CN103274995A - Process for manufacturing polymerization inhibitor 708 - Google Patents
Process for manufacturing polymerization inhibitor 708 Download PDFInfo
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- CN103274995A CN103274995A CN2013102385822A CN201310238582A CN103274995A CN 103274995 A CN103274995 A CN 103274995A CN 2013102385822 A CN2013102385822 A CN 2013102385822A CN 201310238582 A CN201310238582 A CN 201310238582A CN 103274995 A CN103274995 A CN 103274995A
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- stopper
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- polymerization inhibitor
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Abstract
The invention relates to a technological method for manufacturing a polymerization inhibitor in polymeric additives, and aims to provide a process for manufacturing a polymerization inhibitor 708 with a one-pot method so as to fill up a gap in the industry. According to the process for manufacturing the polymerization inhibitor 708, the one-pot method is used; and by the aid of the solid catalyst one-pot method, the reaction efficiency can be effectively improved. The process is combined with actual production, so that the previous multi-step reaction is replaced; and moreover, a liquid catalyst is replaced with solid base. The process is mainly applied to clean production, the quality is improved, and the effects are increased.
Description
Technical field
The present invention relates to the processing method of stopper in a kind of polymeric additive.
Background technology
Stopper molecule and chain free radical reaction form the low activity free radical that the non-free radical material maybe can not cause, thereby polymerization is stopped.Stopper can prevent the carrying out of polymerization, in storage, transportation, often add stopper to prevent producing inductive phase (being that polymerization velocity is for some time of zero) in the polymerization at the polymerization process monomer, the length of inductive phase is directly proportional with level of inhibitor, after stopper runs out of, finish inductive phase, and the usual dispatch when namely existing by no stopper is carried out.At present, have only stopper 701 on the market, be used for substituting and pollute bigger hydroquinone, be widely used in the production of acrylate, methacrylic acid, vinyl acetate, also be used for vinylchlorid, unsaturated polyester and the galloping Malaysia and China of agricultural chemicals.Stopper 708(full name 4-butoxy-2,2,6,6-tetramethyl piperidine-1-oxygen is from free radical) as revitalizing product innovation of chemical development, mainly fill up by stopper 701 field of unstable aspect under the high temperature in use; Through consulting the at present domestic report that does not still have the related products exploitation.
Summary of the invention
Goal of the invention of the present invention provides a kind of manufacturing process that adopts one kettle way to make stopper 708, fills up in the industry blank with this.
For finishing the foregoing invention purpose, the present invention is achieved in that a kind of manufacturing process of stopper 708, it is characterized in that: method is,
(1) with stopper 701 and potassium hydroxide in molar ratio 1:1 carry out proportioning;
(2) solvent toluene is pressed 4 times of addings of the weight of stopper 701, stirred 1 hour, (3) are warmed up between 105 ℃-110 ℃, reflux dewatering, about 1 hour;
(4) be cooled to 80 ℃;
(5) drip the 1-n-butyl bromide, in 100 ℃-106 ℃, reacted 4 hours;
(6) control in the sampling, stopper 701 residual quantities are qualified less than 1%, filter, 90 ℃ of precipitations get product.
Make by technique scheme, product yield can reach 90%-97%.
Stopper 708 manufacturing process adopt one kettle way, adopt the solid catalyst one kettle way can effectively improve reaction efficiency.Through combining with actual production: polystep reaction before replacing, adopt solid alkali to replace liquid catalyst in addition.Main cleaner production, upgrading synergy.
Technique scheme is done further to improve, in the 3rd step, be warming up to 105 ℃ or 106 ℃, reflux dewatering, about 1 hour.
Description of drawings
Fig. 1 is stopper 701 reaction mechanism figure.
