CN104649958A - A preparing method of bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate - Google Patents
A preparing method of bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate Download PDFInfo
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- CN104649958A CN104649958A CN201310580562.3A CN201310580562A CN104649958A CN 104649958 A CN104649958 A CN 104649958A CN 201310580562 A CN201310580562 A CN 201310580562A CN 104649958 A CN104649958 A CN 104649958A
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- tetramethyl
- sebacate
- hydroxy
- organic phase
- piperidyl
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D211/00—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings
- C07D211/04—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D211/06—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D211/36—Heterocyclic compounds containing hydrogenated pyridine rings, not condensed with other rings with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D211/40—Oxygen atoms
- C07D211/44—Oxygen atoms attached in position 4
- C07D211/46—Oxygen atoms attached in position 4 having a hydrogen atom as the second substituent in position 4
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Hydrogenated Pyridines (AREA)
Abstract
A preparing method of bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate is disclosed. The method includes following steps of: (1) adding dimethyl sebacate and 2,2,6,6-tetramethyl-4-hydroxypiperidine in a mass ratio of 1:2.1, as well as an activated carbon loaded catalyst and a solvent into a three-neck distillation flask having a thermometer, a stirrer and a water separator, stirring, heating to 100 DEG C, and reacting for 6 h; and (2) after the reaction is completed, washing with water, collecting an organic phase, and subjecting the organic phase to dehydration, decoloring and crystallization to obtain white crystal powder that is the bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate. The method adopts titanium tert-butoxide loaded by activated carbon as the catalyst and is high in product yield and high in product purity. In addition, the catalyst is low in cost, easily available, high in catalytic activity, non-corrosive to equipment, free of environment pollution and environmental friendly.
Description
Technical field
The present invention relates to a kind of preparation method of hindered amine light stabilizer, be specifically related to a kind of preparation method of sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester.
Background technology
Sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester is the hindered amine light stabilizer of low relative molecular mass high-efficiency low-toxicity.It and most industry solvent phase dissolubility well, have superior polymer intermiscibility.Traditional synthetic method is by dimethyl sebacate and 2,2,6,6-tetramethyl--4-hydroxy piperidine is raw material, take sodium methylate as catalyzer, and dimethylbenzene is carry out transesterification reaction under the condition of solvent, because catalyzer is unstable, dangerous large dimethylbenzene toxicity is large, and the contaminated wastewater that aftertreatment produces is large, is not suitable for modern industrialization and produces.Adopt Lewis acid, alkali etc. to carry out transesterification reaction for catalyzer, the pollution of catalyzer corrosive equipment greatly, poor product quality.
Summary of the invention
The object of the invention is to, a kind of sebacic acid two (2 is provided, 2,6,6-tetramethyl--4-hydroxy piperidine) preparation method of ester, adopt activated carbon supported tetrabutyl titanate ester to be catalyzer, product yield is high, purity is high, and this catalyzer is cheap and easy to get, catalytic activity good, not etching apparatus, non-environmental-pollution, environmental protection.
The preparation method of described sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester, it comprises the following steps:
One, be that the dimethyl sebacate of 1:2.1 and 2,2,6,6-tetramethyl--4-hydroxy piperidine, activated carbon supported catalysts and solvents add in the there-necked flask that thermometer, agitator and water trap are housed by mass ratio, be heated with stirring to 100 DEG C, reaction 6h;
Two, react complete, washing, collect organic phase, organic phase carries out dewatering, decolour, namely crystallization obtain white crystalline powder sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester.
Sebacic acid two (2 provided by the invention, 2,6,6-tetramethyl--4-hydroxy piperidine) preparation method of ester, its beneficial effect is, adopts activated carbon supported tetrabutyl titanate ester to be catalyzer, product yield is high, purity is high, and this catalyzer is cheap and easy to get, catalytic activity good, not etching apparatus, non-environmental-pollution, environmental protection.
Embodiment
Below in conjunction with an embodiment, the preparation method of sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester provided by the invention is described in detail.
Embodiment
One, be that the dimethyl sebacate of 1:2.1 and 2,2,6,6-tetramethyl--4-hydroxy piperidine, activated carbon supported catalysts and solvents add in the there-necked flask that thermometer, agitator and water trap are housed by mass ratio, be heated with stirring to 100 DEG C, reaction 6h;
Two, react complete, washing, collect organic phase, organic phase carries out dewatering, decolour, namely crystallization obtain white crystalline powder sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester.
Claims (1)
1. the preparation method of sebacic acid two (2,2,6, a 6-tetramethyl--4-hydroxy piperidine) ester, is characterized in that: it comprises the following steps:
One, be that the dimethyl sebacate of 1:2.1 and 2,2,6,6-tetramethyl--4-hydroxy piperidine, activated carbon supported catalysts and solvents add in the there-necked flask that thermometer, agitator and water trap are housed by mass ratio, be heated with stirring to 100 DEG C, reaction 6h;
Two, react complete, washing, collect organic phase, organic phase carries out dewatering, decolour, namely crystallization obtain white crystalline powder sebacic acid two (2,2,6,6-tetramethyl--4-hydroxy piperidine) ester.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310580562.3A CN104649958A (en) | 2013-11-19 | 2013-11-19 | A preparing method of bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310580562.3A CN104649958A (en) | 2013-11-19 | 2013-11-19 | A preparing method of bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate |
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| Publication Number | Publication Date |
|---|---|
| CN104649958A true CN104649958A (en) | 2015-05-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310580562.3A Pending CN104649958A (en) | 2013-11-19 | 2013-11-19 | A preparing method of bis(2,2,6,6-tetramethyl-4-hydroxy-piperidyl) sebacate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230511A (en) * | 2021-12-31 | 2022-03-25 | 利安隆凯亚(河北)新材料有限公司 | Preparation method of bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate |
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2013
- 2013-11-19 CN CN201310580562.3A patent/CN104649958A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230511A (en) * | 2021-12-31 | 2022-03-25 | 利安隆凯亚(河北)新材料有限公司 | Preparation method of bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate |
| CN114230511B (en) * | 2021-12-31 | 2024-01-26 | 利安隆凯亚(河北)新材料有限公司 | Preparation method of bis (2, 6-tetramethyl-4-piperidinyl) sebacate |
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| PB01 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150527 |