CN102464609A - Triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical and preparation process thereof - Google Patents
Triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical and preparation process thereof Download PDFInfo
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- CN102464609A CN102464609A CN2010105479245A CN201010547924A CN102464609A CN 102464609 A CN102464609 A CN 102464609A CN 2010105479245 A CN2010105479245 A CN 2010105479245A CN 201010547924 A CN201010547924 A CN 201010547924A CN 102464609 A CN102464609 A CN 102464609A
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- carbonyl
- triacetonamine
- tetramethylpiperidine
- oxygen radical
- tetramethyl piperidine
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Abstract
The invention discloses a triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical, of which the molecular structural formula is shown in the specifications. The invention further discloses a process for preparing the triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical. The process comprises the following steps of: preparing triacetonamine; and mixing, synthesizing, filtering, removing a solvent, packaging, and the like to obtain the triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical. The triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical serving as a polymerization inhibitor and a key intermediate in the process plays important roles in the petrochemical industry. According to the process, the product with an environmentally-friendly process and stable quality is obtained by performing oxosynthesis, and the problem of storage of triacetonamine is solved indirectly simultaneously.
Description
Technical field:
The present invention relates to a kind of triacetonamine 4-carbonyl-2,2,6, the ME of 6-tetramethyl piperidine oxyradical makes through the oxidation synthesis technique.
Background technology:
Product triacetonamine thermo-sensitivity is extremely strong, and is oxidized very easily at normal temperatures, is difficult for storing; And the present triacetonamine of our company can only be done tetramethylpiperidinol as midbody, the triacetonamine 4-carbonyl-2,2 of development of new; 6,6-tetramethyl piperidine oxyradical is as the dark a kind of product in edge, triacetonamine downstream, because outward appearance is an orange; Solved yellowing triacetonamine take off a white difficult problem, improved benefit, reduced cost.
Summary of the invention:
The objective of the invention is to solve the handling problem of triacetonamine variable color material, reduced cost, reach energy saving purposes.
Technical solution of the present invention is: a kind of triacetonamine 4-carbonyl-2,2,6, and the method for manufacture of 6-tetramethyl piperidine oxyradical is characterized in that: said triacetonamine 4-carbonyl-2,2,6, the molecular structural formula of 6-tetramethyl piperidine oxyradical is following:
A kind of manufacturing triacetonamine 4-carbonyl-2,2,6, the ME of 6-tetramethyl piperidine oxyradical is at first made raw material with outward appearance xanchromatic triacetonamine, makes through processes such as mix, synthetic, extraction, filtration, desolventizing, barrellings then; It is characterized in that: the said triacetonamine 4-carbonyl-2,2,6 that makes, the technology of 6-tetramethyl piperidine oxyradical is: it is synthetic to make catalyzer with ydrogen peroxide 50 and outward appearance xanchromatic triacetonamine with alkali formula magnesium, makes through aftertreatment again.
Said synthesis temperature is: 35-38 ℃.
The mol ratio of said 35% ydrogen peroxide 50 and triacetonamine is 1.2: 1.
Beneficial effect: triacetonamine 4-carbonyl-2; 2,6,6-tetramethyl piperidine oxyradical is as stopper and key intermediate; The status that the weight lifting weight is arranged aspect petrochemical complex; This technology obtains the technology environmental protection through oxidation is synthetic, and stable product qualitatively connects the problem that triacetonamine is stored that solved between simultaneously.
Up-to-date technical development requires to have higher to stopper, the environmental protection of high-quality and efficient low toxicity technology is the fundamental of developing new product.So three ketoamine 4-carbonyls-2,2,6, the exploitation of 6-tetramethyl piperidine oxyradical is that company first develops target.
The present invention is through making triacetonamine 4-carbonyl-2,2,6 with oxidation is synthetic, and 6-tetramethyl piperidine oxyradical satisfies client's demand.
Concrete embodiment:
Below in conjunction with instance the present invention is described further:
Embodiment 1:
Preparing method: 27.5% ydrogen peroxide 50, triacetonamine, catalyzer alkali formula magnesium, toluene.
