CN111909528A - Antioxidant emulsion capable of being emulsified and stabilized at normal temperature and preparation method thereof - Google Patents
Antioxidant emulsion capable of being emulsified and stabilized at normal temperature and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an antioxidant emulsion which can be emulsified and stabilized at normal temperature and a preparation method thereof, and the antioxidant emulsion comprises the following components: 1000-2000kg of deionized water, 160-600kg of first-class antioxidant, 500-1200kg of second-class antioxidant, 20-160kg of nonionic surfactant, 10-40kg of anionic surfactant, 20-80kg of cosolvent, 5-20kg of defoamer, and 5-8kg of pH regulator and antifreeze. The preparation process includes mixing surfactant with small amount of water, adding antioxidant and cosolvent into the mixture via stirring, adding the rest water, and stirring to form antioxidant emulsion. The process has no heating and no violent stirring. Low production energy consumption, good color and luster of the antioxidant emulsion and good storage stability.
Description
Technical Field
The invention relates to the technical field of antioxidant production, and particularly relates to an antioxidant emulsion capable of being emulsified and stabilized at normal temperature and a preparation method thereof.
Background
As is well known, different additives are often added to common high polymer polymers such as rubber, plastics, ABS, latex and the like in daily life in the production process to meet the service performance of products, wherein the service life and the stability of the products are more important standards for evaluating the quality of the products. In the daily use process, the materials are easy to oxidize, so that the materials have the problems of loss of luster, hardening, cracking, fading, yellowing, pulverization and the like, and the use is seriously influenced. The most effective method at present is to add various antioxidants into the materials, so as to ensure the service performance and prolong the service life of the materials. The amine antioxidants used first are environmentally harmful and easily color products due to their high toxicity, and are not suitable for light-colored products and high-end products. At present, the method for matching the phenolic antioxidant thioester and the phosphate antioxidant is mainly used in the market. However, these two antioxidants have poor compatibility, non-uniform dispersion and poor synergistic effect when they are mixed and added as powders. At present, two types of antioxidants are mainly prepared into emulsion for use.
However, most emulsion antioxidants on the market at present adopt a powder antioxidant or a compound of powder and a liquid antioxidant, then are melted into an oil phase at high temperature, and are added with an emulsifier and emulsified in water in reverse phase to form an antioxidant emulsion. The emulsions produced by this process require higher melting temperatures and require vigorous agitation due to the higher proportion of powdered antioxidant. The formed emulsion is usually separated out due to powder in the storage process, so that the problems of oil separation, sedimentation, layering and demulsification and the like occur, and the storage period is short.
Patent CN101805458A discloses an emulsion type composite antioxidant. The method comprises the steps of taking wingstay.l and DLDTP as main and auxiliary antioxidants, heating and reacting o.5-1.5 c4-c18 straight chain or branched chain alcohol or a mixture thereof under stirring of 300-400 rpm, then adding NaOH to adjust the pH value, finally adding deionized water at the rotating speed of 180-250 rpm, and naturally cooling to room temperature to obtain the emulsion. In the method, the solid thioester antioxidant DLTDP is selected as the auxiliary antioxidant, but since the wingstsy.L is solid powder with high melting point, the emulsion can be prepared only by high-temperature melting emulsification. In addition, the method is to prepare the emulsion under low-speed stirring, and the prepared emulsion has larger particle size, can increase the coagulation probability and the sedimentation speed of emulsion particles and is not beneficial to long-term storage. Patent CN106928496A discloses an anticoagulant antioxidant. The method takes high melting point phenols and thioesters as main and auxiliary antioxidants, polyoxyethylene ether as an emulsifier, and cellulose, a vegetable gum thickener, propylene glycol, an ethylene glycol antifreezing agent and a potassium fluoride anticoagulant are added. The main and auxiliary antioxidants and the emulsifier are heated and mixed evenly under the mechanical stirring, the heating temperature is 200-210 ℃, and the stirring speed is 500-3000 r/min. The method also needs to prepare the anticoagulation type emulsion by high-temperature melting and high-speed stirring dispersion, and has high requirements on equipment and high production energy consumption in large-scale production.
Therefore, it is necessary to provide an antioxidant emulsion which can be emulsified and stabilized at room temperature and a preparation method thereof to solve the above problems.
Disclosure of Invention
In order to solve the defects in the technology, the invention provides the antioxidant emulsion which can be emulsified and stabilized at normal temperature and the preparation method thereof.
