CN102911377B - Lac resin hydrosol and preparation method thereof - Google Patents
Lac resin hydrosol and preparation method thereof Download PDFInfo
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- CN102911377B CN102911377B CN201210421028.3A CN201210421028A CN102911377B CN 102911377 B CN102911377 B CN 102911377B CN 201210421028 A CN201210421028 A CN 201210421028A CN 102911377 B CN102911377 B CN 102911377B
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Abstract
The invention provides lac resin nanoscale hydrosol and a preparation method thereof. The lac resin hydrosol is composed of lac resin and water. The method comprises the following steps: 1), dissolving lac resin in ethanol so as to obtain a lac resin ethanol solution; and 2), dripping the lac resin ethanol solution in deionized water, and distilling to remove ethanol. The lac resin hydrosol prepared by the method is small in particle size, good in dispersivity, storage stability, centrifugal stability and freeze-thaw stability and can reach national first level standard. The method has the advantages of simplicity and suitability for large-scale popularization and application.
Description
Technical field
The present invention relates to a kind of water-sol and preparation method thereof, particularly a kind of sclerolac water-sol and preparation method thereof.
Background technology
Sclerolac is a kind of crude substance---the chief component composition of lac of tachardia lacca secretion, and sclerolac is ester and the polyester mixture that hydroxy fatty acid and hydroxy sesquiterpene acid form, and its molecular-weight average is 1000, and molecular formula can be used C
60h
90o
5represent, in each molecule, at least contain 1 free carboxy, 5 hydroxyls, 3 ester groups and 1 aldehyde radical.
Owing to containing the multiple functional groups such as hydroxyl, carboxyl, aldehyde radical in sclerolac molecular structure, based on its multi-functional chemical structure, it has some advantageous properties.Sclerolac clinging power is strong, good luster, to UV stable, electrical insulation capability is good, have thermoplasticity and thermoset concurrently, can be dissolved in alcohol and alkali, oil resistant, acidproof, nontoxic to people, non-stimulated, can be used as varnish, rumbling compound, tackiness agent, insulating material and molding material etc., there is waterproof, anticorrosive, anti-salt marsh, oil resistant, acidproof and good film forming properties, good degradation property, be widely used in national defence, electric, coating, rubber, plastics, medicine, process hides, papermaking, printing, the industrial sectors such as food, its purposes is very extensive, there is important economic worth.
Although sclerolac has numerous good characteristics, but due to some defects of sclerolac, the use of sclerolac need to utilize organic solvent or basic solvent to dissolve, and sclerolac is only dissolved in segment polarity solvent, if but required in use that solvent is nontoxic and use cost is low, organic solvent would just be had too many difficulties to cope with.Utilize alkali lye to dissolve sclerolac, can not keep the original character of sclerolac, so alkali lye can not be served as outstanding use solvent systems, sclerolac also has the problems such as the lower and solvent systems of a batch otherness, softening temperature is limited in addition, needs current scientific worker to carry out certain improvement and just can apply.
At present numerous to the research of sclerolac, for example prepare sclerolac soap-free emulsion, Krause etc. are dissolved in lac in sodium hydroxide solution, add hydrochloric acid acid out under the stirring of 9500r/min, then with high pressure homogenizer homogeneous technology, have made the soap-free emulsion of sclerolac.But in its sclerolac emulsion of making, there is a large amount of solubility salt sodium-chlor, can not remove.The existence of a large amount of electrolyte salt will affect the stability of emulsion.So this acid-precipitation method is not to prepare the desirable method of sclerolac soap-free emulsion.And for example prepare sclerolac microcapsule, Xue etc., by sclerolac success wraps around tooth SYNTHETIC OPTICAL WHITNER urea peroxide, have made sclerolac urea peroxide microcapsule and encapsulation ratio and have reached 70%, and this is also for new field has been opened up in the application of sclerolac.Sclerolac can be made the microcapsule of fire retardant, because sclerolac has larger molecular weight, the point of ignition lower than general material, and also has the abundant group can be compatible with other additives, can be applied to the preparation of anti-flaming dope.
Although sclerolac soap-free emulsion can be prepared, need to introduce a large amount of salts and cause the unstable of emulsion, and preparation process is loaded down with trivial details, particle is larger.
Summary of the invention
The object of the invention is to provides a kind of sclerolac water-sol and preparation method thereof for the technical problem in prior art, sclerolac application aspect being existed, the method technique is simple, easy to operate, the sclerolac water-sol clarification of preparation, transparent, the grain diameter of the water-sol is little, and stability and good dispersity all reach one-level national standard, and utilize fully natural resources, improve Business Economic Benefit.
For realizing the object of the invention, one aspect of the present invention provides a kind of preparation method of the sclerolac water-sol, comprises as follows step in sequence:
1) sclerolac is joined in ethanol, dissolve, make sclerolac ethanolic soln;
2) sclerolac ethanolic soln is joined in deionized water, make sclerolac collagen solution;
3) sclerolac collagen solution is distilled to processing, remove ethanol, concentrated, obtain.
Wherein, the weight part proportioning of sclerolac described in step 1) and ethanol is 2 ~ 9:91 ~ 98, be to contain 2 ~ 9g sclerolac in every 100 grams of described sclerolac ethanolic solns, the mass percent concentration that is to say sclerolac in described sclerolac ethanolic soln is 2 ~ 9%; Be preferably 2 ~ 7:93 ~ 98, more preferably 3 ~ 4:96 ~ 97.
Particularly, ethanol described in step 1) is dehydrated alcohol.
Wherein, step 2) described in ratio >=3 of deionized water and the volume of sclerolac ethanolic soln.
Particularly, described deionized water is 3-20:1 with the ratio of the volume of sclerolac ethanolic soln, is preferably 3-10:1.
Wherein, in described step 2) under whipped state, add described sclerolac ethanolic soln, stirring velocity is 6000 ~ 10000rpm, is preferably 6000 ~ 8000rpm.
Particularly, described sclerolac ethanolic soln is with the cylindric of diameter≤8mm or wire liquid is streamed joins in described deionized water.
Wherein, described sclerolac ethanolic soln diameter cylindric or wire liquid stream is 4 ~ 8mm, is preferably 4 ~ 6mm.
Particularly, described sclerolac ethanolic soln, by the nozzle of diameter≤8mm, after flowing, the cylindric or wire liquid that makes sclerolac ethanolic soln form diameter≤8mm is joined in described deionized water.
Especially, after the nozzle that is 4 ~ 8mm by diameter by described sclerolac ethanolic soln, after flowing, the cylindric or wire liquid that makes sclerolac ethanolic soln form diameter 4 ~ 8mm joins in deionized water.
Wherein, the diameter of described nozzle is preferably 4 ~ 6mm.
Particularly, step 2) in to control to adding the speed of described sclerolac ethanolic soln in deionized water be 3 ~ 15ml/min, be preferably 5 ~ 7ml/min, to the speed that drips described sclerolac ethanolic soln in every 1L deionized water, be 3 ~ 15ml/min, be preferably 5 ~ 7ml/min, that is to say if drip sclerolac ethanolic soln in 1L deionized water, rate of addition is 3 ~ 15ml/min, if drip sclerolac ethanolic soln in 2L deionized water, rate of addition is 6 ~ 30ml/min, if drip described sclerolac ethanolic soln in 10L deionized water, rate of addition is 30 ~ 150ml/min, other the like.
Wherein, step 2) described in sclerolac ethanolic soln be 1:3 ~ 10 with the ratio of the volume of described deionized water, be preferably 1:3 ~ 7.
Wherein, described in step 3), distillation is treated to underpressure distillation processing.
Particularly, in described underpressure distillation treating processes, controlling temperature is 35 ~ 50 ℃, is preferably 35 ~ 40 ℃; Control absolute pressure is 0.02 ~ 0.04MPa.
Particularly, in step 3), sclerolac collagen solution is concentrated into 1/5 ~ 1/2 of its original volume, be preferably 1/4 ~ 1/3, the volume of the sclerolac water-sol making after distillation, concentration is 1/5 ~ 1/2 of sclerolac collagen solution volume, that is to say, the ratio of the volume of the sclerolac water-sol that the volume of sclerolac collagen solution makes after processing with distillation and concentration is 5 ~ 2:1.
The present invention provides a kind of sclerolac water-sol being prepared from according to the method described above on the other hand.
Tool of the present invention has the following advantages:
1, in the sclerolac water-sol that prepared by the present invention, grain diameter is little, median size≤134nm, median size is 125 ~ 134nm, and the particle diameter of the water-sol is evenly distributed, good stability, and because water-sol particle diameter is little, the water-sol is at 800nm place, visible region transmittance more than 60%, and the water-sol is clarification, transparence, for aspects such as waterproof, fresh-keeping, drug release, do not affect the attractive in appearance of material, suitable large-scale application.
2, the particle diameter of sclerolac nano-sized hydrosol particle of the present invention is in nanometer range; there is surface effects, small-size effect and macro quanta tunnel effect; the specific surface area of the sclerolac water-sol increases; chemically reactive improves, and at aspects such as material waterproofing protection, preserving fruit and vegetable utilizing are antibacterial, has huge potential application foreground.
3, sclerolac nano-sized hydrosol of the present invention has satisfactory stability and dispersiveness, can dissolve each other with water arbitrary proportion, and centrifugal stability, storage stability and the freeze-thaw stability one-level that is all up to state standards, good dispersity, reach one-level, the long quality-guarantee period of emulsion, is suitable for long-time preservation and use.
4, preparation method of the present invention is simple, step of preparation process is brief, processing condition gentleness, is easy to control, and suitable large-scale promotion application, reduces the production cost of sclerolac nano-sized hydrosol.
Accompanying drawing explanation
Fig. 1 is the Intensity(intensity of embodiment 1 sclerolac nano-sized hydrosol) size distribution figure;
Fig. 2 is the Intensity size distribution figure of embodiment 2 sclerolac nano-sized hydrosols;
Fig. 3 is the Intensity size distribution figure of embodiment 3 sclerolac nano-sized hydrosols;
Fig. 4 is the Intensity size distribution figure of embodiment 4 sclerolac nano-sized hydrosols.
Embodiment
The refining sclerolac using in the embodiment of the present invention, by the extraordinary Biological resources of Resources Insect Inst., Chinese Academy of Forestry Sciences, researching and developing pilot scale base provides; The quality index of sclerolac is as follows:
Hot ethanol insolubles (%)≤3 volatile matter (moisture) (%)≤2.5
Heat embrittlement time (170 ℃ ± 0.5 ℃) (min) >=7 water solubless (%)≤1
Wax (%)≤5.5 acid number (mg/g) 75～90
Rosin without
Ethanol (AR), Qing Chuandong Chemical Co., Ltd..
Embodiment 1:
1, prepare sclerolac ethanolic soln
0.3kg sclerolac is joined in the dehydrated alcohol of 9.7kg, stirring and dissolving, make sclerolac ethanolic soln, wherein sclerolac and mass ratio dehydrated alcohol are 3:97, the mass percent concentration that is sclerolac in sclerolac ethanolic soln is 3%, that is to say, in the dehydrated alcohol of every 97g, add the sclerolac that adds 3kg in 3g sclerolac or 97kg dehydrated alcohol.
2, prepare shellac wax Resin adhesive stoste
3L deionized water is placed in to dispersion machine (Ultra-Turrax T 25 digital dispersion machines, Germany IKA company) in, under whipped state to the sclerolac ethanolic soln 1L that adds step 1 to prepare in dispersion machine, wherein, adopt constant flow pump (Baoding LanGe constant flow pump Co., Ltd, BT100-1J) the sclerolac ethanolic soln of being prepared by step 1 flows out from fluid column flow nozzle (Dongguan rich former spraying treating plant company limited), forming cylindric liquid stream joins in the deionized water of dispersion machine, the diameter of Control Nozzle is 4mm, the diameter that joins the sclerolac ethanolic soln wire liquid stream in deionized water is 4mm, the speed that adds sclerolac ethanolic soln is 9ml/min, to adding the speed of sclerolac ethanolic soln in 1L deionized water, be 3ml/min, sclerolac ethanolic soln adds after end, stop stirring, make sclerolac collagen solution, wherein stir speed (S.S.) is 6000rpm, and sclerolac ethanolic soln is 1:3 with the ratio of the volume of deionized water.
In the present invention, except using fluid column flow nozzle joins sclerolac ethanolic soln in the deionized water of dispersion machine, other nozzle diameters are≤nozzle of 8mm is all applicable to the present invention.
The present invention adopts sclerolac is dissolved in the good solvent ethanol of sclerolac in advance, make sclerolac ethanolic soln, then sclerolac ethanolic soln is joined in the insoluble solvent of sclerolac (being anti-solvent, negative solvent or contrary solvent) water, sclerolac is separated out, by the diameter that regulates sclerolac ethanolic soln, control good solvent in the contact surface size of poor solvent, select cylindric liquid stream, be beneficial to effective contact insoluble solvent most.
3, distillation, concentration
The sclerolac collagen solution of 4L is placed in to reduction vaporization instrument (Shanghai Shen Sheng Bioisystech Co., Ltd) and carries out underpressure distillation processing, ethanol is removed in underpressure distillation, be concentrated into 1L, make the sclerolac water-sol, in wherein underpressure distillation treating processes, distillation temperature is 40 ℃, absolute pressure is 0.04MPa, and sclerolac collagen solution is 4:1 with the ratio of the volume of the sclerolac water-sol, is about to sclerolac collagen solution and is concentrated into 1/4 of its initial volume.
Embodiment 2
1, prepare sclerolac ethanolic soln
0.6kg sclerolac is joined in the dehydrated alcohol of 9.4kg, stirring and dissolving, make sclerolac ethanolic soln, wherein sclerolac and mass ratio dehydrated alcohol are 6:94, the mass percent concentration that is sclerolac in sclerolac ethanolic soln is 6%, that is to say, in the dehydrated alcohol of every 94g, add the sclerolac that adds 6kg in 6g sclerolac or 94kg dehydrated alcohol.
2, prepare sclerolac collagen solution
7L deionized water is placed in to dispersion machine (Ultra-Turrax T 25 digital dispersion machines, Germany IKA company) in, under whipped state to the sclerolac ethanolic soln 1L that adds step 1 to prepare in dispersion machine, wherein, the sclerolac ethanolic soln that adopts constant flow pump prepared by step 1 flows out from fluid column flow nozzle, forming cylindric liquid stream flows in the deionized water of dispersion machine, the diameter of controlling fluid column flow nozzle is 6mm, and the diameter that joins the sclerolac ethanolic soln liquid stream in deionized water is 6mm; The speed that adds sclerolac ethanolic soln is 35ml/min, to the speed that drips sclerolac ethanolic soln in 1L deionized water, be 5ml/min, sclerolac ethanolic soln adds after end, stop stirring, make sclerolac collagen solution, wherein stir speed (S.S.) is 8000rpm, and sclerolac ethanolic soln is 1:7 with the ratio of the volume of deionized water.
3, distillation, concentration
Get the sclerolac collagen solution 6L of preparation in step 2, be placed in reduction vaporization instrument and carry out underpressure distillation processing, ethanol is removed in underpressure distillation, be concentrated into 2L, make the sclerolac water-sol, in wherein underpressure distillation treating processes, distillation temperature is 35 ℃, and absolute pressure is 0.02MPa, sclerolac collagen solution is 3:1 with the ratio of the volume of the sclerolac water-sol, is about to sclerolac collagen solution and is concentrated into 1/3 of its initial volume.
Embodiment 3
1, prepare sclerolac ethanolic soln
0.7kg sclerolac is joined in the dehydrated alcohol of 9.3kg, stirring and dissolving, make sclerolac ethanolic soln, wherein sclerolac and mass ratio dehydrated alcohol are 7:93, the mass percent concentration that is sclerolac in sclerolac ethanolic soln is 7%, that is to say, in the dehydrated alcohol of every 93g, add the sclerolac that adds 7kg in 7g sclerolac or 93kg dehydrated alcohol.
2, prepare shellac wax Resin adhesive stoste
10L deionized water is placed in to dispersion machine, under whipped state to the sclerolac ethanolic soln 1L that adds step 1 to prepare in dispersion machine, wherein, the sclerolac ethanolic soln that adopts constant flow pump prepared by step 1 flows out from fluid column flow nozzle, forming cylindric liquid stream flows in the deionized water of dispersion machine, the diameter of controlling fluid column flow nozzle is 8mm, and the diameter that joins the sclerolac ethanolic soln liquid stream in deionized water is 8mm; The speed that adds sclerolac ethanolic soln is 150ml/min, to the speed that drips sclerolac ethanolic soln in 1L deionized water, be 15ml/min, sclerolac ethanolic soln adds after end, stop stirring, make sclerolac collagen solution, wherein stir speed (S.S.) is 10000rpm, and sclerolac ethanolic soln is 1:10 with the ratio of the volume of deionized water.
3, distillation, concentration
The sclerolac collagen solution 10L that gets in step 2 preparation is placed in reduction vaporization instrument (Shanghai Shen Sheng Bioisystech Co., Ltd) and carries out underpressure distillation processing, ethanol is removed in underpressure distillation, be concentrated into 2L, make the sclerolac water-sol, in wherein underpressure distillation treating processes, distillation temperature is 50 ℃, absolute pressure is 0.04MPa, and sclerolac collagen solution is 5:1 with the ratio of the volume of the sclerolac water-sol, is about to sclerolac collagen solution and is concentrated into 1/5 of its initial volume.
Embodiment 4
1, prepare sclerolac ethanolic soln
0.2kg sclerolac is joined in the dehydrated alcohol of 9.8kg, stirring and dissolving, make sclerolac ethanolic soln, wherein sclerolac and mass ratio dehydrated alcohol are 2:98, the mass percent concentration that is sclerolac in sclerolac ethanolic soln is 2%, that is to say, in the dehydrated alcohol of every 98g, add the sclerolac that adds 2kg in 2g sclerolac or 98kg dehydrated alcohol.
2, prepare shellac wax Resin adhesive stoste
10L deionized water is placed in to dispersion machine, under whipped state to the sclerolac ethanolic soln 2L that adds step 1 to prepare in dispersion machine, wherein, the sclerolac ethanolic soln that adopts constant flow pump prepared by step 1 flows out from fluid column flow nozzle, forming cylindric liquid stream flows in the deionized water of dispersion machine, the diameter of controlling fluid column flow nozzle is 4mm, and the diameter that joins the sclerolac ethanolic soln liquid stream in deionized water is 4mm; The speed that adds sclerolac ethanolic soln is 70ml/min, to the speed that drips sclerolac ethanolic soln in 1L deionized water, be 7ml/min, sclerolac ethanolic soln adds after end, stop stirring, make sclerolac collagen solution, wherein stir speed (S.S.) is 7000rpm, and sclerolac ethanolic soln is 1:5 with the ratio of the volume of deionized water.
3, distillation, concentration
Sclerolac collagen solution 12L prepared by step 2 is placed in reduction vaporization instrument and carries out underpressure distillation processing, ethanol is removed in underpressure distillation, be concentrated into 6L, make the sclerolac water-sol, in wherein underpressure distillation treating processes, distillation temperature is 35 ℃, absolute pressure is 0.02MPa, and sclerolac collagen solution is 2:1 with the ratio of the volume of the sclerolac water-sol, is about to sclerolac collagen solution and is concentrated into 1/2 of its initial volume.
Test example 1 sclerolac water-sol particle size analysis
Adopt laser particle analyzer (PSS particle-size analyzer-380, U.S. Particle Sizing Systems company) measure the Intensity particle diameter of the sclerolac water-sol, intensity median size is as shown in table 1, and the Intensity size distribution figure of the resin water-sol as shown in Figure 1,2,3, 4.
The particle size analysis result of the table 1 sclerolac water-sol
| Intensity median size (nm) | |
| |
129 |
| Embodiment 2 | 128 |
| Embodiment 3 | 134 |
| Embodiment 4 | 125 |
As shown in Table 1: the intensity median size of the sclerolac water-sol prepared by the present invention is 125 ~ 134nm, and sample particulate belongs to nano level, and the particle size distribution of particle is normal distribution shape, and making the sclerolac water-sol is the nano level water-sol.
The Intensity size distribution figure of the water-sol of the present invention is known, the particle diameter major part of the particle of the water-sol prepared by the present invention is below 100nm, and in the distribution plan of particle diameter, peak value is all below 100nm, and sclerolac hydrosol particle particle diameter is little, be clarification, transparence.
Test example 2 sclerolac water-sol Zeta potentials are analyzed
Adopt Zeta potential analyser (NanoZS ZEN3600, Britain Malvern company) to measure the Zeta potential of the sclerolac water-sol, Zeta potential measurement result is as shown in table 2.
The Zeta potential analytical results of the table 2 sclerolac water-sol
| Zeta potential (mV) | |
| Embodiment 1 | -32.5 |
| Embodiment 2 | -30.8 |
| Embodiment 3 | -20.8 |
| Embodiment 4 | -42.4 |
As shown in Table 2: the Zeta potential value of the sclerolac water-sol prepared by the present invention is high, reach-20.8 ~-42.4mV, show that the repulsive force between sclerolac water-sol particle prepared by the present invention is large, particle-stabilised, the good stability of the water-sol of formation; By test, show that the Zeta potential of the sclerolac water-sol prepared by the present invention is to be also normal distribution in addition.
The centrifugal stability of test example 3, dispersed mensuration
1, Stability Determination
According to the assessment method > > [GB 11543-89] of the characteristic test of the middle and high viscosity emulsion of national standard < < tensio-active agent and emulsifying capacity thereof, measure the centrifugal stability of the sclerolac water-sol: sclerolac water-sol 10ml prepared by embodiment 1-4 injects centrifuge tube, put into whizzer (TDL-40B type whizzer, Anting Scientific Instrument Factory, Shanghai) in, with the rotating speed centrifugation of 4000r/min, after centrifugal 10min, observe whether layering
In the assessment method > > [GB 11543-89] of the characteristic test of the middle and high viscosity emulsion of national standard < < tensio-active agent and emulsifying capacity thereof, stability of emulsion evaluation form is as shown in table 3.
Table 3 stability of emulsion evaluation form
| Stability (level) | The phenomenon that emulsion is |
| 1 | Good homogeneity |
| 2 | Preliminary visible denseness is irregular |
| 3 | To inhomogeneous clear conversion |
| 4 | The separation of preliminary |
| 5 | The separation of obviously visible phase |
| 6 | Two separate mutually completely |
This test example is evaluated sclerolac Stability of colloidal dispersion prepared by the present invention with reference to the characteristic test of the middle and high viscosity emulsion of national standard < < tensio-active agent and the assessment method > > [GB 11543-89] of emulsifying capacity thereof, evaluation result is as shown in table 4, and the centrifugal stability of the sclerolac water-sol prepared by the present invention is 1 grade.
2, dispersed mensuration
The sclerolac water-sol prepared by embodiment 1-4 splashes in water, observes the state of the solution after disperseing, and dispersiveness is divided into five grades, and one-level is best, and Pyatyi is the poorest, and dispersed measurement result is as shown in table 4:
One-level: the water-sol is splashed in water, can promptly be dispersed into band blue-fluorescence cloud dispersion liquid, au bleu or pale asphyxia clear solution after stirring a little.
Secondary: the water-sol is splashed in water, can automatically be dispersed into rapidly the dispersion liquid of pearl opal cloud band fluorescence, stir a little the translucent solution of au bleu.
Three grades: the water-sol is splashed in water, and be white in color cloud or strip dispersion liquid, obtain the slightly opaque emulsion with fluorescence of oyster white after stirring.
Level Four: the water-sol is splashed in water, and the particulate that is white in color is kept afloat, still can become the opaque emulsion of oyster white after stirring.
Pyatyi: the water-sol is splashed in water, and the particulate that is white in color is kept afloat, though there is immediately layering, sclerolac particulate floating in energy emulsification after stirring.
The centrifugal stability of the table 4 sclerolac water-sol, dispersivity test result
| Centrifugal stability rank | Dispersed | |
| Embodiment | ||
| 1 | 1 | 1 |
| Embodiment 2 | 1 | 1 |
| Embodiment 3 | 1 | 1 |
| Embodiment 4 | 1 | 1 |
The sclerolac water-sol prepared by the present invention has good centrifugal stability, dispersiveness, and centrifugal stability and dispersiveness all reach one-level national standard.
Test example 4 storage stabilitys, dispersed mensuration
1, storage stability is measured
The sclerolac water-sol prepared by embodiment 1-4 is positioned in the container of sealing, at room temperature store after 15 days, the storage stability of measuring the sclerolac water-sol according to the assessment method > > [GB 11543-89] of the characteristic test of the middle and high viscosity emulsion of national standard < < tensio-active agent and emulsifying capacity thereof, measurement result is as shown in table 5.
2, storage is dispersed measures
The sclerolac water-sol prepared by embodiment 1-4 is positioned in the container of sealing, at room temperature stores after 30 days, and emulsion is splashed in water, the state of observing the solution after disperseing, dispersiveness is divided into five grades, and one-level is best, Pyatyi is the poorest, and the measurement result of emulsion dispersion is as shown in table 5.
The storage stability of the table 5 sclerolac water-sol, dispersivity test result
| Storage stability rank | Dispersed | |
| Embodiment | ||
| 1 | 1 | 1 |
| Embodiment 2 | 1 | 1 |
| Embodiment 3 | 1 | 1 |
| Embodiment 4 | 1 | 1 |
The sclerolac water-sol prepared by the present invention has satisfactory stability, dispersiveness, and storage stability and dispersiveness all reach one-level national standard.
Test example 5 freeze-thaw stabilities, dispersed mensuration
The sclerolac water-sol prepared by embodiment 1-4 packs in 100ml Plastic Bottle, freezing 24h under (20 ± 1) ℃ condition, then 5h thaws under the condition of 30 ℃, complete freeze-thaw cycle one time, repeat above-mentioned freeze-thaw cycle 5 times, in national standard < < tensio-active agent, the assessment method > > [GB 11543-89] of the characteristic test of high viscosity emulsion and emulsifying capacity thereof measures the centrifugal stability of the water-sol after freeze thawing each time, the emulsion 10ml getting after freeze thawing each time injects centrifuge tube, put into whizzer, with the rotating speed centrifugation of 4000r/min, after centrifugal 10min, observe whether layering, measurement result is as shown in table 6.
The water-sol after embodiment 1-4 freeze thawing is each time splashed in water, observe the state of the solution after disperseing, dispersiveness is divided into five grades, and one-level is best, and Pyatyi is the poorest, and the measurement result of the water-sol dispersiveness after freeze thawing is as shown in table 6 each time.
The freeze-thaw stability of the table 6 sclerolac water-sol, dispersivity test result
Test-results shows: the sclerolac water-sol prepared by the present invention has good centrifugal stability, dispersiveness, through repeatedly still keeping goodish centrifugal stability and dispersiveness after (5 times) freeze thawing, centrifugal stability and dispersiveness all reach one-level national standard, can continue to use, have a extensive future.
Test example 6 salt tolerance tests
Compound concentration is 1%, 2% NaCl solution, standby;
Get respectively each 2 parts of sclerolac water-sol 50g prepared by embodiment 1-4, add respectively the each 50g of NaCl solution of different concns, stir, the mass ratio that makes the addition of NaCl in the sclerolac water-sol account for the sclerolac water-sol is 0.5%, 0.1%.
Adopt laser particle analyzer (PSS particle-size analyzer-380, U.S. Particle Sizing Systems company) to measure the particle diameter of the sclerolac water-sol that has added NaCl, Intensity median size is as shown in table 7.
Adopt nano particle size and Zeta potential analyser (NanoZS ZEN3600, Britain Malvern company) to measure the Zeta potential of the sclerolac water-sol, Zeta potential measurement result is as shown in table 7.
The particle diameter of the table 7 sclerolac water-sol, Zeta potential analytical results
Test-results shows: the sclerolac water-sol prepared by the present invention has good salt tolerance, in the sclerolac water-sol, adds after NaCl, and under 0.5%, 1% ionic intension, the median size of the water-sol changes little, does not assemble; Zeta potential only has very little reducing, and in the case of higher electrolyte ion exists, the water-sol is stable, shows that the sclerolac water-sol prepared by the present invention has higher stability, preferably salt tolerance.
The light transmission test of test example 7 water-sols
Get respectively sclerolac water-sol 5ml prepared by embodiment 1-4 in quartz colorimetric utensil, be placed in ultraviolet spectrophotometer (U.S. Beckman Coulter Inc., DU800 type), in the interscan of 200nm ~ 800nm scope, the transmittance of measuring the sclerolac water-sol, measurement result is as shown in table 8.
The transmittance analytical results of the table 8 sclerolac water-sol
| Transmittance (%) | |
| |
70 |
| Embodiment 2 | 75 |
| Embodiment 3 | 80 |
| Embodiment 4 | 65 |
Test-results shows: this is tested the prepared lac water-sol and has good light transmission, at 800nm place, visible region, the transmittance of the sclerolac water-sol prepared by the present invention is more than 60%, transmittance reaches 65-80%, and transmittance height has also embodied the water-sol prepared by the present invention and had a good dispersiveness.
Claims (6)
1. a preparation method for the sclerolac water-sol, comprises as follows step in sequence:
1) sclerolac is joined in ethanol, dissolve, make sclerolac ethanolic soln, wherein, the weight part proportioning of described sclerolac and ethanol is 2～9:98～91;
2) under whipped state, sclerolac ethanolic soln is joined in deionized water, make sclerolac collagen solution, wherein, stirring velocity is 6000～10000rpm, described sclerolac ethanolic soln joins in described deionized water with the form of the liquid stream of diameter 4-6mm, and described sclerolac ethanolic soln is 1:3～10 with the ratio of the volume of described deionized water;
3) sclerolac collagen solution is distilled to processing, remove ethanol, concentrated, obtain.
2. preparation method as claimed in claim 1, is characterized in that step 2) described in the interpolation speed of sclerolac ethanolic soln be 3～15ml/min.
3. preparation method as claimed in claim 1 or 2, is characterized in that described in step 3), distillation is treated to underpressure distillation processing.
4. preparation method as claimed in claim 3, is characterized in that in described underpressure distillation treating processes, controlling temperature is 35～50 ℃; Absolute pressure is 0.02～0.04MPa.
5. preparation method as claimed in claim 1 or 2, is characterized in that step 3) is concentrated into 1/5～1/2 of its original volume by sclerolac collagen solution.
6. a sclerolac water-sol, is characterized in that being prepared from according to method as described in as arbitrary in claim 1-5.
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