carrier, and poured into the heteropolyacid solution , add 6% molecular sieve quality sodium carbonate solid, stir to form a thick pack, treat in an oven at 110°C for 20h, filter after cooling, heat and dry to obtain the required supported heteropolyacid catalyst;

[0031] (2) Add a quantitative amount of 300g stearyl alcohol and 25g citric acid to a reactor equipped with a mechanical stirrer, a thermometer, and an oil-water separator, heat to melt the raw materials, add 0.5g catalyst and continue to heat up to 70°C, add 300ml n-Butanol, heated to reflux until the reaction is complete, and the excess stearyl alcohol is evaporated under reduced pressure;

[0032] (3) Add 15g acetyl chloride in step (2), filter after fully reacting, reclaim catalyst, residue is washed 4 tim...

Embodiment 3

[0035] (1) Phosphotungstomolybdenum heteropolyacid is dissolved in twice distilled water, injected into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, weighed the baked molecular sieve MCM-41 carrier, and added 6% molecular sieve quality carbonic acid Sodium solid, poured into the heteropoly acid solution, stirred to form a thick pack, treated in an oven at 110°C for 24 hours, filtered after cooling, heated and dried to obtain the required supported heteropoly acid catalyst;

[0036] (2) Add a quantitative amount of 400g stearyl alcohol and 30g citric acid to a reactor equipped with a mechanical stirrer, a thermometer, and an oil-water separator, heat to melt the raw materials, add 0.5g catalyst and continue to heat up to 60°C, add 300ml n-Butanol, heated to reflux until the reaction is complete, and the excess stearyl alcohol is evaporated under reduced pressure;

[0037] (3) Add 10g acetyl chloride in step (2), filter after fully reacting, r...

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Abstract

The invention discloses a preparation method of acetyl citrate tri(stearyl alcohol). The steps of the method are: (1) preparing a mesoporous molecular sieve-supported heteropolyacid catalyst by a hydrothermal dispersion method; (2) adding a catalyst to fully react stearyl alcohol with citric acid to remove excess stearyl alcohol; (3) acetyl After chemical reaction, add sodium bicarbonate aqueous solution to wash, and obtain the crude product of acetyl citrate tri(stearyl alcohol) after layering; (4) Add water-carrying agent to remove water to obtain acetyl tri(stearyl alcohol) citrate. The method of the invention has mild reaction conditions, short reaction time, recyclable and reusable catalyst, and is suitable for industrialized production. The reaction process has a high esterification rate, a high product yield, and the product has good thermal stability, extraction resistance and migration resistance.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a kind of acetyl citrate tri(stearyl alcohol) ester and its synthesis method, in particular to a mesoporous molecular sieve loaded heteropolyacid catalytic synthesis of medicinal acetyl citrate tri(stearyl alcohol) ester Methods. Background technique [0002] Plasticizers, also known as plasticizers and plasticizers, are mainly used in polymer materials such as plastics and rubber to increase the plasticity of products. Traditional plasticizers are phthalates. This kind of plasticizers will cause serious harm to the human body. Long-term consumption will cause damage to the human reproductive ability, immune system and digestive system, and will cause cancer and other diseases. occur. Therefore, it is imminent for relevant enterprises to replace phthalate plasticizers with non-toxic and environmentally friendly plasticizers. [0003] Citrate plasticizers are a green alternative ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C67/14C07C69/67B01J31/18B01J31/16
CPCY02P20/584
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA
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