CN111040189A - Fischer-Tropsch wax emulsion and preparation method thereof - Google Patents

Fischer-Tropsch wax emulsion and preparation method thereof Download PDF

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Publication number
CN111040189A
CN111040189A CN201911309877.8A CN201911309877A CN111040189A CN 111040189 A CN111040189 A CN 111040189A CN 201911309877 A CN201911309877 A CN 201911309877A CN 111040189 A CN111040189 A CN 111040189A
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fischer
tropsch wax
emulsifier
wax emulsion
deionized water
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CN111040189B (en
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魏焕曹
许兆坤
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Guangdong Agile Manufacturing Chemical Co ltd
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Guangdong Agile Manufacturing Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2391/00Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C08J2391/06Waxes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02Homopolymers or copolymers of unsaturated alcohols
    • C08J2429/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Colloid Chemistry (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention relates to a Fischer-Tropsch wax emulsion and a preparation method thereof, belonging to the field of chemical industry. The Fischer-Tropsch wax emulsion provided by the invention comprises the following components in percentage by weight: 20-30% of Fischer-Tropsch wax, 15-20% of emulsifier, 2-6% of high molecular amphoteric surfactant, 0.2-0.6% of polyvinyl alcohol and the balance of deionized water. The Fischer-Tropsch wax emulsion provided by the invention is a milky white liquid with blue light in appearance, is easy to emulsify and has high storage stability, and the storage stability at room temperature exceeds 12 months.

