CN113667182A - Method for continuously producing aqueous antioxidant emulsion - Google Patents
Method for continuously producing aqueous antioxidant emulsion Download PDFInfo
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- CN113667182A CN113667182A CN202110974422.9A CN202110974422A CN113667182A CN 113667182 A CN113667182 A CN 113667182A CN 202110974422 A CN202110974422 A CN 202110974422A CN 113667182 A CN113667182 A CN 113667182A
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- C08K5/005—Stabilisers against oxidation, heat, light, ozone
Abstract
The invention discloses a method for continuously producing aqueous antioxidant emulsion, belonging to the field of fine chemical engineering. The invention utilizes a double-screw extruder to melt and blend antioxidant, adds composite emulsifier into the feeding port of the extruder, and uniformly mixes the antioxidant and the molten antioxidant under the action of the screw to form a melt blending body of the antioxidant, namely a water-in-oil antioxidant, and then adds the water-in-oil antioxidant into water to stir and disperse the antioxidant to realize phase inversion, thereby obtaining the water-based antioxidant emulsion. The invention is characterized in that no solvent is used in the whole process, and the method can be used for continuous production, does not use high-speed grinding or shearing, has low energy consumption and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a method for continuously producing aqueous antioxidant emulsion.
Background
The water-based antioxidant is a novel and environment-friendly auxiliary agent and is mainly applied to the fields of synthetic resin, rubber, water-based paint and water-based adhesives. The global demand of aqueous antioxidants is over 30 million tons/year, and with the development of large-scale petrochemical refining integrated projects, the demand of aqueous antioxidants is increasing day by day. The dispersed phase of the aqueous antioxidant is water and does not contain any harmful solvent, and the dispersed phase is antioxidant tiny particles (which can be solid phase or liquid phase), the apparent state of the antioxidant is similar to milk in daily life, and the antioxidant can be classified as aqueous dispersion or colloid. Besides environmental protection, the water-based antioxidant has the greatest advantages that the antioxidant is small in size, so that the dispersibility is easy, and the good dispersion state provides guarantee for the high antioxidant efficiency of the antioxidant.
At present, the preparation technology of the water-based antioxidant is a batch method, for example, patent CN102181072A discloses a method for preparing the water-based antioxidant, which comprises premixing various antioxidants, adding a solvent to completely dissolve the antioxidants in the solvent under a heating condition, adding an emulsifier to disperse under the action of a high-speed homogenizer, and finally preparing a water-based antioxidant emulsion.
Patent CN111909528A discloses an antioxidant emulsion which can be emulsified and stabilized at normal temperature and a preparation method thereof, wherein the process comprises the steps of mixing a composite antioxidant, an emulsifier and a solvent, dissolving the antioxidant in the solvent, adding water, stirring and dispersing, and finally preparing an antioxidant emulsion product. The preparation method of the aqueous antioxidant disclosed in patent CN102924748A also adds an organic solvent as a diluent, and adopts a high-speed shearing method for mixing. The patent CN107805320A is still a batch technology, and utilizes the dissolution equilibrium of the antioxidant in a continuous phase to prepare the aqueous antioxidant on the basis of high-speed shearing.
In addition to the preparation process of the aqueous antioxidant reported in the above patent, antioxidant powder is usually directly ground in a ball mill or a sand mill, and the like, and the method has the characteristics of long grinding time (more than 10 hours), high energy consumption, high price of used grinding consumables, and no contribution to large-scale industrial production. At present, antioxidant manufacturers at home and abroad use a batch method to produce aqueous antioxidant products, and reports on continuous antioxidant emulsion production are not seen.
Disclosure of Invention
In view of the above, the invention provides a method for continuously producing aqueous antioxidant emulsion, which can freely combine antioxidant components to realize continuous production of various antioxidant emulsion products.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for continuously producing an aqueous antioxidant emulsion comprising the steps of:
(1) uniformly mixing at least one antioxidant in a high-speed stirrer, directly adding the mixture into a double-screw extruder, and starting the double-screw extruder to melt and blend the antioxidant to obtain a molten antioxidant;
(2) adding an emulsifier into a feeding port at the tail end of a double-screw extruder, fully mixing the emulsifier with a molten antioxidant, directly adding an antioxidant paste in a water-in-oil state obtained after mixing into a stirring tank, and simultaneously adding deionized water into the stirring tank, so that the retention time of the antioxidant paste in the stirring tank is controlled to be 5-30 min, and obtaining an antioxidant emulsion after the retention time is reached.