The technical scheme provided by the invention is as follows: an antioxidant emulsion which can be emulsified and stabilized at normal temperature, wherein the raw materials used in the emulsion comprise the following components in parts by weight: 1000-2000kg of deionized water, 160-600kg of first-class antioxidant, 500-1200kg of second-class antioxidant, 20-160kg of nonionic surfactant, 10-40kg of anionic surfactant, 20-80kg of cosolvent, 5-20kg of defoamer, and 5-8kg of PH regulator and antifreeze;
the preparation method of the antioxidant emulsion comprises the following steps:
the method comprises the following steps: adding a second antioxidant and a small amount of cosolvent into a reaction tank, stirring uniformly, adding a first antioxidant into a mixed solution of the second antioxidant and the cosolvent, stirring uniformly, soaking for one night or 8 hours, and mixing to prepare a transparent liquid with a certain viscosity;
step two: mixing the emulsifier well, and adding a small amount of deionized water;
step three: adding the liquid antioxidant mixed in the step one into the emulsifier mixed liquid in the step two in batches, and continuously stirring to form viscous stable liquid;
step four: flushing the rest deionized water into the stabilizing solution obtained in the third step, and starting stirring;
step five: and (4) adding auxiliaries such as a defoaming agent, a pH regulator, an anti-freezing agent and the like, and continuously stirring until the stable liquid prepared in the step three is uniformly dispersed, so that the obtained emulsion is the stable antioxidant emulsion.
Preferably, the antioxidant is a phenolic antioxidant, and the antioxidant is one or more of 2- (1-methylcyclohexyl) -4-6-dimethylphenol, 2-methyl-4, 6-dinonylphenol, p-cresol and dicyclopentadiene butylated reactant.
Preferably, the two antioxidants are epoxy soybean oil and diisotridecyl thiodipropionate in different proportions.
Preferably, the nonionic surfactant in the third step is one or two or more of polysorbate, isomeric alcohol ether, isomeric polyoxyethylene ether and alkylphenol polyoxyethylene ether, and the anionic surfactant is one or two or more of alkylphenol sulfate, alkylphenol benzenesulfonate and disproportionated potassium rosinate liquid.
Preferably, the organic cosolvent is one or two of ethanol, propanol, acetone and alkyl rubber oil and the combination of the two.
Preferably, the defoaming agent is one or a combination of two or more of emulsified silicone oil, modified mineral oil, polyether modified organic silicon and polyether.
Preferably, the pH regulator is one of sodium hydroxide solution or potassium hydroxide solution with the mass fraction of 5% -10%, and the pH of the antioxidant emulsion is regulated to 8-10.
Preferably, the antifreeze is one or two of ethylene glycol and propylene glycol.
Preferably, in the fifth step, the stirring speed is set to be 20-180r/min, and the stirring time is set to be 1-2 h.
In the technical scheme, the invention provides the following technical effects and advantages:
phenols, thioesters and epoxidized soybean oil are preferably used as antioxidants, emulsion formed by emulsification has no pollution to light-colored products, and the heat aging resistance and the freezing resistance are good.
The antioxidant is dissolved in the compound liquid of the second antioxidant and the cosolvent, the aqueous solution containing the emulsifier is added in batches for multiple times, the viscosity is gradually increased after each addition, the liquid antioxidant is prepared after the viscous stable liquid is prepared, the emulsion is emulsified without high-temperature heating and violent stirring, the production energy consumption is low, the color and luster of the antioxidant emulsion are good, the heat-resistant stability and the freezing resistance are good, and the antioxidant emulsion can be stored and used for a long time.
Detailed Description
The present invention will be described in further detail below in order to enable those skilled in the art to better understand the technical solution of the present invention.
An antioxidant emulsion which can be emulsified and stabilized at normal temperature, wherein the raw materials used in the emulsion comprise the following components in parts by weight: 1000-2000kg of deionized water, 160-600kg of first-class antioxidant, 500-1200kg of second-class antioxidant, 20-160kg of nonionic surfactant, 10-40kg of anionic surfactant, 20-80kg of cosolvent, 5-20kg of defoamer, and 5-8kg of PH regulator and antifreeze;
the preparation method of the antioxidant emulsion comprises the following steps:
the method comprises the following steps: adding a second antioxidant and a small amount of cosolvent into a reaction tank, stirring uniformly, adding a first antioxidant into a mixed solution of the second antioxidant and the cosolvent, stirring uniformly, soaking for one night or 8 hours, and mixing to prepare a transparent liquid with a certain viscosity;
step two: mixing the emulsifier well, and adding a small amount of deionized water;
step three: adding the liquid antioxidant mixed in the step one into the emulsifier mixed liquid in the step two in batches, and continuously stirring to form viscous stable liquid;
step four: flushing the rest deionized water into the stabilizing solution obtained in the third step, and starting stirring;
step five: and (4) adding auxiliaries such as a defoaming agent, a pH regulator, an anti-freezing agent and the like, and continuously stirring until the stable liquid prepared in the step three is uniformly dispersed, so that the obtained emulsion is the stable antioxidant emulsion.
