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Synthesis process of antioxidant 618

A synthesis process and antioxidant technology, applied in the field of synthesis of phosphite antioxidants, can solve problems such as side reactions, low yield, phosphorus trichloride corrosion, etc., achieve short process cycle, reduce costs, and reduce decomposition Effect

Inactive Publication Date: 2019-07-23
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method also has shortcomings such as phosphorus trichloride is easy to hydrolyze, and the experiment needs to be carried out under anhydrous conditions; aromatic hydrocarbons (toluene) must be added as a solvent in the reaction
The synthesis process is relatively complicated, and the post-processing process is cumbersome
In the conventional method, phosphorus trichloride corrodes seriously in the tank reactor, and the sealing of the tank-type dripping reaction is poor, and it is easy to absorb water to cause side reactions; and in the reaction process, the phosphorus trichloride addition rate needs to be slow. Fast, will make the yield very low, and there are certain potential safety hazards

Method used

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  • Synthesis process of antioxidant 618
  • Synthesis process of antioxidant 618
  • Synthesis process of antioxidant 618

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) 1 part of substance phosphorus trichloride is mixed with 2 parts of substance n-hexane to form a solution, and the solution is pumped into the first module of the microreactor through a metering pump for precooling at 0°C; the amount of 6 substances A portion of ethanol is pumped into the second module through another metering pump for 0°C precooling;

[0029] (2) The pre-cooled phosphorus trichloride, n-hexane solution and ethanol are mixed in the third module and reacted at -10°C for 12s to form a mixed solution;

[0030] (3) The mixed solution flows into the tubular reactor, and in the tubular reactor, 1.5 parts of tributylamine are added for neutralization;

[0031] (4) Carry out negative pressure suction filtration, and rotary steaming removes ethanol and normal hexane, obtains triethyl phosphite reaction liquid; Return separated ethanol and normal hexane to step (1);

[0032] (5) The triethyl phosphite reaction liquid enters into another microreactor, and 0.5...

Embodiment 2

[0038] (1) 1 part of substance phosphorus trichloride is mixed with 2 parts of substance n-hexane to form a solution, and the solution is pumped into the first module of the microreactor through a metering pump for precooling at 0°C; the amount of 6 substances A portion of ethanol is pumped into the second module through another metering pump for 0°C precooling;

[0039] (2) The pre-cooled phosphorus trichloride, n-hexane solution and ethanol are mixed in the third module and reacted at -8°C for 12s to form a mixed solution;

[0040] (3) the mixed solution flows into the tubular reactor, and adds 1.5 parts of liquid ammonia in the tubular reactor for neutralization;

[0041] (4) Carry out negative pressure suction filtration, and rotary steaming removes ethanol and normal hexane, obtains triethyl phosphite reaction liquid; Return separated ethanol and normal hexane to step (1);

[0042] (5) The triethyl phosphite reaction solution enters into another microreactor, and 0.5 par...

Embodiment 3

[0048] (1) 1 part of substance phosphorus trichloride is mixed with 2 parts of substance n-hexane to form a solution, and the solution is pumped into the first module of the microreactor through a metering pump for precooling at 0°C; the amount of 6 substances A portion of ethanol is pumped into the second module through another metering pump for 0°C precooling;

[0049] (2) The pre-cooled phosphorus trichloride, n-hexane solution and ethanol are mixed in the third module and reacted at -10°C for 10s to form a mixed solution;

[0050] (3) The mixed solution flows into the tubular reactor, and adds 1.5 parts of substance, diethylaniline in the tubular reactor for neutralization;

[0051] (4) carry out negative pressure suction filtration, rotary steaming removes ethanol and normal hexane, obtains triethyl phosphite reaction liquid; Return separated ethanol and normal hexane to step (1);

[0052] (5) The triethyl phosphite reaction liquid enters in another microreactor, and 0.5...

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Abstract

The invention belongs to the synthesis technology of phosphite antioxidants, in particular to a synthesis technology of antioxidant 618. Triethyl phosphite is synthesized through a microreactor, pentaerythritol diphosphite is synthesized, and the antioxidant 618 is finally synthesized. The synthesis process of the antioxidant 618 has the advantages of good sealing performance, easy control of reaction conditions, reflux utilization of solvents and products, and cost saving.

Description

technical field [0001] The invention belongs to the synthesis technology of phosphite antioxidant, in particular to a synthesis process of antioxidant 618. Background technique [0002] The traditional process for the production of antioxidant 618 uses triphenyl phosphite, pentaerythritol and stearyl alcohol as raw materials, and uses organotin as a catalyst to synthesize the target product by one-step transesterification. The production process of this method is simple and the reaction conditions are mild. The trace amount of phenol remaining in the product produced by this method cannot be completely removed, which affects the quality of the product and limits the application of the product in food packaging materials. Some researchers proposed the idea of ​​phenol-free synthesis, that is, to synthesize antioxidant 618 in two steps using phosphorus trichloride, pentaerythritol and stearyl alcohol as raw materials. The advantage of this method is that no phenol is produced ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/141
CPCC07F9/1412
Inventor 郭骄阳赵崇鑫
Owner JIANGSU JIYI NEW MATERIAL CO LTD