CN114702985A - Emulsified wax based on Fischer-Tropsch bottom oil reducing and preparation method thereof - Google Patents
Emulsified wax based on Fischer-Tropsch bottom oil reducing and preparation method thereof Download PDFInfo
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- CN114702985A CN114702985A CN202210494972.5A CN202210494972A CN114702985A CN 114702985 A CN114702985 A CN 114702985A CN 202210494972 A CN202210494972 A CN 202210494972A CN 114702985 A CN114702985 A CN 114702985A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/38—Chemical modification of petroleum
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/40—Physical treatment of waxes or modified waxes, e.g. granulation, dispersion, emulsion, irradiation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1022—Fischer-Tropsch products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention provides an emulsifying wax based on Fischer-Tropsch bottom oil reducing and a preparation method thereof. The preparation method comprises the following steps: melting the Fischer-Tropsch bottom reducing oil, and then introducing ozone for reaction to obtain modified oxidized wax; mixing the modified oxidized wax and an emulsifier, and carrying out first stirring; then adding water for second stirring; and carrying out third stirring after blue light appears in the system to obtain the emulsifying wax. The Fischer-Tropsch bottom oil reducing based emulsifying wax provided by the invention is prepared by the preparation method. The preparation method of the emulsified wax based on the Fischer-Tropsch bottom oil has the advantages of controllable raw material cost, simple process and technology, excellent performance of the prepared product, realization of value-added utilization of the Fischer-Tropsch product and improvement of the economic benefit of the emulsified wax manufacturing industry. The prepared emulsifying wax has good dispersibility, high stability and wide application prospect.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to emulsified wax based on Fischer-Tropsch bottom oil reducing and a preparation method thereof.
Background
The emulsifying wax is a uniform and stable emulsion formed by dispersing wax in a water phase, has good dispersibility, is a milky uniform fluid at normal temperature, can be diluted in water at normal temperature when in use, does not need to be dissolved by an organic solvent, has the advantages of safety and stability, and is very convenient to transport and use. Therefore, the emulsifying wax is widely applied to the industries of lubrication, coating, spinning, printing ink, cosmetics and the like.
The Fischer-Tropsch bottom reducing oil is white solid at normal temperature, and mainly comprises normal paraffin and isoparaffin of C20-C50, wherein the normal paraffin content can reach 90%, and in addition, the Fischer-Tropsch bottom reducing oil also comprises weak sulfur and nitrogen components. Compared with the conventional paraffin wax refined by petroleum, the Fischer-Tropsch synthetic wax has the advantages of lower cost, higher economy, high n-alkane content of the obtained product, no aromatic hydrocarbon, polycyclic aromatic hydrocarbon and other components, solid at normal temperature and difficult emulsification, so the Fischer-Tropsch synthetic wax has some limitations in use.
Therefore, it is very important to research how to fully utilize the Fischer-Tropsch bottom oil to produce and prepare the emulsifying wax with wide practicability, realize the value-added utilization of the Fischer-Tropsch products and improve the industrial economic benefit.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of emulsified wax based on Fischer-Tropsch base oil so as to solve the problems.
The second purpose of the invention is to provide the emulsified wax based on the Fischer-Tropsch bottom oil reducing, which has high stability and good dispersibility and can be widely applied.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a preparation method of emulsified wax based on Fischer-Tropsch base oil comprises the following steps:
melting the Fischer-Tropsch bottom-reducing oil, and then introducing ozone for reaction to obtain modified oxidized wax;
mixing the modified oxidized wax and an emulsifier, and carrying out first stirring; then adding water for second stirring;
and carrying out third stirring after blue light appears in the system to obtain the emulsifying wax.
Optionally, the Fischer-Tropsch bottom reducing oil has a melting point of 70-75 ℃; the acid value of the modified oxidized wax is 29-32mgKOH/g, the ester value is 18-20mgKOH/g, and the saponification value is 48-52 mgKOH/g.
Optionally, the concentration of the ozone is 90-110mg/L, and the flow rate is 130-150 mL/min.
