CN107523223B - Method for preparing polishing wax - Google Patents
Method for preparing polishing wax Download PDFInfo
- Publication number
- CN107523223B CN107523223B CN201710444759.2A CN201710444759A CN107523223B CN 107523223 B CN107523223 B CN 107523223B CN 201710444759 A CN201710444759 A CN 201710444759A CN 107523223 B CN107523223 B CN 107523223B
- Authority
- CN
- China
- Prior art keywords
- wax
- acid
- sweating
- oil
- antioxidant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/08—Other polishing compositions based on wax
- C09G1/10—Other polishing compositions based on wax based on mixtures of wax and natural or synthetic resin
- C09G1/12—Other polishing compositions based on wax based on mixtures of wax and natural or synthetic resin mixtures of wax and silicon-containing polycondensates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for preparing polishing wax. The method takes an F-T synthetic product as a raw material, and produces a target product through sweating and blending. On the basis of a common sweating process, an oil-soluble emulsifier and an oil-soluble acid are dissolved in a sweating raw material to serve as an oil phase material, an inorganic salt solution is used as a water phase material, sweating is carried out after emulsification, bubbles generated by the reaction of the oil-soluble acid and the inorganic salt and a salt solution are discharged to form a tiny space, a channel for discharging a liquid component is formed to facilitate the quick discharge of the liquid component, and meanwhile, the liquid component is carried by air flow through a wax layer in the sweating process to forcibly separate the solid component and the liquid component, so that a base material without a low-melting-point component is produced; the base material is then mixed with silicone oil, natural wax, solvent and other components to obtain the wax polish product. The method has the advantages of low investment of production equipment, simple production process, low operation cost, safety, energy conservation, no solvent pollution, good high-temperature resistance of wax polishing products and the like.
Description
Technical Field
The invention belongs to the technical field of production of daily chemical products, and particularly relates to a method for preparing polishing wax, in particular to a method for preparing polishing wax products suitable for various hard surfaces (floors, furniture, automobiles and the like).
Background
The glazing product mainly generates or recovers the gloss of various surfaces (floors, furniture, automobiles and the like), and has the functions of cleaning, abrasion resistance, corrosion resistance (wind and sun exposure), water resistance, high temperature resistance, ultraviolet resistance, static resistance, scratch resistance and the like.
The polishing wax can be classified into solid, paste, liquid, etc. according to different appearance forms. According to different dispersion media, the dispersion media can be divided into types such as solvent dispersion, emulsification dispersion and the like; the polishing wax comprises three main substances, namely a volatile component, a film forming component and an auxiliary component (an emulsifier, an abrasive, a thickening agent, an antioxidant, an anti-ultraviolet agent, essence and the like). The volatile components (various organic solvents for solvent dispersion products, water, alcohol and the like for emulsification dispersion products) are mainly used for improving the workability of the polishing wax and cleaning stains on the surface to be coated; the film forming component plays a role in polishing and the like. The film-forming component of the polishing wax generally includes hydrophobic substances such as wax, silicone oil, resins (polycarbonate resin, polyurethane resin, fluororesin, polyacrylate resin, etc.), and the like. The wax used for the polishing wax mainly includes petroleum wax (paraffin wax, microcrystalline wax), natural wax (beeswax, Chinese insect wax, carnauba wax, candelilla wax, montan wax, rice bran wax, etc.), synthetic wax (polyethylene wax, polypropylene wax, oxidized polyethylene wax, oxidized polypropylene wax), etc.
The hard paste body polishing wax dispersed by the solvent is used earliest, has the advantages of good brightness, gloss durability, water resistance and the like of the wiped wax film, and is widely used up to now.
Some polishing wax products can be exposed to higher environmental temperature in the using process, for example, the highest temperature of the surface of an automobile paint film coating reaches 70-80 ℃ when the automobile paint film coating is exposed to the sun in summer, if the formula contains excessive low-melting-point components, the formed wax film is easy to soften in a high-temperature environment, dust is adsorbed, the gloss of the surface of the coating is reduced, and the appearance of an article needing polishing is influenced. Various natural and synthetic waxes produce good gloss and good heat resistance, but are expensive.
Petroleum wax is a generic name for various wax products prepared from distillate oil containing wax after crude oil refining, and comprises liquid paraffin, soap wax, paraffin wax and microcrystalline wax. The paraffin is obtained by dewaxing, deoiling, refining and refining the lubricating oil fraction in crude oilFormed by the steps of, etc., generally containing C20～C50The normal paraffin, isoparaffin and small amount of naphthene, etc. components of the (C) have a melting point of 50-74 ℃. The microcrystal wax is produced by vacuum residuum through solvent deasphalting, dewaxing, deoiling, refining and forming, and is produced with C30～C60The isoparaffin and a small amount of normal paraffin and cycloparaffin, the drop melting point is usually 65-92 ℃, and the isoparaffin has a needle-shaped crystal structure which is finer than paraffin in a solid state.
In the production process of petroleum wax, dewaxing is a process of preparing cerate with oil content of about 10-30% by using crude oil fractions as raw materials. The deoiling is a process for preparing crude petroleum wax with oil content below 2% by using cerate as a raw material, and the deoiling process mainly comprises solvent deoiling and sweating deoiling. The crude petroleum wax is further treated through clay refining or hydrorefining, forming, packing and other steps to obtain the product petroleum wax.
Petroleum wax is a hydrocarbon mixture of normal paraffins, isoparaffins, naphthenes, and the like having a large number of carbon numbers, and has a wide distribution of carbon numbers, and therefore must contain a certain amount of low-melting components (oil and wax having a low melting point). The excessive use of petroleum waxes such as paraffin wax and microcrystalline wax in the polishing wax results in poor heat resistance of the polishing film.
The Fischer-Tropsch (F-T) synthesis technology is invented in 1923, mainly comprises a high-temperature synthesis technology and a low-temperature synthesis technology, F-T synthesis processes and catalysts have made breakthrough progress since the nineties of the twentieth century, and F-T synthesis products are increasingly abundant. The F-T synthetic product has the chemical composition mainly comprising normal paraffin, a small amount of isoparaffin, more olefin and oxygen-containing compounds and wide carbon number distribution. The fischer-tropsch synthesis also results in a glazing film with poor heat resistance when used directly in a glazing wax formulation because of the large amount of low melting components.
In the production process of wax products, the separation and processing means commonly used include distillation, solvent separation, sweating separation and the like.
The distillation is to utilize the different boiling points of different hydrocarbons to achieve the purpose of separation and purification, and the reduction of the boiling range of the distillation can effectively reduce the width of the carbon distribution of the product, but the distillation process needs to heat the raw material to be above the boiling point, and consumes a large amount of energy. For example, CN201410217632.3 (a method for increasing the freezing point of Fischer-Tropsch wax) describes that the raw material is subjected to high temperature and high vacuum to remove low boiling point substances, and then is further distilled and refined under extremely high vacuum to prepare high melting point wax products. Meanwhile, the boiling point of the hydrocarbon with the melting point of more than 70 ℃ is more than 500 ℃ (normal pressure), and the efficiency is greatly reduced when the distillation is adopted for separation.
The solvent separation method is to separate and purify various components in the wax by utilizing the properties of different solubilities in the solvent, such as CN200410043806.5 (a method for separating polyethylene wax) and CN201110351185.7 (a method for separating polyethylene byproduct polyethylene wax), and the obtained high-melting point polyethylene wax can be used for producing products such as polishing wax and the like. The investment of production equipment of the solvent separation process is large; a large amount of solvent is needed in the production process, and a large amount of energy is consumed for recovering the solvent; the solvent usually contains benzene series substances, which can affect the environment; the solvent is inflammable and is easy to cause production accidents.