Preferably, in the above method for continuously producing an aqueous antioxidant emulsion, the mass ratio of the antioxidant to the emulsifier is 100: (1-20).
The beneficial effects of the above technical scheme are: the whole preparation process of the aqueous antioxidant does not use any organic solvent, the continuous production is realized in the preparation process of the aqueous antioxidant, the particle size of the prepared aqueous antioxidant emulsion is small, the dispersion effect is good, and the whole process is safe, environment-friendly and efficient.
Preferably, in the method for continuously producing the aqueous antioxidant emulsion, the temperature set value of each section of the double-screw extruder is 5-20 ℃ higher than the eutectic point of the antioxidant.
The beneficial effects of the above technical scheme are: aiming at a single-component antioxidant, the eutectic point of the antioxidant is the melting point or the highest temperature of the melting range of the antioxidant; the eutectic point meeting the antioxidant means that the composite antioxidant is completely melted and fully dissolved and then is reduced to the inflection point of the suddenly increased viscosity, and the composite antioxidant can be calibrated by using a change curve of temperature and viscosity.
Preferably, in the above method for continuously producing an aqueous antioxidant emulsion, the temperature of the stirring tank is not lower than the eutectic point of the antioxidant, and if the temperature of the stirring tank is lower than the eutectic point of the antioxidant, the antioxidant paste is difficult to disperse in water, so the temperature of the stirring tank of the present invention is set to 40 to 90 ℃.
Preferably, in the above method for continuously producing the aqueous antioxidant emulsion, the speed of adding the antioxidant paste into the stirring tank and the speed of adding the deionized water into the stirring tank in the step (2) need to be set according to the solid content requirement of the final aqueous antioxidant product. The feed rate ratio of water to antioxidant paste can be determined according to the following formula: and N is 1/S-1, wherein S is the required solid content of the final aqueous antioxidant, and N is the feeding speed of water relative to the antioxidant paste. If the solid content of the final antioxidant product is required to be 50%, the adding speed of the paste antioxidant is equal to the adding speed of water; if the solid content of the final aqueous antioxidant product is required to be 40%, the adding speed of water is 1.5 times of that of the antioxidant paste; if the solid content of the final antioxidant product is required to be 25 percent, the adding speed of the water is 3 times of that of the antioxidant paste. Generally speaking, the speed of adding the antioxidant paste into the stirring tank is preferably 5 to 20 parts/min, and the speed of adding the deionized water into the stirring tank is 5 to 20 min.
Preferably, in the above method for continuously producing the aqueous antioxidant emulsion, the antioxidant is one or more of a phenolic antioxidant and a thioether antioxidant.
Preferably, in the above-mentioned one method for continuously producing the aqueous antioxidant emulsion, the antioxidant includes CPL (p-cresol and dicyclopentadiene butylated product), 1076 (n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), 1010 (pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 3114(1,3,5- (di-tert-butyl-4-hydroxybenzyl) s-triazine-2, 4,6- (1H,3H,5H) trione), GM (2-tert-butyl-6- (3-tert-butyl-5-methyl-2-hydroxyphenyl) -4-methylphenyl acrylate), antioxidant 245 (triethylene glycol ether-bis (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate), antioxidant 300(4,4 '-thiobis (6-tert-butyl-3-methylphenol)), antioxidant DLTP (didodecyl thiodipropionate), and antioxidant DSTP (3,3' -distearyl thiodipropionate).
Preferably, in the above method for continuously producing the aqueous antioxidant emulsion, the emulsifier is obtained by compounding an anionic emulsifier and a nonionic emulsifier.
The beneficial effects of the above technical scheme are: the anionic emulsifier and the nonionic emulsifier are compounded, so that electrostatic repulsion and steric hindrance between the emulsified antioxidant particles can be improved, the stability of the antioxidant emulsion is improved, and the antioxidant emulsion is not layered or separated out in the long-term storage process.