Optionally, the reaction temperature is 130-140 ℃, and the reaction time is 3-4 h.
Optionally, the emulsifier comprises one or more of triethanolamine oleate, Tween80, Span80 and peregal O-15;
optionally, the emulsifier accounts for 7-13% of the total mass of the system.
Optionally, the emulsifier is a mixture of peregal O-15 and Span 80;
optionally, the weight ratio of the triethanolamine oleate to the Span80 is 3:1-4: 1.
Optionally, the emulsifier has an HLB value of 8 to 15.
Optionally, the first stirring, the second stirring and the third stirring are independently performed at 80-90 ℃;
optionally, the water is added into the system for multiple times at a temperature of 80-90 ℃.
Optionally, the first stirring speed is 600r/min, the second stirring speed is 1000r/min, and the third stirring speed is 800 r/min.
The Fischer-Tropsch base oil reducing based emulsified wax is prepared by using the preparation method of the Fischer-Tropsch base oil reducing based emulsified wax.
The invention has the beneficial effects that:
the Fischer-Tropsch bottom reducing oil is subjected to non-catalytic oxidation modification to obtain the modified oxidized wax with light color, light smell and high acid value and saponification value, and then the modified oxidized wax is taken as a basic raw material, an emulsifier is adopted, and the emulsifying wax with good dispersibility is obtained by controlling the temperature and adjusting the stirring speed.
The prepared emulsifying wax is O/W type emulsifying wax, the appearance is milky liquid, the grain diameter is less than 10 mu m, and the emulsifying wax does not break emulsion, agglomerate and have good dispersibility when being mixed with water in any ratio, thereby being an emulsifying wax product with excellent performance.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
First, the present invention is explained in its entirety, specifically as follows:
the invention provides a preparation method of an emulsifying wax based on Fischer-Tropsch bottom oil reducing, which comprises the following steps: melting the Fischer-Tropsch bottom reducing oil, and then introducing ozone for reaction to obtain modified oxidized wax;
mixing the modified oxidized wax and an emulsifier, and carrying out first stirring; then adding water for second stirring;
and carrying out third stirring after blue light appears in the system to obtain the emulsifying wax.
The Fischer-Tropsch bottom reducing oil is solid at normal temperature, is melted before reacting with ozone, introduces oxygen-containing group carboxyl in a non-catalytic oxidation mode, and is subjected to oxidation modification to obtain the modified oxidized wax with light color, light smell and high acid value and saponification value, so that the hydrophilicity of the modified oxidized wax is enhanced, and the using amount of an emulsifier can be reduced as much as possible subsequently. And then, taking the modified oxidized wax as the basic wax, and adjusting the process conditions of the content ratio of the modified oxidized wax to the compound emulsifier, the emulsifying temperature, the stirring speed and the like to prepare the stable and high-dispersion emulsifying wax.
In an alternative embodiment, the Fischer-Tropsch bottoms oil has a drop melting point of from 70 to 75 ℃; the acid value of the modified oxidized wax is 29-32mgKOH/g, the ester value is 18-20mgKOH/g, and the saponification value is 48-52 mgKOH/g.
Optionally, the Fischer-Tropsch bottom oil has a dropping melting point of any value between 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃ and 75 ℃; the acid value of the modified oxidized wax can be any value among 29mgKOH/g, 30mgKOH/g, 31mgKOH/g and 32mgKOH/g, the ester value can be any value among 18mgKOH/g, 19mgKOH/g and 20mgKOH/g, and the saponification value can be any value among 48mgKOH/g, 49mgKOH/g, 50mgKOH/g, 51mgKOH/g and 52 mgKOH/g.
In an alternative embodiment, the concentration of the ozone is 90-110mg/L, and the flow rate is 130-150 mL/min.
The concentration and flow rate of ozone determine its oxidizing power, and ozone has one more active oxygen atom than common oxygen-containing gas such as air and oxygen, so that strong oxidizing property can be generated during decomposition to promote the progress of oxidation reaction. When the concentration of ozone is too low, the oxygen content in the system is low, and the chain reaction can not be normally carried out; when the concentration of ozone is too high, the strong oxidizing property of the ozone can cause the content of short-molecule paraffin in the system to increase, and the quality of the oxidized wax is influenced. Therefore, the optimization of the parameters is beneficial to further improving the reaction efficiency and optimizing the product performance.