The sweating separation method is to separate and purify by utilizing the properties of different melting points of various components in the wax. The melting points of the various components of the wax will vary depending on their molecular weights and structures. When the normal paraffin is the same as the normal paraffin, the melting point of the normal paraffin with larger molecular weight is higher, and the melting point of the normal paraffin with smaller molecular weight is lower; the same molecular weight, isoparaffins and naphthenes have lower melting points than normal paraffins, and the higher the degree of isomerization, the lower the melting point.
Compared with a distillation method, the energy consumption of the sweating separation process is far lower than that of distillation because the melting point temperature of various hydrocarbons is far lower than the boiling point temperature; compared with a solvent separation method, the sweating separation process does not use a solvent, so the sweating separation process is safe and energy-saving and has no influence on the environment.
The common sweating process mainly comprises the following steps: (1) preparation work: filling water (filling the space under the dish plate of the sweating device with water), and then loading the materials (loading the materials into the sweating device when the materials are heated to be liquid above the melting point); (2) and (3) crystallization: the raw material is slowly cooled to 10-20 ℃ below the melting point thereof at a cooling rate of not more than 4 ℃/h. In the cooling process, the components are crystallized sequentially from high to low according to the melting points to form solids; (3) sweating: when the temperature of the wax layer reaches the preset temperature reduction termination temperature, draining the padding water; the material is then slowly heated to a predetermined sweating termination temperature. During sweating, the components are sequentially melted into liquid state according to the sequence of melting point from low to high and flow out (under wax), and finally the wax layer residue (on wax) is the wax with high melting point and low oil content; (4) refining: collecting the crude product (raising the temperature continuously after the sweating process is finished to melt and take out the wax to obtain the crude product), performing clay refining (heating the crude product to a preset temperature after melting, adding clay, stirring at a constant temperature for a preset time, and filtering), and then molding and packaging to obtain the target product.
The common sweating process can produce soap wax and low-melting-point paraffin with the melting point of 40-60 ℃, and is not suitable for producing wax products with the melting point of more than 70 ℃. When the common sweating process is used for producing the soap wax and the low-melting-point paraffin wax at 40-60 ℃, the solid component (the wax with a higher melting point) and the liquid component (the oil and the wax with a lower melting point) are respectively in two phases of solid and liquid in the sweating process, but are difficult to be completely separated. In order to make the final product meet the requirements, a method of prolonging the sweating time (reducing the temperature rise speed) and increasing the sweating termination temperature is generally adopted, but the method has the disadvantages of long production period and low product yield; tests show that when a wax product with the melting point of above 70 ℃ is produced by a common sweating process, the carbon distribution width and the n-alkane content on the wax at the sweating later stage are irrelevant to the yield, namely the carbon distribution width on the wax is not reduced along with the reduction of the yield, and the n-alkane content is not improved along with the reduction of the yield, so that the report of producing the wax product with the melting point of about 70 ℃ by the sweating process is not seen so far.
Compared with solvent separation, the sweating process is intermittent operation, the product yield is low, the production period is long, but the sweating process has the advantages of low investment, simple production process, low operation cost, safe production process, energy conservation, no pollution to the environment and the like, and at present, partial manufacturers still use the method to produce the wax products for the soap.
For many years, the sweating method is developed in the aspects of equipment and processes, such as CN89214332 (vertical square multi-section partition sweating tank), CN94223980.6 (dish type sweating device), CN98233254.8 (paraffin sweating tank), CN200920033500X (novel paraffin sweating tank), CN201210508905.0 (high-efficiency paraffin sweating device), CN201320127680.4 (tubular paraffin deoiling device) and the like, and improvement is made on the sweating equipment; CN91206202 (a high-efficiency paraffin wax sweating pot) is improved in sweating process, but these improvements still cannot produce wax products with melting point above 70 ℃.
The sweating process is the only solvent-free separation method for producing wax products on an industrial scale, and nowadays when green, low carbon, environmental protection and energy conservation are advocated, people are increasingly concerned about producing high-melting-point wax products without low-melting-point substances by adopting the sweating process, and meanwhile, the requirement of reducing the production cost is more urgent while the performances such as high temperature resistance and the like of the polishing wax are not influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing polishing wax, which comprises three parts of emulsification, sweating and blending. Particularly, an F-T synthetic product with the weight content of n-alkane of more than 80 percent is taken as a sweating raw material, on the basis of a common sweating process, an oil-soluble emulsifier and an oil-soluble acid are preferably dissolved in the sweating raw material to be taken as oil phase materials, an inorganic salt solution is taken as a water phase material, the sweating is carried out after emulsification, bubbles and a salt solution generated by the reaction of the oil-soluble acid and the inorganic salt are discharged to form a tiny space, a channel for discharging a liquid component is formed to facilitate the quick discharge of the liquid component, and meanwhile, an air flow is utilized to pass through a wax layer in the sweating process to forcibly separate a solid component and the liquid component, so that the separation effect is enhanced and the separation speed is accelerated; and the constant temperature stages of the crystallization process and the sweating process are added, so that the sweating solvent-free separation method can prepare the base material without low-melting-point components; the base material is then mixed with silicone oil, natural wax, solvent and other components to obtain the wax polish product. The method has the advantages of low investment of production equipment, simple production process, low operation cost, safety, energy conservation, no solvent pollution, good high-temperature resistance of wax polishing products and the like.
The invention discloses a method for preparing polishing wax, which comprises the following steps:
(A) emulsification: the method comprises the following steps:
(A1) preparing an oil phase material: taking an F-T synthetic product with the weight content of normal alkane of more than 80 percent as a sweating raw material, adding an oil-soluble emulsifier and an oil-soluble acid after heating and melting, and uniformly stirring to form an oil phase material;
(A2) preparing a water-phase material: dissolving inorganic salt in water, and forming a water phase material with or without heating;
(A3) preparing an emulsion: adding the water phase material obtained in the step (A2) into the oil phase material obtained in the step (A1) under the stirring condition, and continuously stirring for 5-60 minutes to form an emulsion;
(B) sweating: the method comprises the following steps:
(B1) preparation work: charging the emulsion prepared in the process of (a 3) into a sweating device;
(B2) and (3) crystallization: firstly, cooling the emulsion to the melting point of the sweating raw material drop plus 4-8 ℃ at the speed of 1.0-10.0 ℃/h; then cooling the wax layer to the range of the melting point of the sweating raw material drops to the melting point of the drops plus 4 ℃ at the speed of 1.0 ℃/h-3.0 ℃/h, and keeping the temperature for a period of time; then cooling the wax layer to a cooling termination temperature of 5-30 ℃ below the melting point of the sweating raw material drop at the speed of 2.0-4.0 ℃/h;
(B3) sweating: heating at the rate of 0.5-3.5 ℃/h; stopping sweating after the wax layer reaches a preset temperature and is kept at a constant temperature for a period of time; forcing an air stream through the wax layer during sweating;
(B4) refining: refining the wax to obtain a base material for polishing the wax;
(C) blending: the base material, the silicone oil, the natural wax and the solvent are melted and mixed evenly according to the proportion, and the wax polishing product is obtained after cooling.
In the method of the present invention, the F-T synthesis product has an n-alkane content of 80% by weight or more, preferably 90% by weight or more as a sweating material.
