CN105272355A - Tung oil modified paraffin emulsion and preparation and application methods thereof - Google Patents

Tung oil modified paraffin emulsion and preparation and application methods thereof Download PDF

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CN105272355A
CN105272355A CN201510646301.6A CN201510646301A CN105272355A CN 105272355 A CN105272355 A CN 105272355A CN 201510646301 A CN201510646301 A CN 201510646301A CN 105272355 A CN105272355 A CN 105272355A
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tung oil
paraffin wax
wax emulsions
modified paraffin
water
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CN105272355B (en
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蒋新元
廖媛媛
郭忠
万晓清
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Central South University of Forestry and Technology
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Central South University of Forestry and Technology
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Abstract

The invention discloses a tung oil modified paraffin emulsion and its preparation and application methods. The preparation method comprises the following steps: firstly mixing required paraffin and tung oil and an emulsifier, heating, stirring and fusing; then, adding water and stirring at high speed and simultaneously carrying out high-speed emulsification and shearing by the use of emulsification equipment; and finally naturally cooling. Solid concentration of the prepared tung oil modified paraffin emulsion is 30% and above, and its stability reaches 6 months and above. When the tung oil modified paraffin emulsion is used, a proper amount of a dry-promoter additive is doped in the tung oil modified paraffin emulsion so as to promote film-formation drying of the tung oil modified paraffin emulsion and simultaneously raise water resistance and adhesive force of a paraffine film. According to the invention, the problem that film-formation drying time of the paraffin emulsion is long during the concrete curing and using process, a formed paraffine film has poor adhesive force on the surface of concrete and poor water resistance and is easy to wash out by rain to lead to shedding and low water-retention rate of concrete is solved. By the use of the tung oil modified paraffin emulsion, water-retention rate of concrete reaches 90% and above. The tung oil modified paraffin emulsion can satisfy concrete water-retention rate and concrete strength which are required by the national standards of concrete outdoor maintenance.

Description

A kind of tung oil-modified paraffin wax emulsions and preparation and application thereof
Technical field
The invention belongs to the technical field of paraffin modification and application thereof, be specifically related to a kind ofly utilize tung oil-modified paraffin wax emulsions and preparation and application thereof.
Background technology
1, the source of emulsified olefin and purposes
Paraffin is the popular name of solid-state higher alkane mixture, and molecular formula is C nh 2n+2, wherein n=20-40, is obtained by the waxy distillate fraction cold press of natural or artificial petroleum or the method such as solvent dewaxing, sweating.China is resource big country and the big producing country of paraffin, and paraffin export volume accounts for 70% of world's paraffin total trade volume.Paraffin has been widely used at industry tools such as military affairs, agricultural, papermaking, building materials, food, makeup, medicine, textiless.Paraffin is water insoluble, but dissolves in ether, benzene and some ester.In the world, emulsified olefin is that Mobil Oil Corp. begins one's study in the 1950's exploitation the earliest, namely generally uses in the U.S. after 10 years.During 20 century 70, Britain, Germany, Japan also begin one's study and using emulsion paraffin gradually.Due to emulsified olefin when it uses without the need to heating and melting or by dissolution with solvents, film forming is even, spreadability good, and be easy to and the aqueous solution of other material or emulsion compound use, have the advantages such as safe, efficient and economic environmental protection, therefore the purposes of emulsified olefin is very extensive.
2, the type of emulsified olefin
Paraffin is scattered in water becomes high dispersive, even, stable emulsion, must select suitable emulsifying agent and be realized by certain emulsifying process.Emulsifying agent makes paraffin solid form small drop (particle diameter is at 1 ~ 3um) and energy oriented adsorption is surperficial at it, makes paraffin water termination form the interfacial film with certain physical strength, thus makes stable dispersion not easily coalescent precipitation in water.In actual applications, the emulsified olefin great majority used are O/W type.
The selection of emulsifying agent is the key preparing stable emulsion.At present, domestic and international developed emulsified olefin is mostly non-ionic type and anionic emulsifying wax, and cationic emulsifying wax is due to its product instability, and easy layering, therefore, the cationic emulsifying wax succeeded in developing is very few.The HLB value that Emulsification of Paraffin requires is about 10, obtain stay-in-grade emulsified olefin product, key is the selection of emulsifying agent, and the HLB value of emulsifying agent is substantially equal with the HLB value of paraffin, and Compositional type emulsifying additive instead of the single type emulsifying agent of poor efficiency substantially efficiently now.
The preparation of 2.1 emulsified olefines and the selection of emulsifying agent
Researchist is had to find preparing in emulsified olefin process, emulsified olefin poor stability prepared by single emulsifier, when primary isoamyl alcohol, span-80 and tween-80 are composite with certain proportion, the paraffin wax emulsions good fluidity obtained, dispersiveness is secondary (static 1 month, syneresis rate is less than 1%), wax grain is even, without floating wax.Also have researchist to carry out composite with Span-80, Tween-80, stearic acid etc., obtained 52# paraffin wax emulsions, but the consumption of these emulsifying agents is all more, obtained solid content is lower, and during solid content height, product loses flowability.Be that the stability of paraffin emulsion of 7% preparation, dispersiveness, mobility are better by researchist with the total volume of novel built emulsifying agent that stearic acid, auxiliary agent A P-2, emulsion stabilizer HP-1, auxiliary agent A P-1 form, be assessed as secondary.Researchist utilizes nonionogenic tenside polyoxyethylene octylphenol ether, anion surfactant fatty alcohol-ether phosphate kalium salt and auxiliary agent Pentyl alcohol, has prepared the paraffin microemulsion reaching primary standard.Also researchist is had to adopt rp-emulsification (EIP) method, with Span-20, Tween-20 etc. for compound emulsifying agent, obtained the nanometer paraffin wax emulsions of median size between 96 ~ 126nm, emulsion particle diameter in 5 months without noticeable change, inorganic salt on its permanent stability without impact.There is researchist to pass through the experimental study by colloidal mill production Paraffin emulsion waterproof agent, have developed a set of New type Paraffin Emulsion manufacturing technique.
2.2 influence factors preparing emulsified olefin
Under the prerequisite choosing emulsifying agent, also must consider the impact of the factors such as the feed postition of the consumption of emulsifying agent, emulsifying agent, emulsifying temperature and time, stirring velocity, emulsifying device.Outward appearance, fusing point, pH value, stability, water-soluble be the common index of emulsified olefin.For obtaining stable emulsified olefin, the influence factor that hydrophile-lipophile balance value (HLB), emulsifying temperature, reaction times, granularity etc. are main must be considered, also will consider these relevant influence factors such as emulsifier, emulsifying agent feed postition, speed of cooling and stirring velocity, emulsifying device, emulsified water, bubble simultaneously.The preparation method of emulsified olefin mainly contains: agent-in-water method, agent-in-oil method, in turn liquid feeding method, nascent soap method and phase inversion temperature emulsion process.Emulsifying device mainly adopts the equipment such as high-speed shearing emulsion machine, colloidal mill, homogenizer, high-frequency oscillator and ultrasonic oscillator.
The main performance index of 2.3 emulsified olefines
Can paraffin wax emulsions meet application requiring, and main Testing index has: (1) stability: paraffin wax emulsion is put into whizzer, and with the centrifugal 30min of 4000r/min, not stratified is good stability, is layered as poor stability; (2) time of drying: paraffin wax emulsions is applied on sheet glass uniformly by test determination consumption, putting into temperature is 20 DEG C ± 3 DEG C, relative humidity is in the proofing box of 50% ± 10%, observe the film forming properties of emulsion, 20min observes once, and with finger with the pressure contact surface of appropriateness, during without soft sticky sense, be decided to be time of drying; (3) mensuration of film forming properties: paraffin wax emulsions is applied on sheet glass by test determination, coated area is not less than 15cm × 15cm, putting into temperature is 20 DEG C ± 3 DEG C, relative humidity is in the proofing box of 50% ± 10%, after 4h complete drying, whether whether the beaker putting into filled with water soaks half hour, observe film and dissolve, touch and come off.Water is dripped in the sheet glass central authorities another being loaded with into good film, whether muddyly observes water droplet; (4) mensuration of thermotolerance: paraffin wax emulsions is applied on sheet glass by test determination, coated area is not less than 15cm × 15cm, putting into temperature is 20 DEG C ± 3 DEG C, relative humidity is in the proofing box of 50% ± 10%, after 4h complete drying, be placed in and set in the baking oven of temperature, constant temperature 10min, observe and whether occur thawing, metachromatism.
3, tung oil
Tung oil is a kind of excellent band dry vegetable oil, is fatty acid triglycercide mixture.Have that fast drying, light specific gravity, glossiness are good, strong adhesion, the characteristic such as heat-resisting, acidproof, alkaline-resisting, anticorrosion, antirust, non-conductive, of many uses.It is the main raw material manufacturing paint, ink, a large amount of as building, the waterproof of machinery, weapons, car and boat, fishing gear, electrical equipment, anticorrosion, rust proof paint, and can make oilcloth, oilpaper, soap, agricultural chemicals and pharmaceutical nauseants, agrochemical.
The source of 3.1 tung oil and character
The main products of tung oil tree processing is tung oil, and tung oil is the natural fats and oils proposed by the grease in bancoul nuts by squeezing complete processing.Tung oil belongs to siccative oil, and in oils, rate of drying is the fastest, and gained epithelium is hard, water resistant is alkaline-resisting, excellent property, glossy, can not eat, have the features such as waterproof, airtight, non-conductive, antiacid alkali, protection against corrosion, cold-hot, be the important oils kind manufacturing paint and coating.
3.2 paulownia oil compositions
Tung oil is fatty acid triglycercide mixture, and wherein eleostearic acid triglyceride will account for 80% ~ 85%, and saturated fatty acid accounts for 6% ~ 7% in addition, and oleic acid accounts for 8% ~ 10%.The molecular formula of eleostearic acid: CH (CH 2) 3cH=CH-CH-CH-CH=CH (CH 2) 7cOOR it be a CLnA.Three conjugated double bonds form large two keys, and the Kai Kule ring of this and benzene contrasts, and just the latter is closed.Due to the open loop of two keys large in eleostearic acid molecule, be easy to react with other compound, produce the derivative of thousands of tung oil.
The purposes of 3.3 tung oil
Tung oil is the important oils kind manufacturing paint and coating.Tung oil is applied to coating has more than one thousand years history in China, is mainly used in japanning and the timber dressing of woodwork.In recent decades, the widespread use of synthetic coating, has expanded the range of application of tung oil in coatings industry: tung oil can prepare edible vegetable oil, is used as the paste paint thinner during woodworks such as japanning furniture; Can putty be prepared, process slight crack and the recesses such as wooden and steel; Slushing oil can be prepared, to protect steel non-corrosive, not to be corroded; Can prepare moisture-proof coating, this is construction material the most frequently used in building trade; Can ointment be prepared, mainly be used in Steel Concrete assembling or structure seam, make it airtight, water-tight; Can silicon steel sheet paint be produced, make silieonized plate insulate and antirust; The modifications such as bituminous epoxy can be made to make protective system, and it can improve the antiseptic property of chemical industry equipment greatly; Can phenolic varnish be produced, be used for being in harmonious proportion the Lacquer finish of the material such as former paint, red lead powder and door and window, furniture, stationery; Ester gum varniss can be produced, for wood furniture, door and window and metallic surface Lacquer finish; Synthetic enamel and prepared alkyd paint material can be produced, in the process such as the surface protection of indoor and outdoor common metal, wooden object and building and decoration.Tung oil is also widely used in the fields such as electron trade, senior printing-ink, high grade paint, tackiness agent, synthetic resins, plastic industry, rubber industry and biomass energy, and its application prospect is very wide.
3.4 tung oil drying promoters
Oxidized form siccative: cobalt salt, manganese salt, cerium salt, the organic soap of molysite
Polymerizability siccative: cobalt salt (lead salt), manganese salt, zirconates, the organic soap of rare earth
Auxiliary type siccative: the organic soap of zinc salt, calcium salt.
4, development trend
Comparatively thick, the less stable of paraffin particles in the paraffin wax emulsions prepared with conventional emulsifying agent, period of storage is shorter, film forming properties is poor, not water-fast flushing.According to thermomechanical analysis, when discrete particles diameter reaches 10 ~ 100nm, and oil/water interfacial tension is less than 10 -2during dynes per centimeter, milk sap will become a kind of transparent or semitransparent microemulsion, and this is a kind of thermodynamic stable system, is long placed in not phase-splitting, even also can not be separated in powerful sedimentator.Or in the emulsified olefin of preparation, add suitable stablizer and film forming accelerating, promote stability and the film-forming properties of emulsified olefin.
The strong and water tolerance of the paraffin film adhesion that the paraffin wax emulsions that the present invention is directed to non-modified is formed at concrete surface in as outdoor curing compound use procedure is not by force therefore easily caused caducous problem by rain drop erosion.Utilize tung oil-modified paraffin wax emulsions in use by add iron(ic) chloride be that short dry additive can make the film formation time of tung oil-modified paraffin wax emulsions consistent with the film formation time of the paraffin wax emulsions of non-modified, effectively improve paraffin wax emulsions in the sticking power of concrete surface and water tolerance simultaneously, and film forming difficult drop-off, thus water retention when can improve apparatus for concrete member curing and concrete strength, there is society and economic implications preferably.
Summary of the invention
Technical problem to be solved by this invention is the paraffin rete that formed in as outdoor curing compound use procedure of the paraffin wax emulsions of non-modified concrete surface sticking power is strong and water tolerance is not easily caused caducous problem by force by rain drop erosion, causes not reaching the water retention required by national standard and concrete strength during concrete pouring.
In order to solve the problems of the technologies described above, the invention provides a kind of tung oil-modified paraffin wax emulsions and preparation and application thereof.
A kind of preparation method of tung oil-modified paraffin wax emulsions: first by required paraffin and tung oil and emulsifying agent mixing, heated and stirred melts, and then adds water high-speed stirring, uses emulsifying device to carry out emulsify at a high speed shearing, then naturally cooling simultaneously.
In aforesaid method, the quality of tung oil is the 4%-12% of Quality of Paraffin Waxes.
Emulsifying agent described in aforesaid method is polyvalent alcohol polyoxyethylene ether fatty ester and fat polyoxyethylenated alcohol mixed preparing; Polyvalent alcohol polyoxyethylene ether fatty ester preferably includes: sorbester p17, span 20; Fat polyoxyethylenated alcohol preferably includes the liquid aliphatic polyoxyethylenated alcohol of the various polymerization degree; Preferably further to be prepared by HLB value 9.6-10.2 by polyvalent alcohol polyoxyethylene ether fatty ester and fatty alcohol-polyoxyethylene ether.
In aforesaid method, emulsifying agent quality is the 25%-35% of paraffin and tung oil total mass.
Emulsifying temperature 80-90 DEG C in aforesaid method, emulsification times 40-50min.When emulsify at a high speed is sheared, the velocity range 2000-13000rpm that high speed is concrete.
Control watering quantity in aforesaid method and prepare the tung oil-modified paraffin wax emulsions of solids content more than 30%, preferred deionized water.
Aforesaid method is first by required paraffin and tung oil and emulsifying agent mixing, fusing is stirred at 80-90 DEG C, then the deionized water accounting for total water consumption 15-25% is added, carry out high-speed stirring 8-15min, then remaining deionized water is added in reactor in 15-25min in batches, use emulsifying device to carry out emulsify at a high speed shearing, the emulsify at a high speed finally carrying out 5-10min is again sheared, then naturally cooling simultaneously.
A kind of tung oil-modified paraffin wax emulsions is prepared from by above-mentioned method.
The using method of described tung oil-modified paraffin wax emulsions, short dry additive is spiked in tung oil-modified paraffin wax emulsions, then for improving paraffin wax emulsions in the sticking power of concrete surface and water tolerance, and film forming difficult drop-off, thus improve apparatus for concrete member curing time water retention and concrete strength.
Before specifically described tung oil-modified paraffin wax emulsions uses, first short dry additive is dissolved separately by appropriate amount of deionized water, the short dry additive solution of certain volume is spiked in tung oil-modified paraffin wax emulsions and obtains diluent, the mass percent of the tung oil-modified paraffin wax emulsions in diluent is made to be 15-25%, in diluent, the mass percent of short dry additive is 0.02%-0.08%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution that admixture urgees dry additive requires to finish using in 2 days.
The short dry additive used is preferably the inorganic salt of iron, cerium, manganese or cobalt, comprising: one or more in iron(ic) chloride, ferric sulfate, iron nitrate, Cerium II Chloride, cerous sulfate, cerous nitrate, Manganous chloride tetrahydrate, manganous sulfate, manganous nitrate, cobalt chloride, rose vitriol, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES.
Tung oil described in aforesaid method is the natural fats and oils proposed by the grease in bancoul nuts by squeezing complete processing.Tung oil is fatty acid triglycercide mixture, and wherein eleostearic acid triglyceride will account for 80% ~ 85%, and saturated fatty acid accounts for 6% ~ 7% in addition, and oleic acid accounts for 8% ~ 10%.The molecular formula of eleostearic acid: CH (CH 2) 3cH=CH-CH-CH-CH=CH (CH 2) 7cOOR it be a CLnA, three conjugated double bonds form a large π key, tung oil belongs to siccative oil, and in oils, rate of drying is the fastest, and gained epithelium is hard, water resistant is alkaline-resisting, excellent property, glossy, can not eat, having the features such as waterproof, airtight, non-conductive, antiacid alkali, protection against corrosion, cold-hot, is the important oils kind manufacturing paint and coating.
Paraffin described in aforesaid method is full refining or semi-refined or scale wax.
Polyvalent alcohol polyoxyethylene ether fatty ester in aforesaid method in emulsifying agent mainly comprises anhydrous sorbitol Soxylat A 25-7 oleic acid fat (sorbester p17), Sorbitan polyoxyethylenated alcohol lauric acid fat (span 20) etc., fat polyoxyethylenated alcohol in emulsifying agent comprises the liquid aliphatic polyoxyethylenated alcohol (if AEO-n, n are positive integer) of the various polymerization degree.
The properties-correcting agent that the present invention is paraffin wax emulsions with the tung oil of dryness, by emulsification and the tung oil-modified paraffin wax emulsions using the applicable outdoor concrete pourings of Method and process preparation such as short dry additive, to the concrete water retention of raising and concrete strength, there is positive meaning.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and unrestricted the present invention.
Embodiment 1:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification simultaneously, the last high speed shear emulsification carrying out about about 10min again, then cools, preserves.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 4% of Quality of Paraffin Waxes, control water mixing total mass and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.06%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 2:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, carry out high speed shear emulsification with emulsifying device, the last high speed shear emulsification carrying out about about 10min again, then naturally cooling, preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 6% of Quality of Paraffin Waxes, control water mixing total mass and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.06%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 3:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, the last high speed shear emulsification carrying out about about 10min again, then naturally cooling, preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 8% of Quality of Paraffin Waxes, control water mixing total mass and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.06%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 4:
(1) preparation of tung oil-modified paraffin wax emulsions, first required paraffin and tung oil and emulsifying agent are stirred fusing at about 85 DEG C in the reactor, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 20min is added in reactor, use emulsifying device carry out high speed shear emulsification, finally carry out the high speed shear emulsification of about about 10min again, then naturally cooling, preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 8% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.02%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 5:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, the last high speed shear emulsification carrying out about about 10min again, then naturally cooling, preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 8% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 6:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, last carry out the high speed shear emulsification of about about 10min again after, right naturally cooling, to preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 35% of paraffin and tung oil total mass, mix tung oil quality be 10% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 7:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, last carry out the high speed shear emulsification of about about 10min again after, right naturally cooling, to preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 25% of paraffin and tung oil total mass, mix tung oil quality be 5% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 8:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 10min, then remaining water substep in 20min is added in reactor, use emulsifying device to carry out high speed shear emulsification, last carry out the high speed shear emulsification of about about 15min again after, right naturally cooling, to preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 8% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 9:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, last carry out the high speed shear emulsification of about about 10min again after, right naturally cooling, to preserve.The emulsifying agent used in preparation process is prepared by HLB10.0 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and ethoxylated dodecyl alcohol-9, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 5% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 10:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, last carry out the high speed shear emulsification of about about 10min again after, right naturally cooling, to preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and Brij-10, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 8% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first iron(ic) chloride is dissolved separately by appropriate amount of deionized water, the ferric chloride Solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of iron(ic) chloride is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture iron(ic) chloride requires to finish using in 2 days.
Embodiment 11:
(1) preparation of tung oil-modified paraffin wax emulsions, first by required paraffin and tung oil and emulsifying agent in the reactor about 85 DEG C fusings, stir, then the water accounting for total Water about 20% is added, carry out high-speed stirring and be about 15min, then remaining water substep in 15min is added in reactor, use emulsifying device to carry out high speed shear emulsification, last carry out the high speed shear emulsification of about about 10min again after, right naturally cooling, to preserve.The emulsifying agent used in preparation process is prepared by HLB9.8 for anhydrous sorbitol polyoxyethylene oleic acid ester (also known as sp-80, Arlacel-80) and Brij-10, emulsifying temperature 85 DEG C, emulsifying agent quality is 30% of paraffin and tung oil total mass, mix tung oil quality be 8% of Quality of Paraffin Waxes, control water mixing total amount and prepare the paraffin wax emulsions of solids content more than 30%;
(2) use of tung oil-modified paraffin wax emulsions, before the above-mentioned tung oil-modified paraffin wax emulsions prepared uses, first cerous nitrate is dissolved separately by appropriate amount of deionized water, the cerous nitrate solution of certain volume is spiked in tung oil-modified paraffin wax emulsions, and control the deionized water volume of admixture, thus make the mass concentration of the tung oil-modified paraffin wax emulsions after dilution be about 20%, in tung oil-modified paraffin wax emulsions after dilution, the mass percentage concentration of cerous nitrate is 0.04%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution of admixture cerous nitrate requires to finish using in 2 days.