Preferably, in the above method for continuously producing the aqueous antioxidant emulsion, the anionic emulsifier is one or a mixture of several of disproportionated abietic acid soap, potassium oleate soap, sodium oleate soap, potassium ricinoleate soap, potassium fatty acid soap, potassium stearate soap, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, fatty acid polyoxyethylene ether sulfate and fatty acid polyoxyethylene ether sulfonate;
the nonionic emulsifier is one or more of polyvinyl alcohol, polyethylene glycol, isomeric tridecanol polyoxyethylene ether, castor oil and ethylene oxide polymer (such as El-20, El-40, HEL-20, HEL-40), polyethylene glycol oleate, polyethylene glycol fatty acid ester, and Tween 80.
The antioxidant and the emulsifier are matched according to the principle that HLB values are close, generally, the closer the HLB value of the composite emulsifier and the HLB value of the antioxidant is, the stronger the emulsifying capacity of the emulsifier is, and the smaller and more stable the particle size of the finally prepared aqueous antioxidant emulsion product is.
Preferably, in the above method for continuously producing an aqueous antioxidant emulsion, further comprising the step (3): discharging the antioxidant emulsion at a speed of 10-40 parts/min, cooling and packaging.
According to the technical scheme, compared with the prior art, the invention discloses a method for continuously producing the water-based antioxidant emulsion, the antioxidant is extruded and blended by a double-screw extruder, the antioxidant is changed into a melt uniform state in the process, the composite emulsifier is added at the feed port of the extruder screw to be fully mixed with the antioxidant in the extruder to form the antioxidant paste in a water-in-oil state, and the obtained antioxidant paste is added into water to be simply dispersed, so that the water-based antioxidant emulsion product can be obtained.
The method is characterized in that a double-screw extruder is used for melting the antioxidant product, the antioxidant product and an emulsifier are fully blended, the mixing of an oil phase and a water phase is realized inside the extruder, the antioxidant paste with a water-in-oil structure is prepared, then the antioxidant paste is secondarily dispersed in water, the conversion of the antioxidant paste from a water-in-oil state to an oil-in-water state is realized, and finally the water-based antioxidant product is prepared.
The whole process of the invention does not use any solvent, the process can realize continuous production, the product has small particle size, low viscosity and good emulsion stability, the method can be freely combined with the antioxidant, and the continuous production of various antioxidant emulsion products can be realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a process flow chart of the continuous method for producing the aqueous antioxidant emulsion.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention utilizes a double-screw extruder to melt and blend antioxidant, and adds composite emulsifier into the feeding port of the extruder, and the emulsifier and the antioxidant are uniformly mixed under the action of the screw to form a melt blending body of the antioxidant, namely a water-in-oil antioxidant, and then the water-in-oil antioxidant is added into water to be stirred and dispersed to realize phase inversion, so as to obtain the water-based antioxidant emulsion. The invention is characterized in that no solvent is used in the whole process, and the method can be used for continuous production, does not use high-speed grinding or shearing, has low energy consumption and is suitable for large-scale industrial production.
Example 1
(1) 311460 parts of composite antioxidant and 40 parts of antioxidant DSTP are mixed in a high-speed stirrer and then are directly added into a double-screw extruder, the temperature of each section of the double-screw extruder is set to be 110 ℃, and the double-screw extruder is started to melt and blend the antioxidant;
(2) adding 10 parts of emulsifier (containing 8 parts of disproportionated rosin acid soap, 1 part of isomeric tridecanol polyoxyethylene ether and EL-201 parts) into a feeding port at the tail end of an extruder, fully mixing the emulsifier with a molten antioxidant, directly adding an antioxidant paste obtained after mixing in a water-in-oil state into a stirring tank with stirring temperature of 60 ℃, wherein the adding speed of the antioxidant paste at the tail end of a double screw is 20 parts/min, adding deionized water into the stirring tank at the speed of 20 parts/min, and controlling the retention time of the antioxidant paste in the stirring tank to be 5min, so as to obtain an antioxidant emulsion product after the retention time is reached;
(3) discharging the prepared antioxidant emulsion product at the speed of 40 parts/min, cooling and packaging to obtain the antioxidant emulsion commodity.