In the method of the present invention, the sweating raw material is emulsified with the water phase material in the presence of the oil-soluble emulsifier and the oil-soluble acid, and then sweating is performed. The oil-soluble emulsifier in the step (A1) is selected from one or more of nonionic surfactant, anionic surfactant, cationic surfactant and amphoteric surfactant. The HLB value of the oil-soluble emulsifier is 1-10, preferably 3-8; the freezing point or melting point of the surfactant is lower than the highest temperature at which sweating occurs in step (B3) (i.e., the predetermined temperature). The oil-soluble emulsifier is preferably a composite emulsifier composed of more than two surfactants.
Wherein the nonionic surfactant is selected from the group consisting of sorbitan monooleate, sorbitan monostearate, diethylene glycol fatty acid ester, diethylene glycol monolaurate, sorbitan monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan monolaurate and polyoxyethylene fatty acid ester; the anionic surfactant is selected from fatty alcohol sulfate ester monoethanol amine salt, alkyl polyoxyethylene ether sodium sulfate, oleamido carboxylic acid sodium, sodium alkyl benzene sulfonate, N-methyl oleoyl taurate, butyl naphthalene sodium sulfonate, succinate sodium sulfonate, and maleic acid monoester sodium sulfonate. The cationic surfactant is selected from a group of substances consisting of benzyl quaternary ammonium salt, dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride and triethylamine oleate; the amphoteric surfactant is selected from the group consisting of dodecyl betaine, dodecyl dimethyl ammonium oxide, fatty alkyl imidazoline derivatives, fatty acid derivatives, and amphoteric modified ethylene oxide adduct.
In the method of the present invention, the oil-soluble acid in the step (a 1) is an organic acid which is soluble in the sweating raw material and can react with the inorganic salt in the step (a 2) to generate a gas. The organic acid is selected from the group consisting of n-unitary acid, n-capric acid, n-undecanoic acid, lauric acid, n-tridecanoic acid, myristic acid, n-pentadecanoic acid, palmitic acid, pearlitic acid, stearic acid, n-nonadecanoic acid, arachic acid, n-heneicosanoic acid, behenic acid, n-tricosanoic acid, lignoceric acid, n-pentacosanoic acid, cerotic acid, n-heptacosanoic acid, montanic acid, n-nonacosanoic acid, melissic acid, n-hendecanoic acid, lacca acid, phyllostic acid, linoleic acid, palmitoleic acid, oleic acid, erucic acid and scylleic acid. Preferably, the organic acid which has no special smell, no toxicity, easy obtainment, low price and melting point lower than the highest temperature in the sweating process comprises a group of substances consisting of linoleic acid, palmitoleic acid, oleic acid, erucic acid, scyloleic acid, n-capric acid, n-undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, pearly fatty acid, stearic acid, n-nonadecanoic acid, arachidic acid, n-heneicosanoic acid, behenic acid, n-tricosanic acid, lignoceric acid, n-pentacosanoic acid, cerotic acid and n-heptacosanoic acid.
In the method of the present invention, the inorganic salt in the step (a 2) is a water-soluble inorganic salt which can react with the oil-soluble acid in the step (a 1) to generate a gas. The inorganic salt is selected from one or more of carbonate, bicarbonate, sulfite and bisulfite; preferably one of the carbonates such as sodium carbonate and potassium carbonate and the mixture thereof and/or one of the bicarbonates such as sodium bicarbonate and potassium bicarbonate and the mixture thereof, which have low price, wide source, no toxicity and no pungent smell of the self and reaction products. The concentration (mass%, the same applies hereinafter) of the aqueous solution of the inorganic salt is 0.1% to 10.0%, preferably 0.5% to 5.0%.
In the method of the present invention, the composition of the emulsion obtained in step (a 3) is: 55.0 to 90.0 percent of sweating raw material, 9.8 to 29.0 percent of water phase material, 0.1 to 6.0 percent of oil-soluble emulsifier and 0.1 to 10.0 percent of oil-soluble acid. The preferred composition of the emulsion is: 66.0-83.0 percent of sweating raw material, 15.0-25.0 percent of water phase material, 1.8-4.0 percent of oil-soluble emulsifier and 0.2-5.0 percent of oil-soluble acid.
The emulsification process is conventional in the art. The conditions for emulsification are generally: mixing at 90-98 ℃ for 5-60 minutes at a stirring speed of 50-5000 revolutions per minute; preferably, the mixture is mixed for 10 to 30 minutes at a stirring speed of 100 to 1000 revolutions per minute at a temperature of 90 to 95 ℃.
In the method of the invention, in the step (B2), cooling is carried out at the speed of 1.0 ℃/h to 10.0 ℃/h to the range of the melting point of the sweating raw material drop plus 4 ℃ to the melting point of the drop plus 8 ℃; the cooling rate before the constant temperature section is preferably 1.5-2.5 ℃/h; the temperature of the constant temperature section is from the melting point of the sweating raw material drop to the dropping melting point plus 4.0 ℃. The time of the constant temperature period is 0.1 to 6.0 hours, preferably 0.5 to 5.0 hours, and more preferably 1.0 to 4.0 hours. The cooling rate after the constant temperature section is preferably 2.5 ℃/h to 3.5 ℃/h; the temperature reduction termination temperature is preferably 8-15 ℃ below the melting point of the sweating raw material drops.
In the method of the present invention, the sweating device is preferably a sweating dish, and a pressurizing device is added above the wax layer and/or a vacuum device is added below the wax layer to form a pressure difference above and below the wax layer during the step (B3). The forced airflow is realized by increasing pressure (air pressure) above the wax layer and/or reducing pressure (air pressure) below the wax layer through the wax layer to form pressure difference between the upper part and the lower part (side) of the wax layer. The pressure differential is generally between 0.1 and 5.0 atmospheres, preferably between 0.2 and 2.0 atmospheres, to force the air flow through the wax layer.
In the method of the present invention, the temperature increase rate in the step (B3) is preferably 1.0 ℃/h to 3.0 ℃/h. The predetermined temperature for the temperature increase (i.e., the termination temperature) is from-10 deg.C to the base material drop melting point. After the temperature is raised to the preset temperature, the constant temperature stage is added to enable the solid component and the liquid component to be separated more fully, and the time of the constant temperature stage is 0.1-10.0 hours, preferably 1.0-8.0 hours, and most preferably 2.0-6.0 hours.
In the method of the present invention, the temperature increasing rate and the temperature decreasing rate of the wax layer may be controlled by an air bath, a water bath, an oil bath, or other feasible means, and preferably, a water bath or an oil bath is used. When the temperature rise rate and the temperature reduction rate of the wax layer are controlled by adopting a water bath or oil bath mode, a jacket can be added outside the sweating dish, the jacket is connected with a movable coil and a circulating system, the circulating system has a programmed cooling/heating function, and substances such as water or heat conduction oil and the like are added into the circulating system to serve as circulating media; after loading, the coil pipe is immersed and fixed in the wax layer, so that the temperature rising/reducing process of the wax layer is quicker and the temperature of the wax layer is more uniform.
In the method of the present invention, the forced flow of air through the wax layer in step (B3) may be carried out at any stage of the sweating process, preferably during the initial stage of sweating.
In the method of the present invention, the forced airflow through the wax layer in the step (B3) is achieved by increasing the pressure above the wax layer, for example, a gauge pressure of 0.2 to 2.0 atm can be applied above the wax layer, and the pressure below the wax layer is kept at a normal pressure.
In the method of the present invention, the forced flow of gas through the wax layer in step (B3) is achieved by reducing the pressure of the gas below the wax layer, for example, by maintaining atmospheric pressure above the wax layer and a gauge pressure of-0.2 to-0.8 atm below the wax layer.