In an alternative embodiment, the reaction is carried out at a temperature of 130 ℃ and 140 ℃ for a period of 3-4 h.
The efficiency of the reaction is affected not only by the relevant parameters of the reactants but also by the temperature and time of the reaction, which affects not only the depth of oxidation but also the quality of the product wax, so that preference for reaction time and temperature is of great practical importance.
In an alternative embodiment, the emulsifier comprises one or more of triethanolamine oleate, Tween80, Span80, peregal O-15;
optionally, the emulsifier accounts for 7-13% of the total mass of the system.
Alternatively, the percentage of emulsifier to the total mass of the system may be any value between 7%, 8%, 9%, 10%, 11%, 12% and 13%.
In an alternative embodiment, the emulsifier is a mixture of peregal O-15 and Span 80;
optionally, the mass ratio of the peregal O-15 to the Span80 is 3:1-4: 1.
Alternatively, the mass ratio of the peregal O-15 to the Span80 may be any value between 3:1, 3.2:1, 3.5:1, 3.8:1, and 4: 1.
In an alternative embodiment, the emulsifier has an HLB value of from 8 to 15.
Alternatively, the HLB value of the emulsifier may be any value between 8, 9, 10, 11, 12, 13, 14 and 15.
The emulsifier is a very key factor in the process of preparing the emulsifying wax, different emulsifiers have fixed HLB values, namely hydrophilic-lipophilic balance values, the larger the HLB value is, the stronger the hydrophilicity of the emulsifier is, and when more than two emulsifiers exist, the HLB value of the emulsifier can be calculated according to the mass fraction occupied by the two surfactants. According to the characteristics of hydrophilic groups, the emulsifier can be divided into anionic emulsifier, cationic emulsifier and nonionic emulsifier, and the nonionic emulsifier can be used together with other two types of emulsifiers in the emulsifying process. According to the invention, a proper amount of nonionic emulsifier is selected according to the HLB value of the required emulsifying wax to be matched with the cationic emulsifier for use, so that the particle size can be reduced and the emulsion stability can be improved.
In an alternative embodiment, the first stirring, the second stirring, and the third stirring are each independently performed at 80-90 ℃;
optionally, the water is added into the system for multiple times at a temperature of 80-90 ℃.
The emulsification temperature has a great influence on the emulsification effect. The temperature is too high, the molecular adsorption process is not facilitated, the stability of an interfacial film is poor, the volatilization of a water phase is aggravated near the boiling point of water, the austenite curing phenomenon is caused, and the emulsification effect is not ideal; the emulsion has poor stability due to the fact that the temperature is too low, the molecular kinetic energy of the emulsifier is small, the cohesive energy and viscosity of the system are large, the molecular motion resistance of the emulsifier is large, and small droplets cannot be fully wrapped. Combining various factors to obtain the optimal emulsification temperature of the invention.
In an alternative embodiment, the first stirring speed is 600r/min, the second stirring speed is 1000r/min and the third stirring speed is 800 r/min.
The stirring speed greatly affects the emulsification effect, the stirring is to fully mix the oil phase and the water phase, if the stirring speed is too low, the purpose of fully mixing can not be achieved, but if the stirring speed is too high, bubbles can be brought into the system, so that the system becomes a three-phase system, and the emulsion is unstable. The optimal stirring speed in each reaction process of the invention can ensure the full mixing of the oil phase and the water phase and the stability of the emulsion.
The invention also provides the emulsifying wax based on the Fischer-Tropsch bottom oil reducing, and the emulsifying wax based on the Fischer-Tropsch bottom oil reducing is prepared by the preparation method.
The preparation method provided by the invention has the advantages of low cost, simple operation, good dispersibility of the prepared emulsifying wax, high stability, light color and excellent comprehensive performance.