Example 2
(1) Mixing 101030 parts of composite antioxidant, 107630 parts of antioxidant and 40 parts of antioxidant DLTP in a high-speed stirrer, directly adding the mixture into a double-screw extruder, setting the temperature of each section of the double-screw extruder to 90 ℃, and starting the double-screw extruder to melt and blend the antioxidant;
(2) adding 10 parts of emulsifier (containing 4 parts of potassium oleate, 3 parts of potassium fatty acid, 1 part of polyvinyl alcohol and HEL-402 parts) into a feeding port at the tail end of an extruder, fully mixing the emulsifier with a molten antioxidant, directly adding the antioxidant paste obtained after mixing in a water-in-oil state into a stirring tank with stirring temperature of 50 ℃, wherein the adding speed of the antioxidant paste at the tail end of a double screw is 15 parts/min, adding deionized water into the stirring tank at the speed of 15 parts/min, and controlling the retention time of the antioxidant paste in the stirring tank to be 5min, so as to obtain an antioxidant emulsion product after the retention time is reached;
(3) discharging the prepared antioxidant emulsion product at the speed of 30 parts/min, cooling and packaging to obtain the antioxidant emulsion commodity.
Example 3
(1) Mixing 245730 parts of a composite antioxidant, 40 parts of an antioxidant CPL and 30 parts of an antioxidant DSTP in a high-speed stirrer, and then directly adding the mixture into a double-screw extruder, setting the temperature of each section of the double-screw extruder at 90 ℃, and starting the double-screw extruder to melt and blend the antioxidant;
(2) adding 20 parts of emulsifier (10 parts of potassium stearate, 3 parts of potassium oleate, 5 parts of polyvinyl alcohol and 2 parts of polyethylene glycol stearate) into a feeding port at the tail end of an extruder, fully mixing the emulsifier with a molten antioxidant, directly adding the antioxidant paste obtained after mixing in a water-in-oil state into a stirring tank with stirring temperature of 60 ℃, wherein the adding speed of the antioxidant paste at the tail end of a double screw is 10 parts/min, adding deionized water into the stirring tank at the speed of 10 parts/min, and controlling the retention time of the antioxidant paste in the stirring tank to be 10min, so as to obtain an antioxidant emulsion product after the retention time is reached;
(3) discharging the prepared antioxidant emulsion product at the speed of 20 parts/min, cooling and packaging to obtain the antioxidant emulsion commodity.
Example 4
(1) 100 parts of a composite antioxidant CPL is directly added into a double-screw extruder after being mixed in a high-speed stirrer, the temperature of each section of the double-screw extruder is set to be 120 ℃, and the double-screw extruder is started to melt and blend the antioxidant;
(2) adding 8 parts of emulsifier (comprising 3 parts of potassium ricinoleate, 3 parts of potassium stearate, 1 part of polyvinyl alcohol and 1 part of glycol oleate) into a feeding port at the tail end of an extruder, fully mixing the emulsifier with a molten antioxidant, directly adding an antioxidant paste obtained after mixing in a water-in-oil state into a stirring tank with stirring temperature of 80 ℃, wherein the adding speed of the antioxidant paste at the tail end of a double screw is 5 parts/min, adding deionized water into the stirring tank at the speed of 5 parts/min, controlling the retention time of the antioxidant paste in the stirring tank to be 10min, and obtaining an antioxidant emulsion product after the retention time is reached;
(3) discharging the prepared antioxidant emulsion product at the speed of 10 parts/min, cooling and packaging to obtain the antioxidant emulsion commodity.
The aqueous antioxidant products obtained in the above examples were subjected to a test of average particle size and potential using a laser particle sizer (ZS90) of Marvin, a test of viscosity using a rotational viscometer (LVDV) of Shanghai Jingtian, and a centrifugal test of 3000rpm for 30min using a high speed centrifuge of Shanghai centrifuge research, and the results are shown in Table 1 below.
Table 1 examples 1-4 sample test results
| Sample name | Average particle diameter (nm) | Zeta potential (mV) | Viscosity (CPS) | Centrifugal stability |
| Example 1 | 247 | -43 | 280 | Not delaminating |
| Example 2 | 265 | -39 | 189 | Not delaminating |
| Example 3 | 207 | -30 | 190 | Not delaminating |
| Example 4 | 318 | -52 | 210 | Not delaminating |
Comparative example 1
Preparing a water-based antioxidant product according to the formula composition of the embodiment 3 by the method disclosed in CN111909528A, wherein the particle size of the obtained water-based antioxidant emulsion is 1.2-4 um, and the emulsion is proved to have general stability by the phenomenon of layering after centrifugation.