In the method of the present invention, in the step (C), the silicone oil is selected from one or a mixture of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen-containing silicone oil, methyl phenyl silicone oil, methyl chlorophenyl silicone oil, methyl vinyl silicone oil, methyl hydroxy silicone oil, ethyl hydrogen-containing silicone oil, and amino silicone oil. The natural wax is selected from one or mixture of beeswax, Chinese insect wax, carnauba wax, candelilla wax, montan wax, and rice bran wax. The solvent is selected from n-pentane, n-hexane, n-octane, D40, D60, D80, No. 90, No. 120, No. 180, No. 190, No. 200, Exxsol D40, Exxsol D80, Exxsol D110, Exxsol D130, Exxsol DSP80/100, benzene, toluene, xylene, cyclohexane, cyclohexanone, toluene cyclohexanone, chlorobenzene, dichlorobenzene, dichloromethane, diethyl ether, ethylene oxide, methyl acetate, ethyl acetate, propyl acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, acetone, methyl butanone, methyl isobutyl ketone, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol ethyl ether acetate, ethylene glycol ether ester, phenol, turpentine, odorless kerosene, one or a mixture thereof, preferably, nontoxic, low odor, appropriate volatility, low price, widely available D40, D60, D80, No. 90, No. 120, DSP 180, No. 190, No. 200, Exxsol D40, Exxsol D80, Exxsol D110, Exxsol D130, Exxsol D100/100, Exxsol D80, Exxsol D3982, Ex, One or a mixture of propyl acetate, dimethyl succinate and dimethyl glutarate.
In the method of the present invention, the composition of the polishing wax by mass comprises: 10.0-25.0 percent of base material, 1.0-5.0 percent of silicone oil, 4.0-10.0 percent of natural wax and 60.0-85.0 percent of solvent.
According to the requirement, more than one of antioxidant and essence can be added into the polishing wax as an additive. The addition amount of the additive calculated by the quality of the optical wax is as follows: 0.1-1.0% of antioxidant and 0.1-1.0% of essence.
In the method of the invention, substances such as antioxidant, essence and the like can be added into the polishing wax in the process (C) according to the needs. The antioxidant is selected from one or a mixture of antioxidant BHT, antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 1330, antioxidant 3114, antioxidant 164, antioxidant 168, antioxidant 264, antioxidant B215 and antioxidant B225. The proportion of each component of the polishing wax is as follows: 5.0-29.0% of base material, 0.1-6.0% of silicone oil, 1.0-15.0% of natural wax, 48.0-93.9% of solvent, 0-1.0% of antioxidant and 0-1.0% of essence; the preferred proportions are: 10.0 to 25.0 percent of base material, 1.0 to 5.0 percent of silicone oil, 4.0 to 10.0 percent of natural wax, 59.0 to 84.8 percent of solvent, 0.1 to 0.5 percent of antioxidant and 0.1 to 0.5 percent of essence.
Analysis shows that the F-T synthetic product does not contain impurities such as sulfur, nitrogen, aromatic hydrocarbon and the like, and can easily reach high purity after refining; the chemical composition of the low-temperature F-T synthetic product is mainly normal alkane, has wide distribution and contains a small amount of olefin and oxygen-containing compounds. Oxygenates have a particular odor due to the presence of olefin components which can deteriorate stability at high temperatures. The large amount of the low-melting component causes deterioration of high-temperature resistance when it is directly used as a wax polish component. The F-T synthesis product is therefore not suitable for direct use as a formulating component for a polishing wax.
The sweating separation method utilizes the property that various components have different melting points to carry out separation. Studies on the sweating process have shown that the liquid component is gradually drained along the crystalline portion during sweating, similar to the case where the liquid flows in a capillary. However, for the high melting point wax with the melting point of about 70 ℃, the chemical composition of the raw materials is complex, so that the crystal structure is fine and compact during crystallization, and huge filtration resistance is formed for discharging liquid components, so that the solid components and the liquid components are difficult to completely separate in the ordinary sweating process which naturally separates by gravity only, and therefore, the ordinary sweating separation process cannot produce wax products with the melting point of above 70 ℃.
In order to prepare a low-cost high-temperature-resistant wax polish product, the invention, through the deep research on the composition of an F-T synthetic product, aims at the reason that the F-T synthetic product contains a certain amount of olefin and oxygen-containing compounds (the melting points of the components are usually lower than 65 ℃, and the components belong to low-melting-point components), and a large amount of alkane low-melting-point components cause that the F-T synthetic product is not suitable for being directly used for blending the wax polish product, removes the non-suitable components by adopting a sweating method, and then mixes the components with silicone oil, natural wax and solvent oil to produce the wax polish product.
Through the intensive research on the common sweating process, aiming at the reason that the solid component and the liquid component are difficult to separate, forced airflow is adopted to pass through a wax layer in the sweating process, and meanwhile, the sweating raw material is preferably mixed with oil-soluble acid and oil-soluble emulsifier and then is made into W/O type emulsion with inorganic salt solution, then sweating is carried out, and a constant temperature stage is added in the crystallization and sweating processes, so that the measures effectively remove the non-suitable components such as olefin, oxygen-containing compound, low-melting-point alkane and the like in the sweating raw material, and the product is suitable to be used as the base material of the polishing wax.
Aiming at the reason that the solid component and the liquid component are difficult to separate in the sweating process, the solid component and the liquid component are forced to be separated by adopting a method that the liquid component is carried out by air flow through a wax layer in the sweating process, so that the separation effect is enhanced and the separation speed is accelerated; the wax can be crystallized more greatly by adding a constant temperature stage in the cooling process, which is beneficial to discharge liquid components in the sweating process. Studies on wax crystallization have shown that the chemical composition of wax is the most important factor in determining the crystal morphology, and the cooling process conditions also affect the crystal morphology, especially at temperatures around the dropping point. When the wax is cooled to the vicinity of the dropping point, the n-alkane with larger molecular weight forms crystals to be separated, the crystals can be used as crystal nuclei for subsequent crystal formation, and the high-temperature constant-temperature stage is increased, so that the crystal nuclei can be fully grown to form crystals with larger size, and the crystals with larger size are not as coarse as the crystals of the paraffin with low melting point, but the enlarged crystal structure is also very favorable for discharging liquid components in the sweating stage. Meanwhile, the inorganic salt solution in the emulsion is uniformly distributed in the raw material wax layer in a micro particle form; because the selected oil-soluble acid has weak acidity and is respectively in the oil phase and the water phase with inorganic salt, the reaction of generated gas is carried out at a slow speed; after the sweating raw material is cooled to be below a dropping melting point and the sweating process is ended, the wax layer is in a softer solid state, in the process, the oil-soluble acid and the inorganic salt gradually generate chemical reaction to release gas, and micro bubbles which are uniformly distributed are formed in the raw material wax layer; in the sweating process, the air flow passes through the wax layer, on one hand, the inorganic salt solution can be carried out to form tiny spaces in the wax layer, and the tiny spaces and spaces generated by bubbles are easy to form a plurality of tiny channels in the wax layer in the sweating process, so that the liquid components in the sweating process can be discharged; on the other hand, the solid component and the liquid component are forcibly separated, so that the separation effect is enhanced and the separation speed is accelerated. The oil soluble acid and surfactant selected have melting points below the maximum temperature during sweating, contain functional groups, are poorly compatible with the sweating material, and are capable of being discharged with the liquid component during sweating. And then assisting with a constant temperature stage of a sweating process to more fully separate solid components from liquid components, and the like, so that the sweating process can produce the base material for polishing wax, which does not contain low-melting-point components.
The base material, the silicone oil, the natural wax and the solvent are melted and mixed evenly according to the proportion, and the wax polishing product is obtained after cooling.