Example 1
The preparation method of the emulsified wax based on the Fischer-Tropsch base oil provided by the invention is used for preparing the emulsified wax based on the Fischer-Tropsch base oil, and comprises the following specific operation steps:
1. oxidation modification of Fischer-Tropsch bottom oil:
and (2) taking 20g of solid raw material Fischer-Tropsch bottom-reducing oil, heating the solid raw material Fischer-Tropsch bottom-reducing oil in a three-neck flask to melt the solid raw material, introducing ozone when the temperature is raised to 140 ℃, adjusting the concentration of the ozone to be 100mg/L, the flow to be 140mL/min and the rotating speed to be 300r/min, reacting at constant temperature for 4 hours, taking out the solid raw material Fischer-Tropsch bottom-reducing oil, cooling to room temperature to obtain the modified oxidized wax, and sealing and storing the modified oxidized wax.
The modified oxidized wax had an acid value of 31.25mgKOH/g, an ester value of 19.88mgKOH/g, and a saponification value of 51.13 mgKOH/g.
2. Emulsification:
the weight parts of the raw materials in the emulsification process are as follows: 20 parts of modified oxidized wax, 156 parts of peregal O-156 parts, 802 parts of Span (the HLB of a compound emulsifier is 11.95) and the balance of deionized water.
Taking 10g of modified oxidized wax, proportionally mixing the modified oxidized wax, peregal O-15 and Span80 according to the weight, adding the mixture into a three-neck flask, slowly heating to melt the mixture, starting stirring when the temperature rises to 90 ℃, adjusting the rotation speed to 600r/min, and stirring for 10 min;
increasing the rotation speed to 1000r/min, slowly adding 36g of deionized water at the same temperature of 90 ℃ in batches, reducing the rotation speed to 800r/min when the emulsion generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (2) performing performance test on the product generated in the steps, centrifuging at the speed of 3000rpm for 0.5h, and avoiding the phenomena of sedimentation, demulsification and the like, wherein the average particle size of the emulsifying wax is between 3 and 7 mu m, the solid content is 21 percent, the dispersibility is two levels, and the emulsifying wax can be mixed with water in any proportion and is O/W type emulsifying wax with excellent performance.
Example 2
1. Oxidation modification of Fischer-Tropsch bottom oil:
and (2) taking 20g of solid raw material Fischer-Tropsch bottom-reducing oil, heating the solid raw material Fischer-Tropsch bottom-reducing oil in a three-neck flask to melt the solid raw material, introducing ozone when the temperature is raised to 140 ℃, adjusting the concentration of the ozone to be 100mg/L, the flow to be 140mL/min and the rotating speed to be 300r/min, reacting at constant temperature for 3 hours, taking out the solid raw material Fischer-Tropsch bottom-reducing oil, cooling to room temperature to obtain the modified oxidized wax, and sealing and storing the modified oxidized wax.
The modified oxidized wax had an acid value of 29.46mgKOH/g, an ester value of 18.61mgKOH/g, and a saponification value of 48.07 mgKOH/g.
2. Emulsification:
the weight parts of the raw materials in the emulsification process are as follows: 20 parts of modified oxidized wax, 156.2 parts of peregal O-156, 801.8 parts of Span (the HLB of a compound emulsifier is 12.23), and the balance of deionized water.
Taking 10g of modified oxidized wax, proportionally mixing the modified oxidized wax, peregal O-15 and Span80 in corresponding weight, adding into a three-neck flask, slowly heating to melt the modified oxidized wax, starting stirring when the temperature rises to 80 ℃, adjusting the rotation speed to 600r/min, and stirring for 10 min;
increasing the rotation speed to 1000r/min, taking 36g of 80 ℃ isothermal deionized water, slowly adding the deionized water in batches, reducing the rotation speed to 800r/min when the emulsion generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (3) performing performance test on the product generated in the steps, centrifuging at 3000rpm for 0.5h, and having no phenomena of sedimentation, demulsification and the like, wherein the average particle size of the emulsifying wax is between 3 and 7 mu m, the solid content is 20 percent, the dispersibility is two levels, the emulsifying wax can be mixed with water in any proportion, and the emulsifying effect is ideal.