Comparative example 2
Grinding and emulsifying the antioxidant and the emulsifier in the embodiment 4 by a sand mill for 12 hours, wherein the formula composition and other steps are the same as those in the embodiment 4, finally obtaining the aqueous antioxidant emulsion with the particle size of 560nm, and the layering phenomenon appears after centrifugation, thus proving that the emulsion stability is general.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the scheme disclosed by the embodiment, the scheme corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for continuously producing aqueous antioxidant emulsion is characterized by comprising the following steps:
(1) uniformly mixing at least one antioxidant in a high-speed stirrer, directly adding the mixture into a double-screw extruder, and starting the double-screw extruder to melt and blend the antioxidant to obtain a molten antioxidant;
(2) adding an emulsifier into a feeding port at the tail end of a double-screw extruder, fully mixing the emulsifier with a molten antioxidant, directly adding an antioxidant paste in a water-in-oil state obtained after mixing into a stirring tank, and simultaneously adding deionized water into the stirring tank, so that the retention time of the antioxidant paste in the stirring tank is controlled to be 5-30 min, and obtaining an antioxidant emulsion after the retention time is reached.
2. The method for continuously producing the aqueous antioxidant emulsion as claimed in claim 1, wherein the mass ratio of the antioxidant to the emulsifier is 100: (1-20).
3. The method for continuously producing the aqueous antioxidant emulsion as claimed in claim 1, wherein the temperature setting value of each section of the twin-screw extruder is 5-20 ℃ higher than the eutectic point of the antioxidant.
4. The method for continuously producing the aqueous antioxidant emulsion as claimed in claim 1, wherein the temperature of the stirring tank is 40-90 ℃.
5. The method for continuously producing the aqueous antioxidant emulsion as claimed in claim 1, wherein the antioxidant is one or more of a phenolic antioxidant and a thioether antioxidant.
6. The method for continuously producing the aqueous antioxidant emulsion as claimed in claim 1, wherein the antioxidant comprises CPL, 1076, 1010, 3114, GM, 245, 300, DLTP and DSTP.
7. The method for continuously producing the aqueous antioxidant emulsion as claimed in claim 1, wherein the emulsifier is obtained by compounding an anionic emulsifier and a nonionic emulsifier.
8. The method for continuously producing an aqueous antioxidant emulsion as claimed in claim 7, wherein the anionic emulsifier is one or more selected from disproportionated abietic acid soap, potassium oleate soap, sodium oleate soap, potassium ricinoleate soap, potassium fatty acid soap, potassium stearate soap, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, fatty acid polyoxyethylene vinyl ether sulfate and fatty acid polyoxyethylene vinyl ether sulfonate;
the non-ionic emulsifier is one or more of polyvinyl alcohol, polyethylene glycol, isomeric tridecanol polyoxyethylene ether, castor oil and ethylene oxide polymer, polyethylene glycol oleate, polyethylene glycol fatty acid ester and tween 80.
9. The method for continuously producing an aqueous antioxidant emulsion as claimed in any one of claims 1 to 8, further comprising the step (3): discharging the antioxidant emulsion at a speed of 10-40 parts/min, cooling and packaging.
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| CN114790140A (en) * | 2022-04-01 | 2022-07-26 | 陕西艾科莱特新材料有限公司 | Continuous preparation method of antioxidant 1076 |
| WO2022222746A1 (en) * | 2021-04-22 | 2022-10-27 | 天津利安隆新材料股份有限公司 | Aqueous antioxidant emulsion, preparation method therefor, and application thereof |
| CN116854564A (en) * | 2023-07-06 | 2023-10-10 | 吉林市合润化工有限责任公司 | Method for continuously producing aqueous antioxidant emulsion |
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| CN116854564A (en) * | 2023-07-06 | 2023-10-10 | 吉林市合润化工有限责任公司 | Method for continuously producing aqueous antioxidant emulsion |
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Effective date of registration: 20230724 Address after: 750300 Bayin OBO Industrial Park, WUSITAI Town, Alxa League economic and Technological Development Zone, Inner Mongolia Autonomous Region Patentee after: Inner Mongolia Haopu Technology Co.,Ltd. Address before: No. 2055, Yan'an street, Changchun City, Jilin Province Patentee before: Changchun University of Technology |