The method of the invention has the advantages that: the separation effect of the solid component and the liquid component is enhanced and the separation speed is accelerated by adopting a method of forcing the air flow to carry the liquid component out through the wax layer in the sweating process; the constant temperature stage of the crystallization process is increased, and meanwhile, a space formed by micro bubbles generated by the reaction of the oil soluble acid and the inorganic salt and a micro space generated after the inorganic salt solution is discharged are utilized to form a plurality of fine channels, so that the liquid component can be rapidly discharged; and the constant temperature stage of the sweating process is added, so that the sweating process can prepare the base material for polishing wax without low-melting-point components; the base material is then melted and mixed with silicone oil, natural wax, solvent, antioxidant and essence in proportion to obtain the wax polish product. The method has the advantages of low device investment, simple production process, low operation cost, safety, energy conservation, no solvent pollution to the environment, good high temperature resistance of the wax polishing product and the like.
Detailed Description
The invention selects proper low-temperature F-T synthetic product as sweating raw material, and prepares the target product through the processes of emulsification, sweating, blending and the like. Heating and melting a low-temperature F-T synthetic product, preferably adding an oil-soluble acid and an emulsifier, emulsifying with an inorganic salt solution, and then putting into a sweating dish; the upper part of the sweating dish is connected with a detachable sealing device and is connected with a pressurizing buffer tank and a compressor, and/or the lower part of the sweating dish is connected with a decompression buffer tank and a vacuum pump; controlling the temperature rising and reducing speed of the wax layer by oil bath; adding a constant temperature stage in the crystallization process; during sweating, the compressor is activated to create a positive pressure above the wax layer and/or the vacuum pump is activated to create a negative pressure below the wax layer to force an airflow through the wax layer; stopping the sweating process after the wax layer temperature reaches the preset temperature and is kept at the constant temperature for a period of time; refining wax and polishing the base material for wax; the base material is then melted and mixed with other components such as silicone oil, natural wax, solvent and the like to obtain the wax polish product. The method has the advantages of low device investment, simple production process, low operation cost, safety, energy conservation, no solvent pollution to the environment, good high temperature resistance of the wax polishing product and the like.
The process for preparing a polishing wax according to the present invention is specifically described below by way of examples 1 to 4. Unless otherwise noted, the following references to% are mass percentages and the pressures are gauge pressures.
Example 1
The embodiment comprises the following steps: (A) emulsification, (B) sweating, (C) blending.
(A) Emulsification: comprises three steps of (A1) preparation of oil phase materials, (A2) preparation of water phase materials, and (A3) preparation of emulsion.
(A1) Preparation of oil phase Material
Taking wax oil product (with n-alkane content of 95.50wt%, melting point of 86.2 deg.C, penetration (25 deg.C) of 55 (10 deg.C) of low-temperature F-T synthesis experimental device of China petrochemical Co., Ltd-1mm); penetration (65 ℃) is more than 200 (10)-1mm), the wax oil product contains a large amount of low melting point substances according to the penetration degree of 25 ℃ and 65 ℃) 77.0Kg, 2.0Kg of diethylene glycol monolaurate, 0.5Kg of sorbitan monostearate, 0.3Kg of sodium sulfosuccinate monoester and 2.4Kg of linoleic acid are added after being heated to 92 ℃ for melting, and the mixture is stirred evenly.
(A2) Preparing a water-phase material: KHCO with the concentration of 4.8% is prepared317.8Kg of solution are taken and heated to 95 ℃.
(A3) Preparing an emulsion: stirring the oil phase material prepared in the step (A1) at the speed of 500 r/min, adding the water phase material prepared in the step (A2) into the oil phase material, and continuing stirring for 20min to form the water-in-oil emulsion.
(B) Sweating: the method comprises four steps of (B1) preparation, (B2) cooling-constant temperature-cooling crystallization, (B3) heating-constant temperature sweating, and (B4) refining.
(B1) Preparation work
Connecting a sealing system of the sweating dish with a pressurizing buffer tank and a compressor; a decompression buffer tank is arranged at the lower part of the sweating dish and is connected with a vacuum pump; connecting the sweating dish jacket and the movable coil pipe with a circulating system, and fixing the coil pipe on the sweating dish; heat conducting oil is used as a heating medium; starting the heating function of the circulating system to heat the circulating oil to 91 ℃. And water is filled below the sweating dish plate. The emulsion prepared in (A3) was added to a sweat dish. A sealing system of the sweating dish is installed.
(B2) Cooling-high temperature constant temperature-cooling crystallization
After the emulsion is kept stand for 1.0h, the refrigeration function of a circulating system is started, the temperature of a wax layer is controlled to be reduced to 88.5 ℃ at the cooling rate of 2.5 ℃/h, and the temperature is kept constant for 3.0h for high temperature and constant temperature, so that crystals are fully grown; and then the temperature of the wax layer is reduced to 76.0 ℃ at the temperature reduction rate of 2.5 ℃/h so that the wax layer is crystallized to form a solid. The refrigeration function of the circulation system is closed.
(B3) Temperature rising-constant temperature sweating
Draining the pad water of the sweating dish. The outlet of the sweating dish is connected with the intermediate storage tank (I) to receive wax; starting a compressor, keeping the pressure in a pressurizing buffer tank stable at 1.5-1.7 atmospheric pressure, and keeping the normal pressure below a sweating dish plate; the heating function of the circulating system is started, and the temperature of the wax layer is increased to 86.0 ℃ at the heating rate of 3.0 ℃/h. The compressor is stopped.
Starting a vacuum pump and keeping the pressure in the decompression buffer tank stable at-0.4 to-0.6 atmospheric pressure, and keeping the atmospheric pressure above the wax layer at normal pressure; raising the temperature of the wax layer to 91.0 ℃ at a temperature raising rate of 1.5 ℃/h and keeping the temperature for 4.0 hours so as to fully separate the solid component from the liquid component in the wax layer; stopping the vacuum pump and stopping the sweating process.
The outlet of the sweating dish is connected with a crude product storage tank (I) in a switching way to receive wax; and continuously raising the temperature of the heat transfer oil to 110 ℃ to melt and take out the wax, thus obtaining the crude product (I).
(B4) Refining
And refining the crude product (I) by using clay to obtain the base material (I).
Base material (I) Properties: the dropping melting point is 96.2 ℃; penetration (25 ℃ C.) 2 (10)-1mm); penetration (65 ℃) 40 (10)-1mm). The chromatographic-mass spectrometric analysis did not detect the oxygen-containing compounds such as olefin, alcohol and acid. The yield of the base material (I) was 30.5% (relative to the sweating material F-T synthetic wax oil).
The removal of the substances in the raw materials can be seen from the undetected oxygen-containing compounds such as olefin, alcohol, acid and the like through chromatographic-mass spectrometric analysis; it can be seen from the 25 ℃ and 65 ℃ penetration that the low melting substances have been substantially removed in the antiperspirant product.
(C) Blending
(C1) Weighing 1.8Kg of base material (I) and 0.8Kg of white insect wax (manufactured by Cera flava works in North east China), heating to 110 ℃ for melting, and stirring to be uniform.
(C2) Weighing 2.5Kg of No. 200 solvent oil (Zhongshijinling division) and 4.5Kg of No. 120 solvent oil (Qingjiang petrochemical industry, Limited liability company), 0.3Kg of silicone oil (300, Beijing aviation apple silicon chemical industry) and 0.1Kg of alkyl silicone oil (silok-2300, Guangzhou siloco chemical industry), heating to 35 ℃ and stirring uniformly.