(a) in the reaction flask of the 500ml that condensing surface, return line, TM, whisking appliance and Dropping feeder are housed, with adding 2,2,6 of quantitative 155g; 6-tetramethylpiperidone, catalyzer alkali formula magnesium 2g drop in the reaction kettle, 35-38 ℃ of following agitator, to the reactor drum heating, are warming up to 35 ℃ earlier and begin to drip the 116g ydrogen peroxide 50 simultaneously; Dropwised in 4 hours, and be incubated 2 hours again, add 150ml extracted in toluene material again, lower aqueous solution gets into environment-friendly processing unit and carries out biochemical treatment; Upper materials high vacuum is at low temperatures sloughed solvent, again through overheated filter, obtains product triacetonamine 4-carbonyl-2; 2,6,6-tetramethyl piperidine oxyradical.Sampling analysis can be packed after qualified, and the solvent of deviating from is made the solvent recuperation of extraction and applied mechanically.
Claims (4)
1. triacetonamine 4-carbonyl-2,2,6,6-tetramethyl piperidine oxyradical is characterized in that: triacetonamine 4-carbonyl-2,2,6, the molecular structural formula of 6-tetramethyl piperidine oxyradical is following:
2. make the described triacetonamine 4-of claim 1 carbonyl-2,2,6 for one kind, the ME of 6-tetramethyl piperidine oxyradical at first makes triacetonamine, makes through processes such as mix, synthetic, filtration, desolventizing, packings then; It is characterized in that: the said triacetonamine 4-carbonyl-2,2,6 that makes, the technology of 6-tetramethyl piperidine oxyradical is: with ydrogen peroxide 50 and triacetonamine, add alkali formula magnesium again and synthesize, make through aftertreatment.
3. a kind of triacetonamine 4-carbonyl-2,2,6 according to claim 2, the ME of 6-tetramethyl piperidine oxyradical is characterized in that: said synthesis temperature is: 35 ℃-38 ℃.
4. a kind of manufacturing elaboration triacetonamine 4-carbonyl-2,2,6 according to claim 2, the ME of 6-tetramethyl piperidine oxyradical is characterized in that: the mol ratio of said ydrogen peroxide 50 and triacetonamine is 1.2: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105479245A CN102464609A (en) | 2010-11-18 | 2010-11-18 | Triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical and preparation process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105479245A CN102464609A (en) | 2010-11-18 | 2010-11-18 | Triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical and preparation process thereof |
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| CN102464609A true CN102464609A (en) | 2012-05-23 |
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| CN2010105479245A Pending CN102464609A (en) | 2010-11-18 | 2010-11-18 | Triacetonamine4-carbonyl-2,2,6,6-tetramethylpiperidine oxygen radical and preparation process thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5416215A (en) * | 1992-06-13 | 1995-05-16 | Huels Aktiengesellschaft | Process to preparing 2,2,6,6-tetra-methylpiperidine-n-oxyl and its 4-position substituted derivatives |
| CN101048378A (en) * | 2004-11-02 | 2007-10-03 | 西巴特殊化学品控股有限公司 | Process for the synthesis of n-alkoxyamines |
| CN101475525A (en) * | 2009-02-18 | 2009-07-08 | 常熟市瑞凯添加剂科技有限公司 | Preparation of piperidine nitroxyl radical anti-polymerization inhibitor |
-
2010
- 2010-11-18 CN CN2010105479245A patent/CN102464609A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5416215A (en) * | 1992-06-13 | 1995-05-16 | Huels Aktiengesellschaft | Process to preparing 2,2,6,6-tetra-methylpiperidine-n-oxyl and its 4-position substituted derivatives |
| CN101048378A (en) * | 2004-11-02 | 2007-10-03 | 西巴特殊化学品控股有限公司 | Process for the synthesis of n-alkoxyamines |
| CN101475525A (en) * | 2009-02-18 | 2009-07-08 | 常熟市瑞凯添加剂科技有限公司 | Preparation of piperidine nitroxyl radical anti-polymerization inhibitor |
Non-Patent Citations (2)
| Title |
|---|
| MARK L. SMYTHE，等: "a-Helical versus 3 10-Helical Conformation of Alanine-Based Peptides in Aqueous Solution: An Electron Spin Resonance Investigation", 《J.AM.CHEM.SOC》 * |
| 陈苗琴，等: "1-环己氧基-4-氧-2,2,6,6-四甲基哌啶酮的合成与表征", 《高等化学工程学报》 * |
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Application publication date: 20120523 |