Example 3
1. Oxidation modification of Fischer-Tropsch bottom oil:
and (2) taking 20g of solid raw material Fischer-Tropsch bottom-reducing oil, heating the solid raw material Fischer-Tropsch bottom-reducing oil in a three-neck flask to melt the solid raw material, introducing ozone when the temperature is raised to 130 ℃, adjusting the concentration of the ozone to be 90mg/L, the flow to be 150mL/min and the rotating speed to be 300r/min, reacting at constant temperature for 4 hours, taking out the solid raw material Fischer-Tropsch bottom-reducing oil, cooling to room temperature to obtain the modified oxidized wax, and sealing and storing the modified oxidized wax.
The modified oxidized wax had an acid value of 30.20mgKOH/g, an ester value of 18.11mgKOH/g, and a saponification value of 48.31 mgKOH/g.
2. Emulsification:
the weight parts of the raw materials in the emulsification process are as follows: 20 parts of modified oxidized wax, 156.4 parts of peregal O-156.6 parts of Span 801.6 parts (the HLB of a compound emulsifier is 12.46) and the balance of deionized water.
Taking 10g of modified oxidized wax, proportionally mixing the modified oxidized wax, peregal O-15 and Span80 in corresponding weight, adding into a three-neck flask, slowly heating to melt the modified oxidized wax, starting stirring when the temperature rises to 90 ℃, adjusting the rotation speed to 600r/min, and stirring for 10 min;
increasing the rotation speed to 1000r/min, slowly adding 36g of deionized water at the same temperature of 90 ℃ in batches, reducing the rotation speed to 800r/min when the emulsion generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (2) performing performance test on the product generated in the steps, centrifuging at the speed of 3000rpm for 0.5h, and avoiding the phenomena of sedimentation, demulsification and the like, wherein the average particle size of the emulsifying wax is between 3 and 9 mu m, the solid content is 20 percent, the dispersibility is two levels, and the emulsifying wax can be mixed with water in any proportion and is O/W type emulsifying wax with excellent performance.
Example 4
1. Oxidation modification of Fischer-Tropsch bottom oil:
and (2) taking 20g of solid raw material Fischer-Tropsch bottom-reducing oil to be heated and melted in a three-neck flask, introducing ozone when the temperature is raised to 130 ℃, adjusting the concentration of the ozone to be 110mg/L, the flow rate to be 130mL/min and the rotation speed to be 300r/min, reacting at constant temperature for 4 hours, taking out, cooling to room temperature to obtain the modified oxidized wax, and sealing and storing.
The modified oxidized wax had an acid value of 30.40mgKOH/g, an ester value of 19.50mgKOH/g, and a saponification value of 49.90 mgKOH/g.
2. Emulsification:
the weight parts of the raw materials in the emulsification process are as follows: 20 parts of modified oxidized wax, 806 parts of Tween, 802 parts of Span (the HLB of a compound emulsifier is 12.32) and the balance of deionized water.
Taking 10g of modified oxidized wax, proportionally mixing the modified oxidized wax, Tween-80 and Span80 in corresponding weight, adding into a three-neck flask, slowly heating to melt the modified oxidized wax, starting stirring when the temperature rises to 90 ℃, adjusting the rotation speed to 600r/min, and stirring for 10 min;
increasing the rotation speed to 1000r/min, slowly adding 36g of deionized water at the same temperature of 90 ℃ in batches, reducing the rotation speed to 800r/min when the emulsion generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (3) performing performance test on the product generated in the steps, centrifuging at the speed of 3000rpm for 0.5h, and avoiding the phenomena of sedimentation, demulsification and the like, wherein the average particle size of the emulsifying wax is 4-8 mu m, the solid content is 22%, the dispersibility is two levels, and the O/W type emulsifying wax is excellent in performance.
