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Preparation method for synthesizing polymerization inhibitor 702 from acetone and ammonia gas through one-pot method

A technology of polymerization inhibitor and ammonia gas, which is applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc. It can solve problems such as long reaction time, waste liquid polluting the environment, and product quality not meeting the requirements. , to achieve the effect of simple and convenient preparation method, mild reaction conditions, and reduced manpower and material resources

Active Publication Date: 2021-04-27
上海博栋化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the two-step synthesis process, the yield of the product obtained is low, the reaction time is long, and by-products are easily formed, which makes the product quality not meet the requirements. At the same time, the amount of catalyst used is large and cannot be separated and recovered effectively. The product can only be obtained by crystallization, resulting in A large amount of waste liquid pollutes the environment

Method used

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  • Preparation method for synthesizing polymerization inhibitor 702 from acetone and ammonia gas through one-pot method
  • Preparation method for synthesizing polymerization inhibitor 702 from acetone and ammonia gas through one-pot method
  • Preparation method for synthesizing polymerization inhibitor 702 from acetone and ammonia gas through one-pot method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of Supported Catalysts

[0024] Purification of activated carbon: Add 100 g of activated carbon to 500 mL of hydrochloric acid solution with a mole fraction of 1 mol / L, sonicate for 1 hour, and then let stand for 4 hours. After filtering, the obtained filter cake was rinsed three times with deionized water, then put into a vacuum drying oven, and baked at 100° C. for 4 hours to obtain 98.6 g of purified activated carbon.

[0025] Treatment with hydrochloric acid solution can remove sodium, potassium, calcium, iron and other elements in activated carbon to form water-soluble salts, reduce the gray level of activated carbon, and ensure the relative stability of activated carbon performance.

[0026] Preparation of carrier catalyst: Weigh a certain amount of phosphotungstic acid and dissolve it in 100mL of deionized water, then add 10g of purified activated carbon, heat to reflux for 1 to 4 hours, and then filter. Rinse the obtained filter cake 3 times with de...

Embodiment 1-1

[0028] Preparation of Supported Catalyst PTA / C-0.1

[0029] Weigh 1g of phosphotungstic acid and dissolve it in 100mL of deionized water, then add 10g of the above-mentioned purified activated carbon, heat to reflux for 2 hours, and then filter. The obtained filter cake was rinsed with deionized water three times, then placed in a vacuum drying oven, and baked at 100°C for 8 hours to obtain 10 g of activated carbon-supported phosphotungstic acid carrier catalyst, which was designated as PTA / C-0.1.

[0030] 0.1 in PTA / C-0.1 represents the feed ratio of phosphotungstic acid to activated carbon.

Embodiment 1-2～1-5

[0032] According to the preparation method of embodiment 1-1 carrier catalyst PTA / C-0.1, the carrier catalysts of different loads are prepared, respectively embodiment 1-2, carrier catalyst is marked as PTA / C-0.2; Embodiment 1-3, carrier Catalyst is marked as PTA / C-0.3; Embodiment 1-4, carrier catalyst is marked as PTA / C-0.4 and embodiment 1-5, and carrier catalyst is marked as PTA / C-0.5, as shown in table 1 below:

[0033] The output of table 1 supported catalyst

[0034]

[0035] Preparation of Inhibitor 702

[0036]

[0037] The general preparation steps are: add acetone and a certain amount of carrier catalyst into the reaction kettle, continuously feed ammonia gas, the molar ratio of ammonia gas to acetone is 1:10~1:4, and react at 50~60°C for 4 hours . Then add a certain amount of deionized water, slowly add hydrogen peroxide, and stir for 2 hours at 25°C. The supported catalyst was obtained by filtration, and then the obtained filtrate was subjected to vacuum d...

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Abstract

The invention belongs to the technical field of polymerization inhibitor synthesis, and discloses a preparation method for synthesizing a polymerization inhibitor 702 from acetone and ammonia gas through a one-pot method. The preparation method comprises the following steps: adding acetone and a carrier catalyst into a reaction kettle, introducing ammonia gas, and conducting reacting at 50-60 DEG C for 2-6 hours; and then adding deionized water and hydrogen peroxide, conducting reacting at 15-40 DEG C for 1-3 hours, filtering the reaction solution, and carrying out reduced-pressure distillation on the obtained filtrate to obtain the polymerization inhibitor 702. According to the invention, reaction conditions are mild, the preparation method is simple and convenient, the carrier catalyst is easy to separate, and product yield is high.

Description

technical field [0001] The invention relates to the technical field of synthesis of polymerization inhibitors, in particular to a preparation method for synthesizing polymerization inhibitor 702 in one pot using acetone and ammonia as raw materials. Background technique [0002] Inhibitor 702, also known as nitroxide free radical piperidinone, chemical name 4-oxo-2,2,6,6-tetramethylpiperidine-1-oxyl free radical. The compound has good polymerization inhibition effect on acrylates, methacrylates, acrylic acid, acrylonitrile, styrene and butadiene. Its polymerization inhibition performance is better than that of phenols, aromatic amines, ethers, quinones and nitro compounds and other polymerization inhibitors. [0003] The traditional process mainly includes two steps. First, tetramethylpiperidone is prepared from acetone and ammonia as raw materials. Then use sodium tungstate or phosphotungstic acid as a catalyst, tetramethylpiperidone as a raw material, hydrogen peroxide a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/94B01J27/188B01J37/02
CPCC07D211/94B01J27/188B01J37/0207
Inventor 郭颖毕景峰李嫚嫚王尹卓潘惠英
Owner 上海博栋化学科技有限公司