CN111116983A - Synthetic method for emulsion type antioxidant - Google Patents
Synthetic method for emulsion type antioxidant Download PDFInfo
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- CN111116983A CN111116983A CN201911237318.0A CN201911237318A CN111116983A CN 111116983 A CN111116983 A CN 111116983A CN 201911237318 A CN201911237318 A CN 201911237318A CN 111116983 A CN111116983 A CN 111116983A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/005—Stabilisers against oxidation, heat, light, ozone
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
- C08K5/3432—Six-membered rings
- C08K5/3435—Piperidines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/37—Thiols
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- Polymers & Plastics (AREA)
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- Anti-Oxidant Or Stabilizer Compositions (AREA)
Abstract
The invention discloses a synthesis method of an emulsion type antioxidant, which comprises the following steps: s1, preparing materials, namely, respectively preparing o-cresol, paraformaldehyde, piperidine, n-octylmercaptane and dimethylformamide, S2, heating and stirring, placing the prepared materials into a reaction kettle according to a proper proportion, stirring, S3, cooling, stopping stirring, cooling to room temperature, S4, carrying out primary reduced pressure distillation, and placing the reactant cooled to the room temperature into a reduced pressure distillation machine for reduced pressure distillation. According to the method for synthesizing the emulsion type antioxidant, the distilled solvent can be recovered during reduced pressure distillation, the solvent is convenient to recycle, the effects of saving resources and protecting the ecological environment are achieved, meanwhile, the auxiliary antioxidant, the surfactant, the defoaming agent, the thickening agent and water are heated to 100 ℃ and stirred, the reaction speed can be increased, the working time is saved, and the production efficiency is improved.
Description
Technical Field
The invention relates to the field of antioxidants, and in particular relates to a synthetic method of an emulsion type antioxidant.
Background
The plastic, rubber and other high molecular materials are subjected to chemical changes in structure and gradually lose the use value thereof due to the comprehensive influence of various external factors in the processes of storage, processing and use, the phenomenon is called aging of the high molecular materials, the aging process is an irreversible process which is often seen in daily life, for example, rubber products gradually lose elasticity, plastic films are brittle and broken, the viscosity of fuel oil is increased, and the like, the aging is caused by a plurality of reasons, both external effects and internal reasons are available, the life activities of all living beings on the earth are maintained by oxygen, oxidation reaction is also a source of life activity and energy, however, the oxygen can oxidize and degrade molecular chains of the high molecular polymers, the service life of the materials is shortened, and people think that an effective method is adopted to prevent or delay the oxidation and aging of the materials, the most common method is to use antioxidants, which are substances that readily react with oxygen, in a protected material such that they first react with oxygen to protect the material from or retard oxidation, which in the rubber industry is also known as antioxidants; however, the existing emulsion type antioxidant synthesis method is not beneficial to waste recovery, does not have the effects of saving resources and protecting ecology, and is not beneficial to the production speed of enterprises due to low working efficiency.
Disclosure of Invention
The invention mainly aims to provide a synthetic method for an emulsion type antioxidant, which can effectively solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
a synthetic method for an emulsion type antioxidant comprises the following steps:
s1, preparing materials, wherein the materials are o-cresol, paraformaldehyde, piperidine, n-octylmercaptane and dimethylformamide respectively;
s2, heating and stirring, namely placing the prepared materials into a reaction kettle according to a proper proportion and stirring;
s3, cooling, stopping stirring, and cooling to room temperature;
s4, carrying out primary reduced pressure distillation, putting the reactant cooled to room temperature into a reduced pressure distillation machine for reduced pressure distillation, evaporating water, piperidine, paraformaldehyde and DMF out, stopping heating after no bubbles emerge, cooling to room temperature to obtain a crude product, and simultaneously recovering the distilled solvent by using a solvent recovery machine, wherein the distilled solvent can be reused in S1;
s5, mixing and stirring, adding the reactant subjected to reduced pressure distillation into n-hexane, uniformly mixing, and fully stirring;
s6, washing, namely washing the reactant with a saturated sodium bicarbonate solution and ultrapure water in sequence;
s7, carrying out secondary reduced pressure distillation, slowly raising the temperature to evaporate cyclohexane and residual water, stopping heating and cooling to room temperature to obtain an auxiliary antioxidant, and simultaneously recovering the distilled solvent by using a solvent recovery machine;
s8, mixing and reacting, namely adding the obtained auxiliary antioxidant into a surfactant, a defoaming agent, a thickening agent and water, and placing the mixture into a reaction kettle for mixing and reacting;
and S9, testing, and testing the obtained emulsion type antioxidant.
Preferably, in step S2, the reactant is heated to 120 ℃ while stirring, and the stirring time is 5 hours.
Preferably, in step S3, the stirring at 120 ℃ is stopped for 5 hours, the stirring is continued until the temperature of the reaction product is reduced to 60 ℃, the stirring is stopped, and then the reaction product is allowed to stand and cool to room temperature.