Tung oil-modified paraffin wax emulsions solids concn prepared by the present invention is more than 30%, and stability reaches more than 6 months.
Result of use of the present invention.The solids content using same process condition to prepare is 20% and stable unmodified paraffin wax emulsions, tung oil-modified paraffin wax emulsions, mix the tung oil-modified paraffin wax emulsions of 0.08% iron ion, carry out film forming rate of drying according to universal test method or national standard, become the performance comparison inspections such as film hardness, water tolerance (soaking time) and concrete water retention, each paraffin wax emulsions sample carries out three parallel tests, and result is as shown in table 1.
The different paraffin wax emulsions performance comparison of table 1

Claims (10)

1. the preparation method of a tung oil-modified paraffin wax emulsions, it is characterized in that: first by required paraffin and tung oil and emulsifying agent mixing, heated and stirred melts, and then adds water high-speed stirring, use emulsifying device to carry out emulsify at a high speed shearing, then naturally cooling simultaneously.
2. preparation method according to claim 1, is characterized in that: the quality of tung oil is the 4%-12% of Quality of Paraffin Waxes.
3. preparation method according to claim 1, is characterized in that: described emulsifying agent is polyvalent alcohol polyoxyethylene ether fatty ester and fat polyoxyethylenated alcohol mixed preparing; Polyvalent alcohol polyoxyethylene ether fatty ester preferably includes: sorbester p17, span 20; Fat polyoxyethylenated alcohol preferably includes the liquid aliphatic polyoxyethylenated alcohol of the various polymerization degree; Preferably further to be prepared by HLB value 9.6-10.2 by polyvalent alcohol polyoxyethylene ether fatty ester and fatty alcohol-polyoxyethylene ether.
4. preparation method according to claim 3, is characterized in that: emulsifying agent quality is the 25%-35% of paraffin and tung oil total mass.
5. preparation method according to claim 1, is characterized in that: emulsifying temperature 80-90 DEG C, emulsification times 40-50min; When emulsify at a high speed is sheared, the velocity range 2000-13000rpm that high speed is concrete.
6. preparation method according to claim 1, is characterized in that: control watering quantity and prepare the tung oil-modified paraffin wax emulsions of solids content more than 30%, preferred deionized water.
7. preparation method according to claim 1, it is characterized in that: first by required paraffin and tung oil and emulsifying agent mixing, fusing is stirred at 80-90 DEG C, then the deionized water accounting for total water consumption 15-25% is added, carry out high-speed stirring 8-15min, then remaining deionized water is added in reactor in 15-25min in batches, use emulsifying device to carry out emulsify at a high speed shearing simultaneously, the last emulsify at a high speed carrying out 5-10min is again sheared, then naturally cooling.
8. a tung oil-modified paraffin wax emulsions, is characterized in that, is to be prepared from by the method described in any one of claim 1-7.
9. the using method of tung oil-modified paraffin wax emulsions according to claim 8, it is characterized in that, short dry additive is spiked in tung oil-modified paraffin wax emulsions, then for improving paraffin wax emulsions in the sticking power of concrete surface and water tolerance, and film forming difficult drop-off, thus improve apparatus for concrete member curing time water retention and concrete strength.
10. the using method of tung oil-modified paraffin wax emulsions according to claim 9, it is characterized in that, before described tung oil-modified paraffin wax emulsions uses, first short dry additive is dissolved separately by appropriate amount of deionized water, the short dry additive solution of certain volume is spiked in tung oil-modified paraffin wax emulsions and obtains diluent, the mass percent of the tung oil-modified paraffin wax emulsions in diluent is made to be 15-25%, in diluent, the mass percent of short dry additive is 0.02%-0.08%, use on surface of concrete structure after stirring, the tung oil-modified paraffin wax emulsions of dilution that admixture urgees dry additive requires to finish using in 2 days.
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