Further, in the above technical scheme, the antioxidant is a phenol antioxidant, and the antioxidant is one or more of 2- (1-methylcyclohexyl) -4-6-dimethylphenol, 2-methyl-4, 6-dinonylphenol, p-cresol and dicyclopentadiene butylated reactant.
Further, in the above technical scheme, the second type antioxidant is a combination of epoxidized soybean oil and diisotridecyl thiodipropionate in different proportions.
Further, in the above technical solution, in the second step, the nonionic surfactant is one or two or more of polysorbate, heterogeneous alcohol ether, heterogeneous polyoxyethylene ether and alkylphenol polyoxyethylene ether, and the anionic surfactant is one or two or more of alkylphenol sulfate, alkylphenol benzenesulfonate and disproportionated potassium rosinate solution.
Further, in the above technical scheme, the organic cosolvent is one or a combination of two or more of ethanol, propanol, acetone and alkyl rubber oil, the deionized water is boiling water, and the heating temperature is set to 95-98 ℃.
Further, in the above technical scheme, the defoaming agent is one or a combination of two or more of an emulsified silicone oil defoaming agent, a mineral oil defoaming agent, a polyether modified silicon defoaming agent and a polyether defoaming agent.
Further, in the above technical scheme, the PH regulator is a sodium hydroxide solution or a potassium hydroxide solution with a mass fraction of 5% to 10%, and the PH regulation standard is to make the PH of the antioxidant emulsion be 8 to 10.
Further, in the above technical solution, the antifreeze is one or two of ethylene glycol and propylene glycol.
Further, in the above technical scheme, in the fifth step, the stirring speed is set to be 20-180r/min, and the stirring time is set to be 1-2 h.
Example 1:
adding 80KG of ethanol cosolvent, 300KG of epoxidized soybean oil and 900KG of liquid antioxidant of thiodipropionate bis-isomeric tridecyl diester into a raw material tank, fully stirring, adding 320KG of p-cresol and dicyclopentenyl butylated product, soaking for 8h, continuously stirring at a low speed in the adding process, wherein the stirring speed is 10r/min until the p-cresol and dicyclopentenyl butylated product is completely dissolved in the second antioxidant;
adding 320kg of alkylphenol polyoxyethylene ether-10, 80kg of fatty alcohol polyoxyethylene ether sodium sulfate and 20kg of deionized water into a reaction kettle, and fully and uniformly stirring at the stirring speed of 30 r/min;
adding 16KG, 48KG, 96KG, 160KG, 320KG, 480KG and 480KG into a reaction kettle in batches into the liquid antioxidant in the raw material tank, continuously and fully stirring at the stirring speed of 30r/min, wherein the viscosity of the obtained mixed solution is more than or equal to 1000 cp;
adding 20kg of polyether modified silicon defoamer and 2000kg of boiled deionized water into a reaction kettle, and finishing the addition within 5 min;
accelerating the stirring speed, and stirring for 1h at the stirring speed of 80 r/min;
adding a sodium hydroxide solution with the mass fraction of 5% into a reaction kettle to serve as a pH regulator, and regulating the pH to 10 by using an emulsion;
and reducing the stirring speed for 5min and discharging to obtain 4000kg of stable antioxidant emulsion.
The antioxidant emulsion prepared in the embodiment has fine and uniform texture, no agglomeration, good emulsion fluidity and strong adhesion, is placed in a high-low temperature alternating box at minus 10 ℃ for 8 hours, is thawed at normal temperature for 8 hours, is placed at 50 ℃ for 8 hours at high temperature, has no substance precipitation after three cycles, does not generate oil precipitation, sedimentation and layering demulsification, does not generate phenomena of loss of gloss, hardening, cracking, fading, yellowing and pulverization after being uniformly coated and placed for a period of time on a protected object, has an oxidation induction period of 108min at 160 ℃ after being used, and has a coking time of 385min in a hot air aging test at 180 ℃, and has obvious technical progress compared with the existing similar products.