Embodiment
Specific embodiment 1
Stopper 701 and potassium hydroxide is 1:1 in molar ratio, and solvent toluene is pressed 4 times of addings of the weight of stopper 701, stirs 1 hour, be warming up to 105 ℃, reflux dewatering, about 1 hour, be cooled to 80 ℃, drip the 1-n-butyl bromide, in about 100 ℃, reacted 4 hours, control in the sampling, stopper 701 residual quantities are qualified less than 1%, filter, and 90 ℃ of precipitations get product; Yield 97%.
Specific embodiment 2
Stopper 701 and potassium hydroxide is 1:1.1 in molar ratio, and solvent toluene is pressed 4 times of addings of the weight of stopper 701, stirs 1 hour, be warming up to 110 ℃, reflux dewatering, about 1 hour, be cooled to 80 ℃, drip the 1-n-butyl bromide, in about 106 ℃, reacted 4 hours, control in the sampling, stopper 701 residual quantities are qualified less than 1%, filter, and 90 ℃ of precipitations get product; Yield 90%.
Claims (5)
1. the manufacturing process of a stopper 708 is characterized in that: method is,
(1) with stopper 701 and potassium hydroxide in molar ratio 1:1 carry out proportioning;
(2) solvent toluene is pressed 4 times of addings of the weight of stopper 701, stirred 1 hour, (3) are warmed up between 105 ℃-110 ℃, reflux dewatering, about 1 hour;
(4) be cooled to 80 ℃;
(5) drip the 1-n-butyl bromide, in 100 ℃-106 ℃, reacted 4 hours;
(6) control in the sampling, stopper 701 residual quantities are qualified less than 1%, filter, 90 ℃ of precipitations get product.
2. the manufacturing process of a kind of stopper 708 according to claim 1 is characterized in that: be warming up to 105 ℃, reflux dewatering, about 1 hour in the 3rd step.
3. the manufacturing process of a kind of stopper 708 according to claim 1 is characterized in that: be warming up to 110 ℃, reflux dewatering, about 1 hour in the 3rd step.
4. the manufacturing process of a kind of stopper 708 according to claim 1 is characterized in that: drip the 1-n-butyl bromide, in 100 ℃, reacted 4 hours.
5. the manufacturing process of a kind of stopper 708 according to claim 1 is characterized in that: drip the 1-n-butyl bromide, in 110 ℃, reacted 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102385822A CN103274995A (en) | 2013-06-17 | 2013-06-17 | Process for manufacturing polymerization inhibitor 708 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102385822A CN103274995A (en) | 2013-06-17 | 2013-06-17 | Process for manufacturing polymerization inhibitor 708 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103274995A true CN103274995A (en) | 2013-09-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN2013102385822A Pending CN103274995A (en) | 2013-06-17 | 2013-06-17 | Process for manufacturing polymerization inhibitor 708 |
Country Status (1)
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| CN (1) | CN103274995A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007045886A1 (en) * | 2005-10-20 | 2007-04-26 | A H Marks And Company Limited | Inhibition of polymerisation |
| CN101903572A (en) * | 2007-12-28 | 2010-12-01 | 日本制纸株式会社 | Process for production of cellulose nanofiber, catalyst for oxidation of cellulose, and method for oxidation of cellulose |
-
2013
- 2013-06-17 CN CN2013102385822A patent/CN103274995A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007045886A1 (en) * | 2005-10-20 | 2007-04-26 | A H Marks And Company Limited | Inhibition of polymerisation |
| CN101903572A (en) * | 2007-12-28 | 2010-12-01 | 日本制纸株式会社 | Process for production of cellulose nanofiber, catalyst for oxidation of cellulose, and method for oxidation of cellulose |
Non-Patent Citations (1)
| Title |
|---|
| JAN TRNKA ET.AL.: "A mitochondria-targeted nitroxide is reduced to its hydroxylamine by ubiquinol in mitochondria", 《FREE RADICAL BIOLOGY & MEDICINE》, vol. 44, 5 January 2008 (2008-01-05) * |
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Application publication date: 20130904 |