Example 5
1. Oxidation modification of Fischer-Tropsch bottom oil:
and (2) taking 20g of solid raw material Fischer-Tropsch bottom-reducing oil, heating the solid raw material Fischer-Tropsch bottom-reducing oil in a three-neck flask to melt the solid raw material, introducing ozone when the temperature is raised to 140 ℃, adjusting the concentration of the ozone to be 90mg/L, the flow to be 150mL/min and the rotating speed to be 300r/min, reacting for 3 hours at constant temperature, taking out, cooling to room temperature to obtain the modified oxidized wax, and sealing and storing.
The acid value of the modified oxidized wax was 29.70mgKOH/g, the ester value was 19.01mgKOH/g, and the saponification value was 48.71 mgKOH/g.
2. Emulsification:
the weight parts of the raw materials in the emulsification process are as follows: 20 parts of modified oxidized wax, 8 parts of triethanolamine oleate (the HLB of an emulsifier is 12) and the balance of deionized water.
Taking 10g of modified oxidized wax, mixing the modified oxidized wax and triethanolamine oleate according to the corresponding weight in proportion, adding the mixture into a three-neck flask, slowly heating to melt the mixture, starting stirring when the temperature rises to 80 ℃, adjusting the rotating speed to 600r/min, and stirring for 10 min;
increasing the rotation speed to 1000r/min, taking 36g of 80 ℃ isothermal deionized water, slowly adding the deionized water in batches, reducing the rotation speed to 800r/min when the emulsion generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (3) performing performance test on the product generated in the steps, centrifuging at 3000rpm for 0.5h, and having no phenomena of sedimentation, demulsification and the like, wherein the average particle size of the emulsifying wax is 4-9 μm, the solid content is 21%, the dispersibility is two levels, and the emulsifying effect is good.
Comparative example 1
The comparative example adopts the Fischer-Tropsch wax as the raw material wax to develop the emulsified wax, and the raw material consists of the following components in parts by weight: 20 parts of raw material wax, 156 parts of peregal O-156 parts, 802 parts of Span (the HLB of a compound emulsifier is 11.95) and the balance of deionized water. The preparation method comprises the following steps:
1. taking 10g of raw material wax, proportionally mixing the raw material wax with corresponding weight, peregal O-15 and Span80, adding into a three-neck flask, slowly heating to melt the raw material wax, starting stirring when the temperature rises to 90 ℃, adjusting the rotation speed to 600r/min, and stirring for 10 min;
2. increasing the rotation speed to 1000r/min, slowly adding 36g of deionized water at the same temperature of 90 ℃ in batches, reducing the rotation speed to 800r/min when the system generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (3) performing performance test on the product generated in the steps, centrifuging at 3000rpm for 0.5h to generate a slight layering phenomenon, wherein the average particle size of the emulsifying wax is 8-12 mu m, the solid content is 20%, the dispersibility is four levels, and the emulsion is observed to be white emulsion at normal temperature, has fine particles and has poor comprehensive performance.
Comparative example 2
The comparative example adopts the Fischer-Tropsch wax as the raw material wax to develop the emulsified wax, and the raw material consists of the following components in parts by weight: 20 parts of raw material wax, 806 parts of Tween, 802 parts of Span (the HLB of a compound emulsifier is 11.95) and the balance of deionized water. The preparation method comprises the following steps:
1. taking 10g of raw wax, proportionally mixing the raw wax, Tween80 and Span80 in corresponding weight, adding the mixture into a three-neck flask, slowly heating to melt the mixture, starting stirring when the temperature rises to 90 ℃, adjusting the rotation speed to 600r/min, and stirring for 10 min;
2. increasing the rotation speed to 1000r/min, slowly adding 36g of deionized water at the same temperature of 90 ℃ in batches, reducing the rotation speed to 800r/min when the system generates blue light, and emulsifying at constant temperature for 40min to obtain the emulsion.
3. And (3) product testing:
and (3) performing performance test on the product generated in the steps, centrifuging at 3000rpm for 0.5h to generate layering and emulsion breaking phenomena, wherein the average particle size of the emulsifying wax is 10-15 mu m, the solid content is 22%, the dispersibility is poor, and the emulsifying effect is not ideal.