(C3) And (3) adding the preparation component (C2) into the preparation component (C1), uniformly stirring, cooling to 70 ℃, putting into a container, and cooling to normal temperature to obtain the wax polish product (I).
The glazing wax product (I) has the following properties: high-temperature stability: qualified; low-temperature stability: qualified; gloss increment value: 13. meets the requirements of GB/T23437-.
Example 2
The embodiment comprises the following steps: (A) emulsification, (B) sweating, (C) blending.
(A) Emulsification: comprises three steps of (A1) preparation of oil phase materials, (A2) preparation of water phase materials, and (A3) preparation of emulsion.
(A1) Preparing an oil phase material:
73.0Kg of wax oil product (same as example 1) of a low-temperature F-T synthesis experimental device of China petrochemical industry Co., Ltd is taken, heated to 92 ℃ and melted, and then 2.5Kg of diethylene glycol fatty acid ester, 0.8Kg of tetraethylene glycol monostearate, 0.5Kg of dodecyl betaine and 3.6Kg of pentadecanoic acid are added and stirred uniformly.
(A2) Preparing a water-phase material: na with the concentration of 4.0 percent is prepared2CO319.6Kg of solution are taken and heated to 95 ℃.
(A3) Preparing an emulsion: stirring the oil phase material prepared in the step (A1) at the speed of 300 r/min, adding the water phase material prepared in the step (A2) into the oil phase material, and continuing stirring for 30min to form the water-in-oil emulsion.
(B) Sweating
The same as in example 1.
The base material (II) produced in this example had the following properties: the dropping melting point is 96.5 ℃; penetration (25 ℃ C.) 2 (10)-1mm); penetration (65 ℃) 38 (10)-1mm). chromatography-Mass Spectrometry analysis, no alkene detectedHydrocarbons, and oxygen-containing compounds such as alcohols and acids. The yield of the base material (II) was 31.2% (relative to the sweating material F-T synthetic wax oil).
The removal of the substances in the raw materials can be seen from the undetected oxygen-containing compounds such as olefin, alcohol, acid and the like through chromatographic-mass spectrometric analysis; it can be seen from the 25 ℃ and 65 ℃ penetration that the low melting substances have been substantially removed in the antiperspirant product.
(C) Blending
(C1) Weighing 1.5Kg of base material (II), 0.9Kg of beeswax (from Shanghai dynasty in North and east China beeswax), and 0.03 Kg of antioxidant 1010 (basf), heating to 110 ℃ for melting, and stirring to be uniform.
(C2) Weighing 5.00Kg of D60 (Panjin Macro petrochemical company), 2.24Kg of 120 # solvent oil (Qingjiang petrochemical company, Ltd.), 0.2Kg of silicone oil (300, Beijing aviation apple silicon chemical industry) and 0.1Kg of phenyl silicone oil (silok-2540, Siloco chemical industry, Guangzhou city), heating to 35 ℃ and stirring uniformly.
(C3) Adding the preparation component (C2) into the preparation component (C1), stirring uniformly, adding 0.03 Kg of essence (vanilla flavor, Shenyang cereal field flavor Co., Ltd.), cooling to 70 ℃, putting into a container, and cooling to normal temperature to obtain the glazing wax product (II).
The glazing wax product (II) has the following properties: high-temperature stability: qualified; low-temperature stability: qualified; gloss increment value: 15. meets the requirements of GB/T23437-.
Example 3
The embodiment comprises the following steps: (A) emulsification, (B) sweating, (C) blending.
(A) Emulsification: comprises three steps of (A1) preparation of oil phase materials, (A2) preparation of water phase materials, and (A3) preparation of emulsion.
(A1) Preparing an oil phase material:
81.0Kg of wax oil product (same as example 1) from the low temperature F-T synthesis experimental device of China petrochemical Co., Ltd is heated to 94 ℃ to be melted, and then 1.4Kg of tetraethylene glycol monostearate, 0.3Kg of sorbitan monooleate, 0.5Kg of polyoxyethylene fatty acid ester and 1.2Kg of palmitoleic acid are added and stirred uniformly.
(A2) Preparing a water-phase material: NaHCO with the preparation concentration of 2.6 percent315.6Kg of solution are taken and heated to 97 ℃.
(A3) Preparing an emulsion: stirring the oil phase material prepared in the step (A1) at the speed of 900 r/min, adding the water phase material prepared in the step (A2) into the oil phase material, and continuing stirring for 10min to form the water-in-oil emulsion.
(B) Sweating
The same as in example 1.
The base material (III) produced in this example had the following properties: the dropping melting point is 95.8 ℃; penetration (25 ℃ C.) 2 (10)-1mm); penetration (65 ℃ C.) 41 (10)-1mm). The chromatographic-mass spectrometric analysis did not detect the oxygen-containing compounds such as olefin, alcohol and acid. The yield of the base material (III) was 30.8% (based on the sweating material F-T synthetic wax oil).
The removal of the substances in the raw materials can be seen from the undetected oxygen-containing compounds such as olefin, alcohol, acid and the like through chromatographic-mass spectrometric analysis; it can be seen from the 25 ℃ and 65 ℃ penetration that the low melting substances have been substantially removed in the antiperspirant product.
(C) Blending
(C1) Weighing 2.1Kg of base material (III) and 0.7Kg of carnauba wax (1 #, produced by Brazil), heating to 110 ℃ for melting, and stirring to be uniform.
(C2) 2.9Kg of Exxsol D80 (Exxon Mobil), 4.0Kg of No. 120 solvent oil (Qingjiang petrochemical industry, Limited liability company), 0.1Kg of silicone oil (300, Beijing aviation apple silicon trauma chemical industry) and 0.2Kg of silicone oil (3000, Beijing aviation apple silicon trauma chemical industry) are weighed, heated to 35 ℃ and stirred uniformly.
(C3) And (3) adding the preparation component (C2) into the preparation component (C1), uniformly stirring, cooling to 70 ℃, putting into a container, and cooling to normal temperature to obtain the wax polish product (III).
Glazing wax product (III) Properties: high-temperature stability: qualified; low-temperature stability: qualified; gloss increment value: 14. meets the requirements of GB/T23437-.
Example 4
The embodiment comprises the following steps: (A) emulsification, (B) sweating, (C) blending.
(A) Emulsification: comprises three steps of (A1) preparation of oil phase materials, (A2) preparation of water phase materials, and (A3) preparation of emulsion.
(A1) Preparing an oil phase material:
73.0Kg of wax oil product (same as example 1) of a low-temperature F-T synthesis experimental device of China petrochemical engineering Co., Ltd is taken, heated to 94 ℃ and melted, and then 2.1Kg of sorbitan monostearate, 0.7Kg of diethylene glycol monolaurate, 0.5Kg of triacetyl oleate and 3.2Kg of n-tridecanoic acid are added and stirred uniformly.
(A2) Preparing a water-phase material: k with the preparation concentration of 5.0%2CO320.5Kg of solution are taken and heated to 97 ℃.
(A3) Preparing an emulsion: stirring the oil phase material prepared in the step (A1) at the speed of 750 r/min, adding the water phase material prepared in the step (A2) into the oil phase material, and continuing stirring for 15min to form the water-in-oil emulsion.
(B) Sweating
The same as in example 1.
The base material (IV) produced in this example had the following properties: the dropping melting point is 96.2 ℃; penetration (25 ℃ C.) 2 (10)-1mm); penetration (65 ℃) 40 (10)-1mm). The chromatographic-mass spectrometric analysis did not detect the oxygen-containing compounds such as olefin, alcohol and acid. The yield of the base material (IV) was 31.1% (synthetic wax oil based on the sweating material F-T).