Example 2:
adding 30KG of acetone cosolvent, 200KG of epoxidized soybean oil and 400KG of liquid antioxidant, namely, thiodipropionate bis-isomeric tridecyl diester into a raw material tank, fully stirring, adding 120KG of 2- (1-methylcyclohexyl) -4-6-dimethylphenol, soaking for 8 hours, and continuously stirring at a low speed in the adding process, wherein the stirring speed is 10r/min until the p-cresol and the dicyclopentene butylated product are completely dissolved in the liquid antioxidant;
adding 20kg of polysorbate-80, 30kg of sodium fatty alcohol-polyoxyethylene ether sulfate and 10kg of deionized water into a reaction kettle, and fully and uniformly stirring at the stirring speed of 30 r/min;
adding 1.5%, 2.5%, 5%, 10%, 20%, 26% and 34% of liquid antioxidant in a raw material tank in batches in a reaction kettle, continuously and fully stirring at the stirring speed of 30r/min to obtain a mixed solution with the viscosity of more than or equal to 1000 cp;
adding 15kg of modified mineral oil defoaming agent and 775kg of boiled deionized water into a reaction kettle, and finishing the addition within 3 min;
accelerating the stirring speed, and stirring for 1h at the stirring speed of 100 r/min;
adding 5 mass percent of potassium hydroxide solution into the reaction kettle, and adjusting the pH value of the emulsion to 10;
reducing the stirring speed for 10min and discharging to obtain 1600kg of stable antioxidant emulsion.
Compared with the example 1, the antioxidant emulsion prepared in the example has the advantages of fine and uniform texture, no agglomeration, good emulsion fluidity and strong adhesion; placing the emulsion in a high-low temperature alternating box, placing for 8 hours at minus 10 ℃, unfreezing for 8 hours at normal temperature, placing for 8 hours at 50 ℃ and high temperature, and after three cycles, no sedimentation and layering demulsification appear, and a little floating oil exists; after the protected object is uniformly coated and kept still for a period of time, phenomena of loss of gloss, hardening, cracking, fading, yellowing and powdering do not occur, the antioxidant emulsion prepared in the embodiment has an oxidation induction period of 113min at 160 ℃ and a coking time of 390min measured in a hot air aging test at 180 ℃ after being used, and has obvious technical progress compared with the prior similar products.
Example 3:
adding 40KG of isopropanol cosolvent, 200KG of epoxidized soybean oil and 400KG of liquid antioxidant, namely, thiodipropionate bis-isomeric tridecyl thiodipropionate, into a raw material tank, fully stirring, then adding 160KG of 2- (1-methylcyclohexyl) -4-6-dimethylphenol, soaking for 8h, and continuously stirring at a low speed in the adding process, wherein the stirring speed is 10r/min until the p-cresol and the dicyclopentene butylated product are completely dissolved in the liquid antioxidant;
adding 60kg of polysorbate-80, 20kg of sodium fatty alcohol-polyoxyethylene ether sulfate and 10kg of deionized water into a reaction kettle, and fully and uniformly stirring at the stirring speed of 30 r/min;
adding 1.5%, 2.5%, 5%, 5%, 10%, 10%, 15%, 21%, 30% of antioxidant stabilizing solution in a raw material tank in batches in a reaction kettle, continuously and fully stirring at the stirring speed of 30r/min to obtain a mixed solution with the viscosity of more than or equal to 1000 cp;
adding 10kg of modified mineral oil defoaming agent and 1000kg of boiled deionized water into a reaction kettle, and finishing the addition within 3 min; accelerating the stirring speed, and stirring for 1h at the stirring speed of 60 r/min; adding a pH regulator into the reaction kettle, and regulating the pH value to 10 by using an emulsion;
the stirring speed is reduced for 10min, and then the materials are discharged, thus obtaining 2000kg of stable antioxidant emulsion.
Comparing examples 1 and 2, the antioxidant emulsion prepared in the example has fine and uniform texture, no agglomeration, good emulsion fluidity and strong adhesion, the emulsion is placed in a high-low temperature alternating box, is placed at minus 10 ℃ for 8 hours, is thawed at normal temperature for 8 hours, is placed at 50 ℃ for 8 hours, does not generate oil precipitation, sedimentation and layering demulsification after three cycles, does not generate phenomena of loss of gloss, hardening, cracking, fading, yellowing and chalking after uniformly coating and standing for a period of time on a protected object, the antioxidant emulsion prepared in the example has an oxidation induction period of 110min at 160 ℃ after being used, and has a coking time of 382min in a hot air aging test at 180 ℃, and compared with the existing similar products, the antioxidant emulsion has obvious technical progress.
The following table is obtained according to examples 1 to 3:
| oxidation induction period (min) | Coking time (min) | Cold and heat cycle | |
| Example 1 | 108 | 385 | Without change |
| Example 2 | 113 | 390 | Slight oil slick |
| Example 3 | 110 | 382 | Without change |
As can be seen from the above table, the raw materials in example 1 have moderate proportion, the processing is simple and convenient, the antioxidant emulsion produced by the process has better overall performance, and is most suitable for the production and preparation of the antioxidant emulsion, phenols, thioesters and epoxidized soybean oil are preferably used as the antioxidant, and the emulsion formed by emulsification has no pollution to light-colored products, good heat-resistant aging performance and good storage stability.
The method comprises the steps of dissolving a first antioxidant in a second antioxidant and cosolvent compound solution, adding an emulsifier-containing aqueous solution in batches for multiple times, gradually increasing the viscosity of the aqueous solution in each addition, preparing a viscous stable solution, and emulsifying the prepared liquid antioxidant without high-temperature heating and violent stirring, wherein the production energy consumption is low, and the antioxidant emulsion is good in color and good in storage stability.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Therefore, the above description is illustrative in nature and should not be construed as limiting the scope of the invention, which is defined by the appended claims, and any modifications, equivalents, improvements and the like, which come within the spirit and scope of the invention are intended to be embraced therein.
Claims (9)
1. An antioxidant emulsion which can be emulsified and stabilized at normal temperature is characterized in that: the used main materials comprise the following components in parts by weight: 1000-2000kg of deionized water, 160-600kg of first-class antioxidant, 500-1200kg of second-class antioxidant, 20-160kg of nonionic surfactant, 10-40kg of anionic surfactant, 20-80kg of organic cosolvent, 5-20kg of defoamer, and 5-8kg of PH regulator and antifreeze;
the preparation method of the antioxidant emulsion comprises the following steps:
the method comprises the following steps: adding a second antioxidant and a small amount of cosolvent into a reaction tank, stirring uniformly, adding a first antioxidant into a mixed solution of the second antioxidant and the cosolvent, stirring uniformly, soaking for one night or 8 hours, and mixing to prepare a transparent liquid with a certain viscosity;
step two: mixing the emulsifier well, and adding a small amount of deionized water;
step three: adding the liquid antioxidant mixed in the step one into the emulsifier mixed liquid in the step two in batches, and continuously stirring to form viscous stable liquid;
step four: flushing the rest deionized water into the stabilizing solution obtained in the third step, and starting stirring;
step five: and (4) adding auxiliaries such as a defoaming agent, a pH regulator, an anti-freezing agent and the like, and continuously stirring until the stable liquid prepared in the step three is uniformly dispersed, so that the obtained emulsion is the stable antioxidant emulsion.
2. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: the antioxidant is one or more compounds of p-cresol and dicyclopentenyl butylated product, 2- (1-methylcyclohexyl) -4-6 dimethylphenol and 2-methyl-4, 6-dinonylphenol.
3. The antioxidant emulsion as claimed in claim 2, which is stable for emulsification at room temperature, and comprises: the second antioxidant is the combination of epoxidized soybean oil and diisotridecyl thiodipropionate in different proportions.
4. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: in the second step, the nonionic surfactant is one or two or more of polysorbate, isomeric alcohol ether, isomeric polyoxyethylene ether and alkylphenol polyoxyethylene ether, and the anionic surfactant is one or two or more of alkylphenol sulfate, alkylphenol benzene sulfonate and disproportionated potassium rosinate liquid.
5. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: the organic cosolvent is one or a combination of two or more of ethanol, propanol, acetone and alkyl rubber oil.
6. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: the defoaming agent is one or a combination of two or more of an emulsified silicone oil defoaming agent, a mineral oil defoaming agent, a polyether modified silicon defoaming agent and a polyether defoaming agent.
7. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: the PH regulator is a sodium hydroxide solution or a potassium hydroxide solution with the mass fraction of 5% -10%, and the standard of PH regulation is to ensure that the PH range of the antioxidant emulsion is 8-10.
8. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: the antifreeze is one or more of ethylene glycol and propylene glycol.
9. The antioxidant emulsion as claimed in claim 1, which is stable for emulsification at room temperature, and comprises: in the fifth step, the stirring speed is set to be 20-180r/min, and the stirring time is set to be 1-2 h.
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| CN113667182A (en) * | 2021-08-24 | 2021-11-19 | 长春工业大学 | Method for continuously producing aqueous antioxidant emulsion |
| WO2023202971A1 (en) * | 2022-04-20 | 2023-10-26 | Basf Se | An aqueous antioxidant suspoemulsion and a process for preparing the same |
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