From the examples 1 to 5, the preparation method of the Fischer-Tropsch bottom oil reducing based emulsified wax provided by the invention has the advantages of simple operation process, easily available raw materials and controllable cost, and the prepared emulsified wax has the advantages of no sedimentation, no damage, good dispersibility, high stability, uniform particle size distribution, good solid content value, capability of being mixed with water in any proportion and excellent comprehensive performance.
Compared with the comparative example 1, the scheme provided by the invention firstly carries out oxidation modification on Fischer-Tropsch bottoms and then carries out emulsification under the condition that other reaction conditions are the same, the scheme provided by the comparative example 1 has no modification process, and finally the product performance difference is larger.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of emulsified wax based on Fischer-Tropsch base oil is characterized by comprising the following steps:
melting the Fischer-Tropsch bottom reducing oil, and then introducing ozone for reaction to obtain modified oxidized wax;
mixing the modified oxidized wax and an emulsifier, and carrying out first stirring; then adding water for second stirring;
and carrying out third stirring after blue light appears in the system to obtain the emulsifying wax.
2. The preparation method according to claim 1, wherein the Fischer-Tropsch base oil has a drop melting point of 70-75 ℃; the acid value of the modified oxidized wax is 29-32mgKOH/g, the ester value is 18-20mgKOH/g, and the saponification value is 48-52 mgKOH/g.
3. The method as claimed in claim 1, wherein the concentration of ozone is 90-110mg/L, and the flow rate is 130-150 mL/min.
4. The method as claimed in claim 1, wherein the reaction temperature is 130-140 ℃ and the reaction time is 3-4 h.
5. The preparation method of claim 1, wherein the emulsifier comprises one or more of triethanolamine oleate, Tween80, Span80, peregal O-15;
preferably, the emulsifier comprises 7% to 13% of the total mass of the system.
6. The method according to claim 5, wherein the emulsifier is a mixture of peregal O-15 and Span 80;
preferably, the mass ratio of the peregal O-15 to the Span80 is 3:1 to 4: 1.
7. The method according to claim 5, wherein the emulsifier has an HLB value of 8 to 15.
8. The method according to claim 1, wherein the first stirring, the second stirring and the third stirring are independently performed at 80 to 90 ℃;
preferably, the water is added to the system in several portions at a temperature of 80 to 90 ℃.
9. The method of any one of claims 1 to 8, wherein the first stirring speed is 600r/min, the second stirring speed is 1000r/min, and the third stirring speed is 800 r/min.
10. A fischer-tropsch bottoms reducing oil based emulsifying wax produced by the process of any one of claims 1 to 9.
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| GB951308A (en) * | 1959-04-09 | 1964-03-04 | Hoechst Ag | Process for the manufacture of wax-like oxidation products from solid low pressure polyolefines |
| SU878783A1 (en) * | 1979-08-06 | 1981-11-07 | Институт Химии Башкирского Филиала Ан Ссср | Method of producing modified turf or lignite wax |
| CH648045A5 (en) * | 1981-01-04 | 1985-02-28 | Zernov Vitalij S | Process for the preparation of solid, oxidised polyethylene wax |
| JP2004036029A (en) * | 2002-07-02 | 2004-02-05 | Mitsui Chemicals Inc | Wax for fiber treating agent and fiber treating agent |
| JP2004300378A (en) * | 2003-04-01 | 2004-10-28 | San Nopco Ltd | Emulsified wax dispersion |
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| GB951308A (en) * | 1959-04-09 | 1964-03-04 | Hoechst Ag | Process for the manufacture of wax-like oxidation products from solid low pressure polyolefines |
| SU878783A1 (en) * | 1979-08-06 | 1981-11-07 | Институт Химии Башкирского Филиала Ан Ссср | Method of producing modified turf or lignite wax |
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| JP2004036029A (en) * | 2002-07-02 | 2004-02-05 | Mitsui Chemicals Inc | Wax for fiber treating agent and fiber treating agent |
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