The removal of the substances in the raw materials can be seen from the undetected oxygen-containing compounds such as olefin, alcohol, acid and the like through chromatographic-mass spectrometric analysis; it can be seen from the 25 ℃ and 65 ℃ penetration that the low melting substances have been substantially removed in the antiperspirant product.
(C) Blending
(C1) Weighing 2.4Kg of basic material (IV) and 0.6Kg of carnauba wax (3 #, brazil), heating to 110 ℃ for melting, and stirring to be uniform.
(C2) Weighing 2.7Kg of D60 (Qingjiang petrochemical industry, Ltd.), 4.0Kg of 200 # solvent oil (Zhongshijinling division), 0.2Kg of silicone oil (300, Beijing aviation apple silicon production) and 0.1Kg of phenyl silicone oil (RB-1558, Guangzhou Ribang chemical industry), heating to 35 ℃ and stirring uniformly.
(C3) And (3) adding the preparation component (C2) into the preparation component (C1), uniformly stirring, cooling to 70 ℃, putting into a container, and cooling to normal temperature to obtain the wax polishing product (IV).
Glazing wax product (IV) Properties: high-temperature stability: qualified; low-temperature stability: qualified; gloss increment value: 13. meets the requirements of GB/T23437-.
As can be seen from examples 1-4, the process of the present invention for preparing a polishing wax, the modification of the sweating device by adding pressure and/or vacuum means, etc.; the improvement of the sweating process is realized by mixing the sweating raw material into oil-soluble acid, forming micro bubbles in a wax layer by gas generated by reaction with inorganic salt and discharging a salt solution to form a micro space, forcing airflow to pass through the wax layer in the sweating process, increasing the constant temperature stage of crystallization and sweating process and the like; the separation effect of the solid component and the liquid component is enhanced and the separation speed is accelerated, so that the low molecular weight component in the raw material is effectively removed, and the base material without the low melting point component can be produced by the sweating process. The base material is then melted and mixed with other components such as silicone oil, natural wax, solvent and the like to obtain the wax polish product. The method has the advantages of low device investment, simple production process, low operation cost, safety, energy conservation, no solvent pollution to the environment, good high temperature resistance of the wax polishing product and the like.
Claims (26)
1. A method of making a polishing wax comprising:
(A) emulsification: the method comprises the following steps:
(A1) preparing an oil phase material: taking an F-T synthetic product with the weight content of normal alkane of more than 80 percent as a sweating raw material, adding an oil-soluble emulsifier and an oil-soluble acid after heating and melting, and uniformly stirring to form an oil phase material;
(A2) preparing a water-phase material: dissolving inorganic salt in water to form a water phase material;
(A3) preparing an emulsion: adding the water phase material obtained in the step (A2) into the oil phase material obtained in the step (A1) under the stirring condition, and continuously stirring for 5-60 minutes to form an emulsion;
(B) sweating: the method comprises the following steps:
(B1) preparation work: charging the emulsion prepared in the process of (a 3) into a sweating device;
(B2) and (3) crystallization: firstly, cooling the wax layer to the melting point of the sweating raw material drop plus 4 ℃ to the melting point of the drop plus 8 ℃ at the speed of 1.0 ℃/h to 10.0 ℃/h; then cooling the wax layer to the melting point of the sweating raw material drops to the melting point of the drops plus 4 ℃ at the speed of 1.0-3.0 ℃/h, and keeping the temperature for 0.1-6.0 hours; then cooling the wax layer to a cooling termination temperature of 5-30 ℃ below the melting point of the sweating raw material drop at the speed of 2.0-4.0 ℃/h;
(B3) sweating: heating at the rate of 0.5-3.5 ℃/h; stopping sweating after the wax layer reaches the preset temperature and is kept at the constant temperature for 0.1-10.0 hours; forcing an air stream through the wax layer during sweating; the predetermined temperature is the melting point of the base material drop ranging from-10 ℃ to the melting point of the base material drop;
(B4) refining: refining the wax to obtain a base material for polishing the wax;
(C) blending: the base material, the silicone oil, the natural wax and the solvent are melted and mixed evenly according to the proportion, and the wax polishing product is obtained after cooling.
2. The method according to claim 1, wherein the oil-soluble emulsifier of step (a 1) is selected from the group consisting of nonionic surfactants, anionic surfactants, cationic surfactants, and amphoteric surfactants; the HLB value of the oil-soluble emulsifier is 1-10; the melting point or freezing point of the oil-soluble emulsifier is lower than the highest temperature for sweating in step (B3).
3. The method of claim 2, wherein the nonionic surfactant is selected from the group consisting of sorbitan monooleate, sorbitan monostearate, diethylene glycol fatty acid ester, sorbitan monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan monolaurate, polyoxyethylene fatty acid ester; the anionic surfactant is selected from a group of substances consisting of fatty alcohol sulfate ester monoethanolamine salt, alkyl polyoxyethylene ether sodium sulfate, oleamido carboxylic acid sodium, sodium alkyl benzene sulfonate, N-methyl oleoyl taurate, butyl naphthalene sodium sulfonate, succinate sodium sulfonate and maleic acid monoester sodium sulfonate; the cationic surfactant is selected from a group of substances consisting of benzyl quaternary ammonium salt, dodecyl dimethyl benzyl ammonium chloride, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride and triethylamine oleate; the amphoteric surfactant is selected from a group consisting of dodecyl betaine, dodecyl dimethyl ammonium oxide, fatty alkyl imidazoline derivatives, fatty acid derivatives and amphoteric modified ethylene oxide adducts.
4. The method according to claim 2, wherein the oil-soluble emulsifier is a complex emulsifier comprising two or more surfactants.
5. The method of claim 1, wherein said oil soluble acid of step (a 1) is an organic acid soluble in the antiperspirant material and capable of reacting with said inorganic salt of (a 2) to form a gas.
6. The method of claim 5, wherein said oil soluble acid is selected from the group consisting of n-unitary, n-capric, n-undecanoic, lauric, n-tridecanoic, myristic, n-pentadecanoic, palmitic, margaritic, stearic, n-nonadecanoic, arachidic, n-heneicosanoic, behenic, n-tricosanoic, lignoceric, n-pentacosanoic, cerotic, heptacosanoic, montanic, n-nonacosanoic, melissic, n-hendecanoic, laccerotic, phylloceric, linoleic, palmitoleic, oleic, erucic, and scylleic acids.
7. The method of claim 6, wherein said oil soluble acid is selected from at least one of linoleic acid, palmitoleic acid, oleic acid, erucic acid, scylleic acid, n-capric acid, n-undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, nacreous acid, stearic acid, n-nonadecanoic acid, arachidic acid, n-heneicosanoic acid, behenic acid, n-tricosanoic acid, lignoceric acid, n-pentacosanoic acid, cerotic acid, and n-heptacosanoic acid.
8. The method of claim 1, wherein said inorganic salt of step (A2) is at least one selected from the group consisting of carbonate, bicarbonate, sulfite, bisulfite and metal sulfide.
9. The method of claim 8, wherein the inorganic salt is at least one selected from the group consisting of sodium carbonate, potassium carbonate, sodium bicarbonate, and potassium bicarbonate.
10. The method according to claim 1, wherein the mass concentration of the inorganic salt in the aqueous phase material of step (A2) is 0.1-10.0%.
11. The method according to claim 1, wherein the stirring speed in the step (A3) is 50 to 5000 rpm, and the temperature for preparing the emulsion is 90 to 98 ℃.
12. The method of claim 1, wherein the emulsion obtained in step (a 3) has a composition of: 55.0-90.0 percent of sweating raw material, 9.8-29.0 percent of water phase material, 0.1-6.0 percent of oil-soluble emulsifier and 0.1-10.0 percent of oil-soluble acid.