Description

Fischer-Tropsch wax emulsion and preparation method thereof
Technical Field
The invention relates to a Fischer-Tropsch wax emulsion and a preparation method thereof, belonging to the field of chemical industry.
Background
The Fischer-Tropsch wax comprises the main component C21-C86The content of normal alkane is about 90%, and the contents of sulfur, nitrogen and aromatic hydrocarbon are lower. Compared with paraffin, the Fischer-Tropsch wax does not contain components such as benzene, aromatic hydrocarbon, polycyclic aromatic hydrocarbon and the like, and the indexes such as environmental protection performance, electrical performance and the like of the Fischer-Tropsch wax are superior to those of the paraffin. The Fischer-Tropsch wax raw material is not influenced by the price and the production place of petroleum, has stable quality and price, and is widely applied to textiles, coatings, printing ink, food packaging and cosmetics. However, Fischer-Tropsch waxes are more difficult to emulsify than paraffin waxes, and thus limit the range of applications of Fischer-Tropsch waxes.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a Fischer-Tropsch wax emulsion which is easy to emulsify and has high storage stability.
It is another object of the present invention to provide a process for the preparation of the above fischer-tropsch wax emulsion.
The Fischer-Tropsch wax emulsion which is easy to emulsify and has high storage stability is obtained by using the macromolecular amphoteric surfactant and the low molecular weight polyvinyl alcohol (PVA) and then assisting the nonionic emulsifier.
In order to achieve the purpose, the invention adopts the technical scheme that: the Fischer-Tropsch wax emulsion comprises the following components in percentage by weight: 20-30% of Fischer-Tropsch wax, 15-20% of emulsifier, 2-6% of high molecular amphoteric surfactant, 0.2-0.6% of polyvinyl alcohol and the balance of deionized water.
Preferably, the emulsifiers include emulsifier AEO-3, emulsifier O-30 and emulsifier LA-80.
Preferably, the weight ratio of the emulsifier AEO-3, the emulsifier O-30 and the emulsifier LA-80 is 3:3: 4.
Preferably, the emulsifiers include the emulsifiers AEO-3, emulsifier O-30 and emulsifier LA-100.
Preferably, the weight ratio of the emulsifier AEO-3, the emulsifier O-30 and the emulsifier LA-100 is 3:3: 4.
Preferably, the preparation method of the macromolecular amphoteric surfactant comprises the following steps: mixing a macromonomer, acrylic acid, diethylaminoethyl acrylate, ammonium persulfate and water to obtain an aqueous solution, introducing nitrogen, polymerizing for 12 hours at a constant temperature of 60 ℃ to obtain a light yellow transparent viscous body, wherein the viscosity of the viscous body is 2000mpa.s at 25 ℃, and the high molecular amphoteric surfactant is obtained; wherein, the structural general formula of the macromonomer is: r1O(CH2CH2O)nCH2CH(OH)R2Wherein: r1Is straight chain C9~C15Alkyl, n is 3-15; r2Is CH2CH2CH=CH2、CH2CH=CH2、CH=CH2、CH2OCH2CH=CH2、CH2OCH= CH2Or OCH ═ CH2
Preferably, the polyvinyl alcohol has an alcoholysis degree of 88 and a viscosity of less than 10 cp.
Preferably, the melting point of the fischer-tropsch wax is 85 ℃.
The invention provides a preparation method of Fischer-Tropsch wax emulsion, which comprises the following steps:
(1) weighing the components according to the proportion, adding Fischer-Tropsch wax, an emulsifier, a high molecular amphoteric surfactant and polyvinyl alcohol into a container with a heating and stirring device, heating to 100 ℃, uniformly stirring, and keeping the temperature for 60min to obtain a mixture;
(2) and (2) heating deionized water to 100 ℃, taking a quarter of water amount, slowly adding the water amount into the mixture in the step (1), keeping the temperature at 95-100 ℃ and stirring for 60min, taking a quarter of 100 ℃ deionized water, repeating the step of keeping the temperature and stirring until the deionized water is completely added, keeping the temperature and stirring for 60min, and continuously stirring until the mixture is naturally cooled to obtain the Fischer-Tropsch wax emulsion.
Compared with the prior art, the invention has the beneficial effects that: the Fischer-Tropsch wax emulsion provided by the invention is a milky white liquid with blue light in appearance, is easy to emulsify and has high storage stability, the storage stability at room temperature exceeds 12 months, and the Fischer-Tropsch wax emulsion is still stable after being centrifuged for more than 30min on a centrifuge with the rotating speed of 3000 revolutions per minute.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
In this embodiment, the fischer-tropsch wax emulsion provided by the invention comprises the following components in percentage by weight: 20 percent of Fischer-Tropsch wax, 4.5 percent of emulsifier AEO-3, 4.5 percent of emulsifier O-30, 6 percent of LA-80, 2 percent of macromolecular amphoteric surfactant, 0.2 percent of polyvinyl alcohol (PVA) and 62.8 percent of deionized water in balance.
The preparation method of the Fischer-Tropsch wax emulsion comprises the following steps: adding 20% of Fischer-Tropsch wax (melting point 85 ℃), 4.5% of emulsifier AEO-3, 4.5% of emulsifier O-30, 6% of LA-80, 2% of high-molecular amphoteric surfactant and 0.2% of PVA into a four-neck flask with a heating and stirring device, heating to 100 ℃, uniformly stirring, preserving heat for 60min, heating 62.8% of deionized water to 100 ℃, taking a quarter of water amount, slowly adding the water amount into the uniformly stirred mixture, preserving heat and stirring at 95 ℃ for 60min, taking a quarter of 100 ℃ of deionized water, repeating the steps until the deionized water is completely added, preserving heat and stirring for 60min, continuously stirring until natural cooling, and obtaining a milky Fischer-Tropsch wax liquid with blue light, wherein the concentration is 38%;
the preparation method of the 2% high-molecular amphoteric surfactant comprises the following steps: mixing 50% of macromolecular monomer, 10% of acrylic acid, 10% of diethylaminoethyl acrylate, 10% of ammonium persulfate and water by weight percentage to obtain an aqueous solution, then introducing 20% of nitrogen, and polymerizing at the constant temperature of 60 ℃ for 12 hours to obtain a light yellow transparent viscous body, wherein the viscosity of the viscous body at the temperature of 25 ℃ is 2000mpa.s, and the macromolecular amphoteric surfactant is obtained; wherein, the general structural formula of the macromolecule monomer is as follows: r1O(CH2CH2O)nCH2CH(OH)R2Wherein: r1Is straight chain C9~C15Alkyl, n is 3-15; r2Is CH2CH2CH=CH2、CH2CH=CH2、CH=CH2、CH2OCH2CH =CH2、CH2OCH=CH2Or OCH ═ CH2
The Fischer-Tropsch wax emulsion described in this example was stable for twelve months at room temperature.
Example 2
In this embodiment, the fischer-tropsch wax emulsion provided by the invention comprises the following components in percentage by weight: 30 percent of Fischer-Tropsch wax, 5.4 percent of emulsifier AEO-3, 5.4 percent of emulsifier O-30, 7.2 percent of LA-100, 6 percent of macromolecular amphoteric surfactant, 0.6 percent of polyvinyl alcohol (PVA) and the balance of 45.4 percent of deionized water.
The preparation method of the Fischer-Tropsch wax emulsion comprises the following steps: adding 30% Fischer-Tropsch wax (melting point 85 ℃), 5.4% emulsifier AEO-3, 5.4% emulsifier O-30, 7.2% LA-100, 6% macromolecular amphoteric surfactant and 0.6% PVA into a four-neck flask with a heating and stirring device, heating to 100 ℃, uniformly stirring, preserving heat for 60min, heating 45.4% deionized water to 100 ℃, taking a quarter of water, slowly adding the water into the uniformly stirred mixture, preserving heat and stirring at 100 ℃ for 60min, taking a quarter of 100 ℃ deionized water, repeating the steps until the deionized water is completely added, preserving heat and stirring for 60min, and continuously stirring until natural cooling to obtain the milky Fischer-Tropsch wax liquid with blue light, wherein the concentration is 50%.
The preparation method of the 6% macromolecular amphoteric surfactant comprises the following steps: mixing 5% of macromolecular monomer, 30% of acrylic acid, 30% of diethylaminoethyl acrylate, 30% of ammonium persulfate and water into an aqueous solution in percentage by weight, then introducing 5% of nitrogen, and polymerizing at the constant temperature of 60 ℃ for 12 hours to obtain a light yellow transparent viscous body, wherein the viscosity of the viscous body at the temperature of 25 ℃ is 2000mpa.s, and the macromolecular amphoteric surfactant is obtained; wherein, the general structural formula of the macromolecule monomer is as follows: r1O(CH2CH2O)nCH2CH(OH)R2Wherein: r1Is straight chain C9~C15Alkyl, n is 3-15; r2Is CH2CH2CH=CH2、CH2CH=CH2、CH=CH2、CH2OCH2CH =CH2、CH2OCH=CH2Or OCH ═ CH2
The Fischer-Tropsch wax emulsion of the embodiment is centrifuged for more than 30min on a centrifuge with the rotating speed of 3000 r/min, and is still stable.
Example 3
In this embodiment, the fischer-tropsch wax emulsion provided by the invention comprises the following components in percentage by weight: 25% of Fischer-Tropsch wax, 6% of emulsifier AEO-3, 6% of emulsifier O-30, 8% of LA-80, 4% of high molecular amphoteric surfactant, 0.4% of polyvinyl alcohol (PVA) and 50.6% of deionized water.
The preparation method of the Fischer-Tropsch wax emulsion comprises the following steps: adding 25% of Fischer-Tropsch wax (melting point 85 ℃), 6% of emulsifier AEO-3, 6% of emulsifier O-30, 8% of LA-100, 4% of macromolecular amphoteric surfactant and 0.4% of PVA into a four-neck flask with a heating and stirring device, heating to 100 ℃, uniformly stirring, preserving heat for 60min, heating 50.6% of deionized water to 100 ℃, taking a quarter of water, slowly adding the water into the uniformly stirred mixture, preserving heat and stirring at 100 ℃ for 60min, taking a quarter of 100 ℃ of deionized water, repeating the steps until the deionized water is completely added, preserving heat and stirring for 60min, and continuously stirring until natural cooling to obtain a milky Fischer-Tropsch wax emulsion with blue light, wherein the concentration is 50%.
The preparation method of the 4% macromolecular amphoteric surfactant comprises the following steps: mixing 9% of macromolecular monomer, 30% of acrylic acid, 30% of diethylaminoethyl acrylate, 30% of ammonium persulfate and water into 30% of aqueous solution by weight percentage, then introducing 1% of nitrogen, and polymerizing at the constant temperature of 60 ℃ for 12 hours to obtain a light yellow transparent viscous body, wherein the viscosity of the viscous body at the temperature of 25 ℃ is 2000mpa.s, and the macromolecular amphoteric surfactant is obtained; wherein, the general structural formula of the macromolecule monomer is as follows: r1O(CH2CH2O)nCH2CH(OH)R2Wherein: r1Is straight chain C9~C15Alkyl, n is 3-15; r2Is CH2CH2CH=CH2、CH2CH=CH2、CH=CH2、CH2OCH2CH =CH2、CH2OCH=CH2Or OCH ═ CH2
The Fischer-Tropsch wax emulsion described in this example was stable for twelve months at room temperature.
Comparative example 1
The Fischer-Tropsch wax emulsion comprises the following components in percentage by weight: 20% of Fischer-Tropsch wax, 4.5% of emulsifier AEO-3, 4.5% of emulsifier O-30, 6% of LA-80, 0.2% of polyvinyl alcohol (PVA) and the balance of 64.8% of deionized water.
The preparation method of the Fischer-Tropsch wax emulsion is the same as that of the example 1.
Experimental example 1
The Fischer-Tropsch wax emulsions prepared in example 1 and comparative example 1 were subjected to storage stability tests
The test results show that the Fischer-Tropsch wax emulsion described in example 1 is stable for twelve months at room temperature, while the Fischer-Tropsch wax emulsion described in comparative example 1, which does not contain a polymeric surfactant, can be separated when stored at room temperature for 10 days.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (9)

1. The Fischer-Tropsch wax emulsion is characterized by comprising the following components in percentage by weight: 20-30% of Fischer-Tropsch wax, 15-20% of emulsifier, 2-6% of high molecular amphoteric surfactant, 0.2-0.6% of polyvinyl alcohol and the balance of deionized water.
2. A fischer-tropsch wax emulsion according to claim 1, wherein the emulsifiers comprise emulsifier AEO-3, emulsifier O-30 and emulsifier LA-80.
3. A fischer-tropsch wax emulsion according to claim 2, wherein the weight ratio of emulsifier AEO-3, emulsifier O-30 to emulsifier LA-80 is 3:3: 4.
4. A fischer-tropsch wax emulsion according to claim 1, wherein the emulsifiers comprise emulsifiers AEO-3, emulsifiers O-30 and emulsifiers LA-100.
5. A Fischer-Tropsch wax emulsion according to claim 4, wherein the weight ratio of the emulsifier AEO-3, the emulsifier O-30 and the emulsifier LA-100 is 3:3: 4.
6. The Fischer-Tropsch wax emulsion of claim 1, wherein the emulsion is a liquid emulsion of a Fischer-Tropsch waxThe preparation method of the macromolecular amphoteric surfactant comprises the following steps: mixing a macromonomer, acrylic acid, diethylaminoethyl acrylate, ammonium persulfate and water to obtain an aqueous solution, introducing nitrogen, polymerizing at a constant temperature of 60 ℃ for 12 hours to obtain a light yellow transparent viscous body, wherein the viscosity of the viscous body at 25 ℃ is 2000mpa.s, and the high-molecular amphoteric surfactant is obtained; wherein, the structural general formula of the macromonomer is: r1O(CH2CH2O)nCH2CH(OH)R2Wherein: r1Is straight chain C9~C15Alkyl, n is 3-15; r2Is CH2CH2CH=CH2、CH2CH=CH2、CH=CH2、CH2OCH2CH=CH2、CH2OCH=CH2Or OCH ═ CH2
7. A fischer-tropsch wax emulsion as claimed in claim 1, wherein the polyvinyl alcohol has an alcoholysis degree of 88 and a viscosity of less than 10 cp.
8. A fischer-tropsch wax emulsion according to claim 1, wherein the fischer-tropsch wax has a melting point of 85 ℃.
9. A process for the preparation of a Fischer-Tropsch wax emulsion according to any one of claims 1 to 8, comprising the steps of:
(1) weighing the components according to the proportion, adding Fischer-Tropsch wax, an emulsifier, a high molecular amphoteric surfactant and polyvinyl alcohol into a container with a heating and stirring device, heating to 100 ℃, uniformly stirring, and keeping the temperature for 60min to obtain a mixture;
(2) heating deionized water to 100 ℃, adding one fourth of water into the mixture in the step (1), keeping the temperature at 95-100 ℃ and stirring for 60min, then taking one fourth of deionized water at 100 ℃, repeating the step of keeping the temperature and stirring until all the deionized water is added, keeping the temperature and stirring for 60min, and continuing stirring until natural cooling to obtain the Fischer-Tropsch wax emulsion.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102553504A (en) * 2012-01-18 2012-07-11 朗盛(无锡)化工有限公司 Preparation method of emulsion, leather care emulsion, and use leather care emulsion
CN104109507A (en) * 2013-04-19 2014-10-22 3M创新有限公司 Antistatic wax
CN104961856A (en) * 2015-07-01 2015-10-07 广东灵捷制造化工有限公司 High-molecular amphoteric surfactant, preparation method and use

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102553504A (en) * 2012-01-18 2012-07-11 朗盛(无锡)化工有限公司 Preparation method of emulsion, leather care emulsion, and use leather care emulsion
CN104109507A (en) * 2013-04-19 2014-10-22 3M创新有限公司 Antistatic wax
CN104961856A (en) * 2015-07-01 2015-10-07 广东灵捷制造化工有限公司 High-molecular amphoteric surfactant, preparation method and use

Non-Patent Citations (1)

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Title
杨继生等: "《表面活性剂原理与应用》", 31 December 2012, 东南大学出版社, pages: 139 - 141 *

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