Preferably, in step S8, the auxiliary antioxidant is added into the surfactant, the defoamer, the thickener and the water, and the mixture is placed in a reaction kettle and heated to 100 ℃, mixed and stirred for 3 hours, and then cooled to room temperature.
Preferably, the proportions of o-cresol, paraformaldehyde, piperidine, n-octylmercaptan and dimethylformamide in step S1 are 10%, 12%, 30% and 36%, respectively.
Compared with the prior art, the invention has the following beneficial effects: in the invention, during reduced pressure distillation, the distilled solvent can be recovered, the solvent is convenient to reuse, the effect of saving resources and protecting the ecological environment is achieved, and meanwhile, the auxiliary antioxidant, the surfactant, the defoaming agent, the thickening agent and water are heated to 100 ℃ for stirring, the reaction speed can be increased, the working time is saved, and the production efficiency is improved.
Drawings
FIG. 1 is a flow chart of a method for synthesizing an emulsion type antioxidant according to the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "connected," and the like are to be construed broadly, such as "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
As shown in figure 1, the synthesis method for the emulsion type antioxidant comprises the following steps:
s1, preparing materials, wherein the materials are o-cresol, paraformaldehyde, piperidine, n-octylmercaptane and dimethylformamide respectively;
s2, heating and stirring, namely placing the prepared materials into a reaction kettle according to a proper proportion and stirring;
s3, cooling, stopping stirring, and cooling to room temperature;
s4, carrying out primary reduced pressure distillation, putting the reactant cooled to room temperature into a reduced pressure distillation machine for reduced pressure distillation, evaporating water, piperidine, paraformaldehyde and DMF out, stopping heating after no bubbles emerge, cooling to room temperature to obtain a crude product, and simultaneously recovering the distilled solvent by using a solvent recovery machine, wherein the distilled solvent can be reused in S1;
s5, mixing and stirring, adding the reactant subjected to reduced pressure distillation into n-hexane, uniformly mixing, and fully stirring;
s6, washing, namely washing the reactant with a saturated sodium bicarbonate solution and ultrapure water in sequence;
s7, carrying out secondary reduced pressure distillation, slowly raising the temperature to evaporate cyclohexane and residual water, stopping heating and cooling to room temperature to obtain an auxiliary antioxidant, and simultaneously recovering the distilled solvent by using a solvent recovery machine;
s8, mixing and reacting, namely adding the obtained auxiliary antioxidant into a surfactant, a defoaming agent, a thickening agent and water, and placing the mixture into a reaction kettle for mixing and reacting;
s9, checking, namely checking the obtained emulsion type antioxidant;
in the step S2, the reactant is heated to 120 ℃ while being stirred, and the stirring time is 5 hours; in the step S3, stirring at 120 ℃ for 5 hours, stopping heating, continuously stirring until the temperature of the reactant is reduced to 60 ℃, stopping stirring, and then standing and cooling to room temperature; in the step S8, adding the auxiliary antioxidant into the surfactant, the defoaming agent, the thickening agent and the water, placing the mixture into a reaction kettle, heating the mixture to 100 ℃, mixing and stirring the mixture for 3 hours, and then cooling the mixture to room temperature; the proportions of o-cresol, paraformaldehyde, piperidine, n-octylmercaptan and dimethylformamide in step S1 were 10%, 12%, 30% and 36%, respectively.
When in use, the o-cresol, the paraformaldehyde, the piperidine, the n-octyl mercaptan and the dimethylformamide are respectively placed into a reaction kettle according to the proportion of 10%, 12%, 30% and 36%, then the reactants are heated to 120 ℃ and stirred, the heating is stopped after the reactants are heated for 5 hours, then the stirring is continued, when the temperature of the reactants is reduced to 60 ℃, the stirring is stopped, then the reaction mixture is kept still and cooled to room temperature, then the reactants cooled to the room temperature are placed into a reduced pressure distillation machine for reduced pressure distillation, the water, the piperidine, the paraformaldehyde and the DMF are evaporated out, the heating is stopped after no bubbles are emitted, the reactants are cooled to the room temperature to obtain a crude product, and meanwhile, the solvent recovery machine is utilized to recover the distilled solvent, so that the method has the effects of saving resources and protecting the ecological environment, meanwhile, the material cost of enterprises can be saved, the practicability is higher, then n-hexane is added into reactants after reduced pressure distillation for uniform mixing, the reactants are fully stirred, the reactants are sequentially washed by saturated sodium bicarbonate solution and ultrapure water, then secondary reduced pressure distillation is carried out, cyclohexane and residual water are evaporated at a slowly increased temperature, heating and cooling are stopped to room temperature to obtain an auxiliary antioxidant, a solvent recovery machine is used for recovering the distilled solvent, the solvent can be reused, then surfactant, defoaming agent, thickening agent and water are added into the auxiliary antioxidant, the mixture is placed in a reaction kettle and heated to 100 ℃, the mixture is stirred for 3 hours, then the mixture is cooled to room temperature, an emulsion type antioxidant can be obtained, and the emulsion type antioxidant is packaged after being inspected to be qualified.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A synthetic method for an emulsion type antioxidant is characterized by comprising the following steps:
s1, preparing materials, wherein the materials are o-cresol, paraformaldehyde, piperidine, n-octylmercaptane and dimethylformamide respectively;
s2, heating and stirring, namely placing the prepared materials into a reaction kettle according to a proper proportion and stirring;
s3, cooling, stopping stirring, and cooling to room temperature;
s4, carrying out primary reduced pressure distillation, putting the reactant cooled to room temperature into a reduced pressure distillation machine for reduced pressure distillation, evaporating water, piperidine, paraformaldehyde and DMF out, stopping heating after no bubbles emerge, cooling to room temperature to obtain a crude product, and simultaneously recovering the distilled solvent by using a solvent recovery machine, wherein the distilled solvent can be reused in S1;
s5, mixing and stirring, adding the reactant subjected to reduced pressure distillation into n-hexane, uniformly mixing, and fully stirring;
s6, washing, namely washing the reactant with a saturated sodium bicarbonate solution and ultrapure water in sequence;
s7, carrying out secondary reduced pressure distillation, slowly raising the temperature to evaporate cyclohexane and residual water, stopping heating and cooling to room temperature to obtain an auxiliary antioxidant, and simultaneously recovering the distilled solvent by using a solvent recovery machine;
s8, mixing and reacting, namely adding the obtained auxiliary antioxidant into a surfactant, a defoaming agent, a thickening agent and water, and placing the mixture into a reaction kettle for mixing and reacting;
and S9, testing, and testing the obtained emulsion type antioxidant.
2. The method of claim 1, wherein the method comprises: in step S2, the reaction mixture was heated to 120 ℃ while stirring, and the stirring time was 5 hours.
3. The method of claim 1, wherein the method comprises: in the step S3, the heating is stopped when the reaction mixture is stirred at 120 ℃ for 5 hours, the stirring is continued until the temperature of the reaction mixture is reduced to 60 ℃, the stirring is stopped, and then the reaction mixture is kept standing and cooled to room temperature.
4. The method of claim 1, wherein the method comprises: in the step S8, the auxiliary antioxidant is added with the surfactant, the defoamer, the thickener and the water, and the mixture is placed in a reaction kettle and heated to 100 ℃, mixed and stirred for 3 hours, and then cooled to room temperature.
5. The method of claim 1, wherein the method comprises: the proportions of o-cresol, paraformaldehyde, piperidine, n-octylmercaptan and dimethylformamide in step S1 were 10%, 12%, 30% and 36%, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911237318.0A CN111116983A (en) | 2019-12-05 | 2019-12-05 | Synthetic method for emulsion type antioxidant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911237318.0A CN111116983A (en) | 2019-12-05 | 2019-12-05 | Synthetic method for emulsion type antioxidant |
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| CN111116983A true CN111116983A (en) | 2020-05-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909528A (en) * | 2020-06-18 | 2020-11-10 | 福建瑞森新材料股份有限公司 | Antioxidant emulsion capable of being emulsified and stabilized at normal temperature and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080081929A1 (en) * | 2006-09-29 | 2008-04-03 | Lee Hyung-Jae | Method for preparing thiomethylphenols |
| CN105418469A (en) * | 2015-11-28 | 2016-03-23 | 常州大学 | Preparation method for antioxidant 2,4-bi(n-octyl sulfur methylene)-6-methylphenol |
| CN107501143A (en) * | 2017-09-15 | 2017-12-22 | 常州大学 | A kind of preparation method of the methylphenol of antioxidant 2,4 2 (n-octylthiomethylene) 6 |
| CN112251066A (en) * | 2020-11-06 | 2021-01-22 | 南京同溧晶体材料研究院有限公司 | Mildew-proof and oxidation-resistant coating auxiliary agent and preparation process thereof |
-
2019
- 2019-12-05 CN CN201911237318.0A patent/CN111116983A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080081929A1 (en) * | 2006-09-29 | 2008-04-03 | Lee Hyung-Jae | Method for preparing thiomethylphenols |
| CN105418469A (en) * | 2015-11-28 | 2016-03-23 | 常州大学 | Preparation method for antioxidant 2,4-bi(n-octyl sulfur methylene)-6-methylphenol |
| CN107501143A (en) * | 2017-09-15 | 2017-12-22 | 常州大学 | A kind of preparation method of the methylphenol of antioxidant 2,4 2 (n-octylthiomethylene) 6 |
| CN112251066A (en) * | 2020-11-06 | 2021-01-22 | 南京同溧晶体材料研究院有限公司 | Mildew-proof and oxidation-resistant coating auxiliary agent and preparation process thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909528A (en) * | 2020-06-18 | 2020-11-10 | 福建瑞森新材料股份有限公司 | Antioxidant emulsion capable of being emulsified and stabilized at normal temperature and preparation method thereof |
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Application publication date: 20200508 |