13. The method of claim 12, wherein the emulsion obtained in step (a 3) has a composition of: the mass percent of the sweating raw material is 66.0-83.0%, the mass percent of the water phase material is 15.0-25.0%, the mass percent of the oil-soluble emulsifier is 1.8-4.0%, and the mass percent of the oil-soluble acid is 0.2-5.0%.
14. The method of claim 1, wherein said forcing air flow through the wax layer in step (B3) is accomplished by increasing the pressure of air above the wax layer and/or decreasing the pressure of air below the wax layer to create a pressure differential between the upper and lower sides of the wax layer, said pressure differential being between 0.1 and 5.0 atmospheres.
15. The method of claim 1, wherein said forcing of said air stream through said wax layer in step (B3) is performed during an initial sweating session.
16. A method according to claim 14, wherein said forcing of the gas through the wax layer is accomplished by increasing the pressure of the gas above the wax layer by applying a gauge pressure of 0.2 to 2.0 atmospheres above the wax layer while maintaining a constant pressure below the wax layer.
17. A method according to claim 14, wherein said forced gas flow through the wax layer is achieved by reducing the gas pressure below the wax layer, maintaining a constant pressure above the wax layer and a gauge pressure of-0.2 to-0.8 atmospheres below the wax layer.
18. The process of claim 1, wherein the composition of the polishing wax of process (C) is, by mass: 10.0-25.0 percent of base material, 1.0-5.0 percent of silicone oil, 4.0-10.0 percent of natural wax and 60.0-85.0 percent of solvent.
19. The method as claimed in claim 18, wherein more than one of an antioxidant and a perfume is further added into the polishing wax as an additive; the addition amount of the additive calculated by the quality of the optical wax is as follows: 0.1-1.0% of antioxidant and 0.1-1.0% of essence.
20. The method according to claim 1, 18 or 19, wherein the silicone oil is at least one selected from the group consisting of methyl silicone oil, ethyl silicone oil, phenyl silicone oil, methyl hydrogen silicone oil, methyl phenyl silicone oil, methyl chlorophenyl silicone oil, methyl vinyl silicone oil, methyl hydroxy silicone oil, ethyl hydrogen silicone oil and amino silicone oil.
21. The method of claim 1, 18 or 19, wherein the natural wax is at least one selected from the group consisting of beeswax, chinese insect wax, carnauba wax, candelilla wax, montan wax, rice bran wax.
22. The method of claim 1, 18 or 19, wherein the solvent is selected from at least one of n-pentane, n-hexane, n-octane, D40, D60, D80, No. 90, No. 120, No. 180, No. 190, No. 200, exxsol D40, exxsol D80, exxsol D110, exxsol D130, exxsol dsp80/100, benzene, toluene, xylene, cyclohexane, cyclohexanone, toluenecyclohexanone, chlorobenzene, dichlorobenzene, dichloromethane, diethyl ether, ethylene oxide, methyl acetate, ethyl acetate, propyl acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, acetone, methyl butanone, methyl isobutyl ketone, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol ethyl ether acetate, ethylene glycol ether ester, phenol, turpentine, and odorless kerosene.
23. The method of claim 19, wherein the antioxidant is at least one selected from the group consisting of antioxidant BHT, antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 1330, antioxidant 3114, antioxidant 164, antioxidant 168, antioxidant 264, antioxidant B215, and antioxidant B225.
24. The process of claim 1 wherein the F-T synthesis product has a normal alkane content of greater than 80% by weight.
25. The method of claim 1 wherein said sweating device is a sweating dish.
26. The method of claim 14, wherein the pressure differential is between 0.2 and 2.0 atmospheres.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016104330118 | 2016-06-17 | ||
| CN201610433011 | 2016-06-17 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107523223A CN107523223A (en) | 2017-12-29 |
| CN107523223B true CN107523223B (en) | 2020-04-14 |
Family
ID=60748600
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710444759.2A Active CN107523223B (en) | 2016-06-17 | 2017-06-13 | Method for preparing polishing wax |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107523223B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114437826B (en) * | 2020-11-05 | 2024-01-26 | 内蒙古伊泰煤基新材料研究院有限公司 | Method for producing phase-change energy-storage wax |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA421565A (en) * | 1944-07-18 | Standard Oil Development Company | Wax sweating process | |
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN101148565A (en) * | 2007-09-08 | 2008-03-26 | 李而淮 | Wax polish and preparation method thereof |
| CN102925214A (en) * | 2011-08-09 | 2013-02-13 | 苏喜红 | Fischer-Tropsch synthesis wax refinement method |
| CN103102972A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation process for thermoinduction wax medium for automatic enrichment valve of motorcycle |
| CN103773427A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Method for preparing liquid wax |
-
2017
- 2017-06-13 CN CN201710444759.2A patent/CN107523223B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA421565A (en) * | 1944-07-18 | Standard Oil Development Company | Wax sweating process | |
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN101148565A (en) * | 2007-09-08 | 2008-03-26 | 李而淮 | Wax polish and preparation method thereof |
| CN102925214A (en) * | 2011-08-09 | 2013-02-13 | 苏喜红 | Fischer-Tropsch synthesis wax refinement method |
| CN103102972A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation process for thermoinduction wax medium for automatic enrichment valve of motorcycle |
| CN103773427A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Method for preparing liquid wax |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107523223A (en) | 2017-12-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR20140029522A (en) | Process oil, process for production of deasphalted oil, process for production of extract, and process for production of process oil | |
| CN107523223B (en) | Method for preparing polishing wax | |
| WO2019232982A1 (en) | Non-silicon defoaming agent and preparation method therefor | |
| CN107523224B (en) | Method for producing polishing wax | |
| US9879189B2 (en) | Treatment of wax | |
| CN107523222B (en) | Preparation method of polishing wax | |
| CN107513411A (en) | A kind of production method of wax polish | |
| CN107523076B (en) | Warm-mixed epoxy asphalt, mixture containing warm-mixed epoxy asphalt and preparation method of warm-mixed epoxy asphalt | |
| CN107513423B (en) | The method for preparing Wax-for preventing rubber | |
| CN104130387A (en) | Modified high hardness odorless light alkyd resin adopting glycidyl tertcarbonate and preparation method thereof | |
| CN107523350B (en) | A kind of sweating and the method for preparing grinding wheel processing wax | |
| CN106883875A (en) | A kind of production method of Wax-for preventing rubber | |
| CN110105773B (en) | Environment-friendly alkane rubber oil and preparation method thereof | |
| CN107513306B (en) | Method for producing wax for printing ink | |
| CN107523343B (en) | A kind of method of sweating production plastic processing wax | |
| CN105779002A (en) | Method for sweating and preparing microcrystalline wax | |
| CN107513114B (en) | Method for producing wax for plastic processing | |
| CN105733679B (en) | A kind of sweating and the method for production soap wax and paraffin | |
| CN107523354B (en) | A kind of method of sweating production Wax-for preventing rubber | |
| CN105778996A (en) | Method for sweating and preparing saponated paraffin and paraffin | |
| CN112795397B (en) | Composite solvent for separating cyclane and aromatic hydrocarbon from naphtha | |
| CN112625749B (en) | Candle wax and preparation method thereof | |
| CN115651701B (en) | Deoiling method and device for Fischer-Tropsch wax | |
| CN107523344B (en) | A kind of method of sweating production soap manufacturing paraffin and low melt point paraffin | |
| CN107513425B (en) | A kind of grinding wheel processing preparation method of wax |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |