CN102408832B - Method for beaching shellac using chlorine dioxide and alcohol solvent, and application thereof - Google Patents
Method for beaching shellac using chlorine dioxide and alcohol solvent, and application thereof Download PDFInfo
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- CN102408832B CN102408832B CN2011102359532A CN201110235953A CN102408832B CN 102408832 B CN102408832 B CN 102408832B CN 2011102359532 A CN2011102359532 A CN 2011102359532A CN 201110235953 A CN201110235953 A CN 201110235953A CN 102408832 B CN102408832 B CN 102408832B
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- shellac
- lac
- bleaching
- white shellac
- white
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- 229920001800 Shellac Polymers 0.000 title claims abstract description 110
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- 229940113147 shellac Drugs 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000002904 solvent Substances 0.000 title claims abstract description 19
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 title abstract 8
- 239000004155 Chlorine dioxide Substances 0.000 title abstract 4
- 235000019398 chlorine dioxide Nutrition 0.000 title abstract 4
- 238000004061 bleaching Methods 0.000 claims abstract description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 15
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000003292 glue Substances 0.000 claims description 37
- 150000002978 peroxides Chemical class 0.000 claims description 24
- 239000000460 chlorine Substances 0.000 claims description 18
- 229910052801 chlorine Inorganic materials 0.000 claims description 18
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 17
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 239000007844 bleaching agent Substances 0.000 claims description 7
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 2
- DXRKLUVKXMAMOV-UHFFFAOYSA-N 3-heptadecylcatechol Chemical compound CCCCCCCCCCCCCCCCCC1=CC=CC(O)=C1O DXRKLUVKXMAMOV-UHFFFAOYSA-N 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 3
- 230000033228 biological regulation Effects 0.000 abstract description 2
- 238000002835 absorbance Methods 0.000 abstract 1
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 24
- 239000004146 Propane-1,2-diol Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 10
- RHAXKFFKGZJUOE-UHFFFAOYSA-N 7-acetyl-6-ethyl-3,5,8-trihydroxy-9,10-dioxoanthracene-1,2-dicarboxylic acid Chemical compound O=C1C2=CC(O)=C(C(O)=O)C(C(O)=O)=C2C(=O)C2=C1C(O)=C(CC)C(C(C)=O)=C2O RHAXKFFKGZJUOE-UHFFFAOYSA-N 0.000 description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical group [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000006298 dechlorination reaction Methods 0.000 description 5
- 229960000935 dehydrated alcohol Drugs 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000003637 basic solution Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- PKTBUSPVTXIOCN-QHIUXXQWSA-N 4-{[4-(dimethylamino)phenyl]diazenyl}phenyl-beta-lactoside Chemical compound C1=CC(N(C)C)=CC=C1N=NC(C=C1)=CC=C1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)[C@@H](CO)O1 PKTBUSPVTXIOCN-QHIUXXQWSA-N 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- -1 makeup Substances 0.000 description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
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- CUXYLFPMQMFGPL-UHFFFAOYSA-N (9Z,11E,13E)-9,11,13-Octadecatrienoic acid Natural products CCCCC=CC=CC=CCCCCCCCC(O)=O CUXYLFPMQMFGPL-UHFFFAOYSA-N 0.000 description 1
- WSASFFHWOQGSER-MUAIWGBPSA-N 82xgf31q2y Chemical group C1[C@@]23[C@H](C(O)=O)CC[C@H]2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O WSASFFHWOQGSER-MUAIWGBPSA-N 0.000 description 1
- 206010009866 Cold sweat Diseases 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 241001516928 Kerria lacca Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
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- 238000003379 elimination reaction Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for beaching shellac using chlorine dioxide and an alcohol solvent. The method comprises the following steps of: dissolving shellac using the alcohol solvent into solution, adding chlorine dioxide to the solution under the condition of constant temperature and stirring the solution for bleaching for certain time, thereby obtaining bleached shellac solution; adding dilute sulphuric acid to the bleached shellac solution so that the bleached shellac is separated out, and then repeatedly washing the bleached shellac until the pH of washing water is neutral; and drying the shellac at the room temperature, thus obtaining the bleached shellac, wherein the absorbance of the ethanol solution in the position of 490 nm can be reduced to 1.6% of the raw material shellac, while the color index thereof can be reduced to be less than 0.5#; and other technical indexes are capable of meeting the requirements of the refined bleached shellac level I. The method is characterized in that: bleaching conditions are mild; a non-alkaline condition is adopted; the bleaching temperature is low; the dosage of an acidic precipitator is low; the color index of the obtained bleached shellac is low; and accurate control and regulation can be performed by adjusting the dosage of the chlorine dioxide, etc; therefore, the application of the bleached shellac in special fields can be extended.
Description
Technical field
The present invention relates to a kind of method and application thereof of dioxide peroxide alcoholic solvent white shellac.
Background technology
Lac also is shellac, is that tachardia lacca colonizes on host plant and to draw secretion a kind of red-purple colloid out after resin, is the natural condenses that the components such as eleostearic acid, shellolic acid form.Because it has reddish brown color and luster, film-forming properties and prevents steam breathability, often be used to extract natural pigment, manufacture furniture lacquer and insulating material.
The contained component of lac is different slightly different because of the place of production, but usually contains about 67.9% C, 9.1% H and 23.0% O, and its molecular formula meets empirical formula (C
4H
6O)
n, the relative molecular mass of bright shellac (uncured shellac) is approximately 1000, and the n value that goes out in the shellac molecular formula of deducibility is approximately 15 according to this, is generally 6-22.Average each shellac molecule contains carboxyl, three ester bonds, 5 hydroxyls and an aldehyde radical freely.Owing to containing these groups, spontaneous aging or polymerization can occur in shellac, makes the pure dissolubility reduction corresponding to steam breathability of shellac.
Along with the expansion of light lac in aspect purposes such as food, medicine, makeup, dyestuff, coating, fresh-keeping and tackiness agents, the demand to white shellac on market enlarges increasingly.White shellac is destroyed contained color substance in lac by SYNTHETIC OPTICAL WHITNER, makes the product of lac light.The SYNTHETIC OPTICAL WHITNER of applying at most is NaClO, and typical bleaching process is that the lac raw material is dissolved in to Na
2CO
3In the aqueous solution, with NaClO, bleach this aqueous solution after elimination impurity, then through acid precipitation, go out to bleach glue, then become product through washing, drying.The catalysis of the chlorine that bleaching process is introduced and residual bronsted lowry acids and bases bronsted lowry and the effect of being heated, thereby the polymerization of lac has aggravated its performance degradation, shortened dramatically its storage period, and in application, occur that solvability reduces, film forming is dry slow and cause film to feel like jelly and the problem such as be clamminess.
Under this background, in the lac bleaching process, finding gentle bleaching and analysing the adhesive tape part just becomes the focus of technical study with the preparation method who obtains high whiteness and high-storage stability white shellac.In recent years, the technology development work carried out in this field mainly concentrates on the technical scheme of 3 types: (1) is at traditional NaClO/Na
2CO
3In the basic solution bleaching process, introduce dechlorination process or add stablizer; (2) at traditional NaClO/Na
2CO
3In the basic solution bleaching process, improve the pH value that the acidifying of bleaching glue is separated out; (3) find new SYNTHETIC OPTICAL WHITNER/solvent system and improve conditions of bleaching.Chinese invention patent application (CN101191034A) discloses a kind of preparation method of bleached shellac, employing be traditional NaClO/Na
2CO
3The basic solution bleaching process increases the hydrogen peroxide dechlorination process; The preparation method of the disclosed a kind of low-chlorine bleach lac of Chinese invention patent application (101157828A) has increased sodium ethylate afterreaction operation after traditional bleaching process; Chinese invention patent application (CN1778853A) discloses a kind of shellac rapid bleach and dechlorination method, and being has increased intensification (85-95 ℃) dechlorination process in traditional bleaching process; Chinese invention patent application (CN1377592A) discloses a kind of refined edible lac and preparation method thereof, the mixing such as clorox, Textone, ozone and dioxide peroxide are floated to agent and be combined in traditional lac bleaching process, and in the finished product, added the stablizers such as sodium borohydride.The 1st type of technology is by reducing the cl content in white shellac or utilizing the stabilization of stablizer, period of storage and the thermostability of white shellac have been improved to a certain extent, but improving to some extent in the alkaline high-temperature bleaching of traditional lac bleaching process and low pH not being analysed to the adhesive tape part of mistake, and depend on complicated mixing and float agent system and loaded down with trivial details dechlorination reaction operation, add stablizer and cause that in addition white shellac viscosity increases, and then affect the risk of time of drying and the final performance of product.
The United States Patent (USP) (US6348217B1) of take is the technology of the 2nd type of representative, when shellac is stablized in preparation, still adopts traditional NaClO/Na
2CO
3The basic solution bleaching process, its technological improvement is mainly that glue pH value is analysed in the acidifying promoted as much as possible after lac is bleached, namely preferably in the solution of pH5.2-5.5, carry out separating out of shellac particle, this pH value is higher than the representative value pH4.1-4.5 of traditional bleaching process, and gained is stablized the shellac particle than common shellac stability in storage is better, the life-span is longer, coating hardness is larger.But this technology is had relatively high expectations to analysing glue pH value control accuracy, analyses the too high difficulty that will increase shellac consumption and increase follow-up dehydration of glue pH, analyses the too low product life of glue pH shorter again.The Chinese patent application (92105048.8) of take is carried out the lac bleaching by sodium chlorate as the 3rd type of technology of representative in ethanol system, its technical characterictic is to change the water solution system of traditional bleaching process into ethanol system, the alkalescence bleaching changes the pH neutrallty condition into and has also reduced simultaneously bleaching temperature, the color index of white shellac is hanged down the gentleness of conditions of bleaching and thermostability improves to some extent, but the problem existed is, SYNTHETIC OPTICAL WHITNER sodium chlorate used
Solubleness in ethanol is lower, and the bleaching efficiency that has affected this system has extended bleaching time.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of dioxide peroxide alcoholic solvent bleaching is provided
The method of lac, this be a kind of technique and SYNTHETIC OPTICAL WHITNER simple, bleach and analyse the lac bleaching method that the adhesive tape part is gentle, bleaching efficiency is high and the bleaching degree is controlled.
The present invention is achieved through the following technical solutions:
The dissolving of A, lac: add in proportion the alcoholic solvent preparation in lac (dewaxing sheet glue or seed lac)
Become shellac solution, described alcoholic solvent is methyl alcohol, ethanol and propyl alcohol, and preferred alcoholic solvent is ethanol; Described alcoholic solvent: lac (ratio of mass parts) is 2-8, and preferred alcoholic solvent: the lac ratio is 3-5.
The bleaching of B, lac: add by a certain percentage dioxide peroxide in constant temperature and control in above-mentioned shellac solution
PH value processed forms the bleaching glue after the lower stirring bleaching scheduled time.The available chlorine content of described dioxide peroxide is 5g/L-40g/L, and preferred dioxide peroxide available chlorine is 20g-30g/L; The adding proportion of described dioxide peroxide is ClO
2/ lac (mL/g) is than being 2-16, the add-on ClO of preferred dioxide peroxide
2/ lac (mL/g) is than being 8-12; The steady temperature of described lac bleaching is 20-80
0C, preferred steady temperature is 60-70
0C; During described lac bleaching, pH should be controlled at 4.0-7.0, and preferred pH should be controlled at 4.0-6.0; The stirring bleaching scheduled time of described lac bleaching is 0.5-8h, and the preferred stirring bleaching scheduled time is 2-4h.
Separating out of C, white shellac: the pH value that adds dilute sulphuric acid to regulate the bleaching glue makes to bleach glue and separates out.Described to make the dilute sulphuric acid that white shellac is separated out be that mass percentage concentration is the dilute sulphuric acid of 0.5-10%, preferably the dilute sulphuric acid of 3-5%; The pH value of the described bleaching glue of controlling when adding dilute sulphuric acid white shellac being separated out should be between 2-4, preferably the pH value 3-4 that should be situated between.
The rinsing of D, white shellac is with dry: after water repeatedly rinses white shellac to washing water and is neutrality, and Vac-dry sheliac under room temperature.
Method provided by the invention is all applicable to regular bleached lac and refined bleached lac, and the white shellac color index can accurately regulate and control by regulating Chlorine.
The mensuration product hierarchy that the color index of gained white shellac of the present invention and other technology refer to is distinguished and is carried out with reference to GB8140-87 and GB8143-87, due to the color index employing is the dilution visual method mensuration of lac ethanolic soln and iodine standard solution, (maximum absorption wavelength of iodine is 460nm because there are larger difference in lac and iodine liquid absorption spectrum curve, and the Lac dye maximum absorption wavelength is 490nm, the lac ethanolic soln absorption peak do not occur at the 490nm place in addition) and naked eyes measurement result difference that color sensitivity difference is brought, the present invention also utilizes ultraviolet-visible pectrophotometer (752-ultraviolet-visible pectrophotometer, Shanghai essence science and technology Instrument Ltd.) measured raw material lac and gained white shellac at 490nm(Lac dye maximum absorption wavelength) locate absorbancy
E 490variation, utilize
E 490%(
E 490conservation rate=bleaching glue
E 490/ raw material lac
E 490* 100%) carry out the bleaching degree of quantitatively characterizing lac.
The present invention compared with prior art has the following advantages and effect: (1) adopts technical scheme of the present invention can under gentle condition, realize the lac bleaching and separate out, specifically can under neutrality or solutions of weak acidity, realize the bleaching of lac and separate out, be conducive to the raising of white shellac stability; (2) in alcoholic solvent, can realize that raw material lac and dioxide peroxide float the abundant dissolving of agent, improve bleaching efficiency, shortened bleaching time and promoted the whiteness of white shellac; (3) bleaching process and SYNTHETIC OPTICAL WHITNER formula are simple, without adding the lac stability additive; (4) the white shellac color index can be able to accurate regulation and control by regulating Chlorine.Adopt the white shellac that technical scheme of the present invention obtains can meet the technical indicator of white shellacs at different levels in the concerned countries standard, thereby increased the range of application of white shellac in each field.
The accompanying drawing explanation
Fig. 1 is the absorption spectrum curve (5.1g/L ethanolic soln) of lac and white shellac, and wherein 1 is the raw material lac, and 2 is the white shellac of embodiment 3, and 3 is the white shellac of embodiment 5, and 5 is the white shellac of embodiment 7.
Fig. 2 is dioxide peroxide/lac comparison white shellac
E 490The impact of conservation rate and color index.
The present invention will be further described in detail below in conjunction with the drawings and specific embodiments.
Embodiment
Get 100g shellac (commercially available first class shellac, color is red-purple, color index≤No. 18) and the 300g dehydrated alcohol mix, water bath with thermostatic control is warming up to 65 ℃, mixture is put into water-bath and is fully stirred and be made into the lac ethanolic soln that mass ratio is 1:3, add 210mL dioxide peroxide (commercially available industrial goods), available chlorine content is 10g/L, in bleaching process, control pH between 4.0-6.0, in 65 ℃ of lower constant temperature, stir bleaching 2h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is 5% dilute sulphuric acid, the pH value of regulating the bleaching glue is 3, and make white shellac be cotton-shaped to separate out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is deep yellow, its ethanolic soln is in the absorbancy of 490nm
E 490for 45.1% of raw material shellac, color index is 11.
Get 100g shellac (commercially available first class shellac, color is red-purple, color index≤No. 18) and the 500g dehydrated alcohol mix, water bath with thermostatic control is warming up to 70 ℃, mixture is put into water-bath and is fully stirred and be made into the lac methanol solution that mass ratio is 1:5, add 420mL dioxide peroxide (commercially available industrial goods), available chlorine content is 20g/L, in bleaching process, control pH between 4.0-6.0, in 70 ℃ of lower constant temperature, stir bleaching 4h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is that the pH value that 3% dilute sulphuric acid is regulated the bleaching glue is 4, making white shellac be cotton-shaped separates out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is yellow,
E 490for 11.3% of stick lac sheet, color index is 4.
Embodiment 3
Get 100g shellac (commercially available first class shellac, color is red-purple, color index≤No. 18) and the 200g dehydrated alcohol mix, water bath with thermostatic control is warming up to 80 ℃, mixture is put into water-bath and is fully stirred and be made into the lac ethanolic soln that mass ratio is 1:2, add 595mL dioxide peroxide (commercially available industrial goods), available chlorine content is 20g/L, in bleaching process, control pH between 4.0-7.0, in 80 ℃ of lower constant temperature, stir bleaching 1h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is that the pH value that 10% dilute sulphuric acid is regulated the bleaching glue is 2, making white shellac be cotton-shaped separates out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is light yellow,
E 490for 9.6% of stick lac sheet, color index is 3.
Get 100g shellac (commercially available first class shellac, color is red-purple, color index≤No. 18) and the 800g dehydrated alcohol mix, water bath with thermostatic control is warming up to 20 ℃, mixture is put into water-bath and is fully stirred and be made into the lac ethanolic soln that mass ratio is 1:8, add 800mL dioxide peroxide (commercially available industrial goods), available chlorine content is 20g/L, in bleaching process, control pH between 4.0-6.0, in 20 ℃ of lower constant temperature, stir bleaching 8h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is 1% dilute sulphuric acid, the pH value of regulating the bleaching glue is 3, and make white shellac be cotton-shaped to separate out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is light yellow,
E 490for 7.2% of stick lac sheet, color index is 2, and all the other technical indicators meet GB8140-87 refined bleached lac (II level) requirement.
Embodiment 5
Get 100g shellac (commercially available first class graning lac, color is red-purple, color index≤No. 18) and the 400g anhydrous methanol mix, water bath with thermostatic control is warming up to 60 ℃, mixture is put into water-bath and is fully stirred and be made into the lac ethanolic soln that mass ratio is 1:4, add 1050mL dioxide peroxide (commercially available industrial goods), available chlorine content is 30g/L, in bleaching process, control pH between 4.0-6.0, in 60 ℃ of lower constant temperature, stir bleaching 3h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is 4% dilute sulphuric acid, the pH value of regulating the bleaching glue is 3, and make white shellac be cotton-shaped to separate out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is light yellow,
E 490for 4.1% of stick lac sheet, color index is 1, and all the other technical indicators meet GB8140-87 refined bleached lac (I level) requirement.
Get 100g shellac (commercially available first class graning lac, color is red-purple, color index≤No. 18) and the anhydrous propyl alcohol of 300g mix, water bath with thermostatic control is warming up to 65 ℃, mixture is put into water-bath and is fully stirred and be made into the lac ethanolic soln that mass ratio is 1:3, add 1270mL dioxide peroxide (commercially available industrial goods), available chlorine content is 35g/L, in bleaching process, control pH between 4.0-6.0, in 65 ℃ of lower constant temperature, stir bleaching 5h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is that the pH value that 5% dilute sulphuric acid is regulated the bleaching glue is 3, making white shellac be cotton-shaped separates out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is white,
E 490for 1.7% of stick lac sheet, color index≤0.5, all the other technical indicators meet GB8140-87 refined bleached lac (I level) requirement.
Embodiment 7
Get 100g shellac (commercially available first class graning lac, color is red-purple, color index≤No. 18) and the 300g dehydrated alcohol mix, water bath with thermostatic control is warming up to 65 ℃, mixture is put into water-bath and is fully stirred and be made into the lac ethanolic soln that mass ratio is 1:3, add 1600mL dioxide peroxide (commercially available industrial goods), available chlorine content is 40g/L, in bleaching process, control pH between 4.0-6.0, in 65 ℃ of lower constant temperature, stir bleaching 3h and obtain bleaching glue, in bleaching, adding mass percentage concentration in glue is that the pH value that 3% dilute sulphuric acid is regulated the bleaching glue is 3, making white shellac be cotton-shaped separates out, then after water repeatedly rinses and separates out lac to washing water pH value and be 7, be filtered dry, at room temperature dry more than 7 days, obtain white shellac, color is white
E 490for 1.6% of stick lac sheet, color index≤0.5, all the other technical indicators meet GB8140-87 refined bleached lac (I level) requirement.
From embodiment, finding out that the gained white shellac is along with the difference of floating the agent Chlorine, its color gradually changes, can obtain the white shellac of different mass requirement, embodiment 5-7 the white shellac color that all can meet GB white shellacs at different levels refer to tree and other technical requirement.
What Fig. 1 showed is the absorption spectrum curve of raw material lac and white shellac ethanolic soln, can find out that therefrom the absorption peak of Lac dye does not all appear in raw material lac and white shellac at the 490nm place, but, along with white shellac has significantly and reduces the equal collagen material of the absorbancy at each wavelength place lac, lac is bleached to the realization of purpose from the technology adopted another angle proved invention.Fig. 2 has shown dioxide peroxide/lac comparison white shellac
E 490Conservation rate affect rule, result shows white shellac
E 490Conservation rate reduces along with the increasing of floating the agent Chlorine, when
E 490After being less than 4.1%, the white shellac color index can meet the requirement of GB I level white shellac, also from the another one angle, show, can by regulating Chlorine, accurately regulate and control the color index of white shellac to meet the requirement of different stage white shellac in technology of the present invention.
Claims (8)
1. the method for a dioxide peroxide alcoholic solvent white shellac, it is characterized in that carrying out as follows: the dissolving of (1) lac: will take off cured graning lac or sheet and be dissolved in by a certain percentage in alcoholic solvent and form solution, described alcoholic solvent is 2-8:1 with the ratio of the mass parts of lac; (2) bleaching of lac: dioxide peroxide is pressed to ClO
2Volume mL number: the amount of lac weight g number=2-16:1 is added in laccol solution, and the available chlorine content of dioxide peroxide is 5g/L-40g/L, forms the bleaching glue after pH is under 4.0-6.0,20-80 ℃ constant temperature, to stir bleaching 0.5-8h; (3) separating out of white shellac: in white shellac liquid, adding mass percentage concentration is that the pH value that the 0.5-10% dilute sulphuric acid is regulated the bleaching glue is 2-4, makes to bleach glue to separate out; (4) rinsing of white shellac is with dry: after water repeatedly rinses white shellac to washing water and is neutrality, dry under room temperature, obtain white shellac;
Wherein said alcoholic solvent is methyl alcohol, ethanol and propyl alcohol;
The ratio of described alcoholic solvent and lac is 3-5:1.
2. white shellac method according to claim 1, is characterized in that described alcoholic solvent is ethanol.
3. white shellac method according to claim 1, the adding proportion that it is characterized in that dioxide peroxide is ClO
2: lac=8-12:1.
4. according to the described white shellac method of claim 1 or 3, the available chlorine content that it is characterized in that dioxide peroxide is 20g-30g/L.
5. white shellac method according to claim 1, is characterized in that the constant temperature of lac bleaching is 60-70 ℃.
6. white shellac method according to claim 1 or 5, it is characterized in that bleaching churning time is 2-4h.
7. white shellac method according to claim 1, is characterized in that using when lac is separated out the dilute sulphuric acid of 3-5%.
8. according to the described white shellac method of claim 1 or 7, it is characterized in that the pH value of bleaching glue when white shellac is separated out is between 3-4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072437A (en) * | 1992-06-21 | 1993-05-26 | 中国林业科学研究院资源昆虫研究所 | A kind of production method of bleached shellac |
| US6348217B1 (en) * | 2000-08-04 | 2002-02-19 | Mantrose-Haeuser Co. Inc. | Method for preparing stable bleached shellac |
| CN1377592A (en) * | 2002-04-24 | 2002-11-06 | 陈东海 | Refined edible lac and its preparing method |
| CN1778853A (en) * | 2004-11-18 | 2006-05-31 | 李琳 | Fast-speed lakh bleaching and antichlorating method |
-
2011
- 2011-08-17 CN CN2011102359532A patent/CN102408832B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072437A (en) * | 1992-06-21 | 1993-05-26 | 中国林业科学研究院资源昆虫研究所 | A kind of production method of bleached shellac |
| US6348217B1 (en) * | 2000-08-04 | 2002-02-19 | Mantrose-Haeuser Co. Inc. | Method for preparing stable bleached shellac |
| CN1377592A (en) * | 2002-04-24 | 2002-11-06 | 陈东海 | Refined edible lac and its preparing method |
| CN1778853A (en) * | 2004-11-18 | 2006-05-31 | 李琳 | Fast-speed lakh bleaching and antichlorating method |
Non-Patent Citations (3)
| Title |
|---|
| 紫胶的特性及应用;黄喜坚;《杭州化工》;20090315;第39卷(第1期);第11-15页 * |
| 陈骿声.《林产化工与产品》.《林产化工与产品》.化学工业出版社,2003,(第1版),第220页. * |
| 黄喜坚.紫胶的特性及应用.《杭州化工》.2009,第39卷(第1期),第. |
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