CN102660139A - Preparation of high-quality arthamin yellow - Google Patents
Preparation of high-quality arthamin yellow Download PDFInfo
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- CN102660139A CN102660139A CN2012101547331A CN201210154733A CN102660139A CN 102660139 A CN102660139 A CN 102660139A CN 2012101547331 A CN2012101547331 A CN 2012101547331A CN 201210154733 A CN201210154733 A CN 201210154733A CN 102660139 A CN102660139 A CN 102660139A
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- elutriant
- yellow
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 15
- 238000010828 elution Methods 0.000 claims abstract description 10
- 238000000605 extraction Methods 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- 239000007788 liquid Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 23
- 239000000049 pigment Substances 0.000 claims description 19
- 235000003255 Carthamus tinctorius Nutrition 0.000 claims description 18
- 244000020518 Carthamus tinctorius Species 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 14
- 239000003112 inhibitor Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 9
- 238000005538 encapsulation Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 238000001179 sorption measurement Methods 0.000 claims description 9
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000001054 red pigment Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims description 4
- 229920000858 Cyclodextrin Polymers 0.000 claims description 4
- 239000001116 FEMA 4028 Substances 0.000 claims description 4
- 239000005913 Maltodextrin Substances 0.000 claims description 4
- 229920002774 Maltodextrin Polymers 0.000 claims description 4
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 4
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 4
- 229960004853 betadex Drugs 0.000 claims description 4
- 229940035034 maltodextrin Drugs 0.000 claims description 4
- 235000019983 sodium metaphosphate Nutrition 0.000 claims description 4
- 229940037003 alum Drugs 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 3
- 229960005055 sodium ascorbate Drugs 0.000 claims description 3
- 238000004440 column chromatography Methods 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003963 antioxidant agent Substances 0.000 abstract 1
- 230000003078 antioxidant effect Effects 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- WLYGSPLCNKYESI-RSUQVHIMSA-N Carthamin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@@]1(O)C(O)=C(C(=O)\C=C\C=2C=CC(O)=CC=2)C(=O)C(\C=C\2C([C@](O)([C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(O)=C(C(=O)\C=C\C=3C=CC(O)=CC=3)C/2=O)=O)=C1O WLYGSPLCNKYESI-RSUQVHIMSA-N 0.000 description 4
- DYQVDISPPLTLLR-HJQYTNQXSA-N Carthamin Natural products CC[C@H]1O[C@H]([C@H](O)[C@@H](O)[C@@H]1O)[C@]2(O)C(=C(C=C/3C(=O)C(=C(O)[C@](O)([C@@H]4O[C@H](CO)[C@@H](O)[C@H](O)[C@H]4O)C3=O)C(=O)C=Cc5ccc(O)cc5)C(=O)C(=C2O)C(=O)C=Cc6ccc(O)cc6)O DYQVDISPPLTLLR-HJQYTNQXSA-N 0.000 description 4
- 229930006000 Sucrose Natural products 0.000 description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 4
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- 238000005303 weighing Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
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- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
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- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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Landscapes
- Cosmetics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a preparation method of high-quality arthamin yellow, and the preparation method is characterized in that fresh arthamin is adopted as a raw material, continuous production of washing, slicing, extraction, filtering, column chromatography, color protection, concentration, color matching, ultrafiltration, microcapsulization, atomizing drying and mixed treatment is undertaken for the fresh arthamin, a arthamin yellow product is obtained by utilizing a method combining a macroporous resin staging elution process of a particular model number, pure water with particular conductivity and mixed antioxidant, the color value of the arthamin yellow product is more than or equal to 260, and the prepared arthamin yellow has characteristics of light resistance, heat resistance, stability and the like. The arthamin yellow is better than similar products standard both at home and abroad.
Description
Technical field
The present invention relates to the preparation method that a kind of natural safflower extracts the method, particularly a kind of high-quality Yellow Color TH-S of Yellow Color TH-S.
Background technology
It is gorgeous naturally that natural pigment has safety non-toxic, color, is loved by the people, and painted, the foreign exchange earning to food, medicine, healthcare products, fine chemical product brings huge economic benefit especially, and national governments and entrepreneur very pay close attention to.The natural carthamin yellow that from safflower, extracts also has characteristics such as cost is low, steady quality is reliable.At present the disclosed Yellow Color TH-S of China prepares the patent No. has 02133563.X, 03157479.3 etc.But the prepared pigment color value of the technology of preparing of existing Yellow Color TH-S is lower, also has pigment thermostability and light stability not strong simultaneously, and complicated process of preparation is not suitable for the shortcoming of large-scale industrial production.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high-quality Yellow Color TH-S is characterized in that the Yellow Color TH-S look valency that makes is high, and pigment thermostability and light stability are strong, and technology is simple, and large-scale industrial production is convenient in the production serialization.
The object of the invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise:
(1) extracts filtration
With safflower 500kg; With 3 tons/hour safflower is sent in the multi-function extractor by travelling belt; Press safflower: the acidic aqueous solution soaking and extracting of solution=1:15-30 4-8 hour, the PH=2.5-5 of acidic aqueous solution collects the Yellow Color TH-S aqueous solution at the multi-function extractor liquid outlet.The red pigment solution of collecting is filtered with diatomite filter, get clarifying Yellow Color TH-S liquid.
Wherein acidic aqueous solution is a kind of in Hydrocerol A, lactic acid, the acetic acid.
(2) column chromatography
With macroporous resin adsorption post on the clarifying Yellow Color TH-S liquid, the high 3m of post, diameter 0.8m, loaded resin 300kg, feed rate are 2-10kg/min, with the pure water cleaning of specific conductivity 20-30us.Then, with aqueous ethanolic solution wash-out, separation, extremely neutral with washed with de-ionized water again.
Wherein the model of adsorption resin column is a kind of among D101, DM-21, the NSA-9.
Wherein the classification wash-out is the gradient elution that carries out four-stage from capital, at the bottom of post, collects flow point, and elution requirement is:
Fs: it is 70% ethanol that the volume of elutriant is formed proportioning;
Subordinate phase: it is 60% ethanol that the volume of elutriant is formed proportioning;
Phase III: it is 50% ethanol that the volume of elutriant is formed proportioning;
Stage: it is 40% ethanol that the volume of elutriant is formed proportioning;
(3) protect look
Elutriant is collected in together, transfers between the pH3.5-6.0, add the inhibitor of 0.5%-2% again.
Wherein inhibitor is the mixture of 10%L-sodium ascorbate, 60% sodium-metaphosphate, 10% alum, 20% Hydrocerol A composition.
(4) concentrated and ultrafiltration
Elutriant is concentrated Yellow Color TH-S with being pumped into vacuum-evaporator, and vacuum tightness is 0.02-0.08MPa, and temperature is controlled at 40-80 ℃, treats that the Yellow Color TH-S liquor ratio weighs to stop to concentrate in 1.1 o'clock.Liquid concentrator is used ultrafiltration membrance filter.
(5) micro encapsulation
With behind the embedding medium dissolution filter with ultrafiltration after liquid concentrator mix, through high pressure homogenizer, make pigment composition parcel fully, homogenization pressure is 20-60MPa.
Wherein embedding medium is a kind of in maltodextrin, beta-cyclodextrin, the XG 550.
(6) spraying drying
With micro encapsulation pigment solution employing completely spraying drying, inlet temperature is 160-220 ℃, and temperature out is 70-90 ℃, obtains pale brown toner end product.
(7) mixing of sieving
The pale brown toner end product that the different batches spraying drying is obtained is through 80 purpose screen cloth and tramp iron separators, places the homogeneous Yellow Color TH-S product that obtains look valency >=250 behind the powder mixing machine thorough mixing to the powder after sieving then.
The pigment detection method:
1, look valency
(1) reagent and solution: zero(ppm) water
(2) plant and instrument: spectrophotometer.
(3) mensuration program: take by weighing sample 0.1g in little weighing bottle, place moisture eliminator, at room temperature dry 24h.Accurately weighing (claiming accurate to 1.0000g) is dissolved in the 100m1 volumetric flask,, shakes up, filters to scale with distilled water diluting.Filtrate in the 100m1 volumetric flask with pipette, extract l0ml, be diluted with water to scale, this liquid is as determined solution.Take out diluent and place the lcm cuvette,, make reference liquid, measure its absorbancy with zero(ppm) water with ultraviolet spectrophotometer and 400nm wavelength.
(4) calculation formula:
The look valency of sample is calculated as follows:
In the formula, A
1Absorbancy for the actual measurement sample.
G
1Be the sample quality of accurate weighing, g.
2, pigment rate of loss
(1) thermostability
Under 100 ℃ of condition of water bath heating of temperature; By look price ratio example is absorbancy 0.800 sample 1g (accurately to 0.0002g), adds in the 5% sucrose water of 500ml, observes colour-change after 2 hours; Use visible spectrophotometer; Make blank at wavelength 400nm place with 5% sucrose water, detect the absorbancy of trial-product, conversion is the pigment rate of loss according to absorbancy.
In the formula: A
1Be the absorbancy before the sample test;
A
2Be the absorbancy after the sample test.
(2) light stability
At 1m
3In the encloses container, 8 of the uv lamps of 40W are arranged, 8 of the fluorescent lamps of 40W; By look price ratio example absorbancy is the sample 1g (accurately to 0.0002g) of 0.800 (part by weight is 0.01%), adds in the 5% sucrose water of 500ml, observes colour-change after 24 hours; Use visible spectrophotometer; Sucrose water at wavelength 400nm place with 5% is made blank, detects the absorbancy of trial-product, and conversion is the pigment rate of loss according to absorbancy.
In the formula: A
1Be the absorbancy before the sample test;
A
2Be the absorbancy after the sample test.
The present invention has following advantage:
1, the invention provides a kind of look valency height, fast light, heat-resisting, stable sailor yellow edible natural pigment, applied range is an ideal food additives.
2, with short production cycle, equipment is simple, processing condition are gentle, the less investment instant effect, but the continuous large-scale suitability for industrialized production.
The waste water of 3, discharging returns respectively and recycles after flocculation, deposition, sterilization, stripped safflower residue with alkali neutralization, dehydration after, make medicinal material with the drying plant oven dry and sell, bring abundant added value.
4, three-waste free discharge, pollution-free in the production process is environmentally friendly; Raw material can extensively be planted, and remarkable economic efficiency and social benefit are arranged.
Specific embodiment
Embodiment 1:
(1) extracts filtration
With safflower 500kg; With 3 tons/hour safflower is sent in the multi-function extractor by travelling belt; Press safflower: the aqueous citric acid solution soaking and extracting of solution=1:22 6 hours, the PH=3.5 of acidic aqueous solution collects the Yellow Color TH-S aqueous solution at the multi-function extractor liquid outlet.The red pigment solution of collecting is filtered with diatomite filter, get clarifying Yellow Color TH-S liquid.
(2) column chromatography
With D101 macroporous resin adsorption post on the clarifying Yellow Color TH-S liquid, the high 3m of post, diameter 0.8m, loaded resin 300kg, feed rate are 6kg/min, with the pure water cleaning of specific conductivity 25us.Then, with aqueous ethanolic solution wash-out, separation, extremely neutral with washed with de-ionized water again.
Wherein the classification wash-out is the gradient elution that carries out four-stage from capital, at the bottom of post, collects flow point, and elution requirement is:
Fs: it is 70% ethanol that the volume of elutriant is formed proportioning;
Subordinate phase: it is 60% ethanol that the volume of elutriant is formed proportioning;
Phase III: it is 50% ethanol that the volume of elutriant is formed proportioning;
Stage: it is 40% ethanol that the volume of elutriant is formed proportioning;
(3) protect look
Elutriant is collected in together, transfers pH4.5, add 1.5% inhibitor again.
Wherein inhibitor is the mixture of 10%L-sodium ascorbate, 60% sodium-metaphosphate, 10% alum, 20% Hydrocerol A composition.
(4) concentrated and ultrafiltration
Elutriant is concentrated Yellow Color TH-S with being pumped into vacuum-evaporator, and vacuum tightness is 0.06MPa, and temperature is controlled at 60 ℃, treats that the Yellow Color TH-S liquor ratio weighs to stop to concentrate in 1.1 o'clock.Liquid concentrator is used ultrafiltration membrance filter.
(5) micro encapsulation
With behind the embedding medium maltodextrin dissolution filter with ultrafiltration after liquid concentrator mix, through high pressure homogenizer, make pigment composition parcel fully, homogenization pressure is 40MPa.
Wherein embedding medium is a kind of in maltodextrin, beta-cyclodextrin, the XG 550.
(6) spraying drying
With micro encapsulation pigment solution employing completely spraying drying, inlet temperature is 190 ℃, and temperature out is 80 ℃, obtains pale brown toner end product.
(7) mixing of sieving
The pale brown toner end product that the different batches spraying drying is obtained is through 80 purpose screen cloth and tramp iron separators, places the homogeneous Yellow Color TH-S product that obtains look valency >=250 behind the powder mixing machine thorough mixing to the powder after sieving then.
Embodiment 2:
(1) extracts filtration
With safflower 500kg, with 3 tons/hour safflower is sent in the multi-function extractor by travelling belt, press safflower: the lactic acid aqueous solution soaking and extracting of solution=1:15 4 hours, the PH=2.5 of acidic aqueous solution collects the Yellow Color TH-S aqueous solution at the multi-function extractor liquid outlet.The red pigment solution of collecting is filtered with diatomite filter, get clarifying Yellow Color TH-S liquid.
(2) column chromatography
With DM-21 macroporous resin adsorption post on the clarifying Yellow Color TH-S liquid, the high 3m of post, diameter 0.8m, loaded resin 300kg, feed rate are 2kg/min, with the pure water cleaning of specific conductivity 20us.Then, with aqueous ethanolic solution wash-out, separation, extremely neutral with washed with de-ionized water again.
Wherein the classification wash-out is with embodiment 1.
(3) protect look
Elutriant is collected in together, transfers pH3.5, add 0.5% inhibitor again.
Wherein inhibitor is with embodiment 1.
(4) concentrated and ultrafiltration
Elutriant is concentrated Yellow Color TH-S with being pumped into vacuum-evaporator, and vacuum tightness is 0.02MPa, and temperature is controlled at 40 ℃, treats that the Yellow Color TH-S liquor ratio weighs to stop to concentrate in 1.1 o'clock.Liquid concentrator is used ultrafiltration membrance filter.
(5) micro encapsulation
With behind the embedding medium beta-cyclodextrin dissolution filter with ultrafiltration after liquid concentrator mix, through high pressure homogenizer, make pigment composition parcel fully, homogenization pressure is 20MPa.
(6) spraying drying
With micro encapsulation pigment solution employing completely spraying drying, inlet temperature is 160 ℃, and temperature out is 70 ℃, obtains pale brown toner end product.
(7) mixing of sieving
The pale brown toner end product that the different batches spraying drying is obtained is through 80 purpose screen cloth and tramp iron separators, places the homogeneous Yellow Color TH-S product that obtains look valency >=250 behind the powder mixing machine thorough mixing to the powder after sieving then.
Embodiment 3:
(1) extracts filtration
With safflower 500kg, with 3 tons/hour safflower is sent in the multi-function extractor by travelling belt, press safflower: the aqueous acetic acid soaking and extracting of solution=1:30 8 hours, the PH=5 of acidic aqueous solution collects the Yellow Color TH-S aqueous solution at the multi-function extractor liquid outlet.The red pigment solution of collecting is filtered with diatomite filter, get clarifying Yellow Color TH-S liquid.
(2) column chromatography
With NSA-9 macroporous resin adsorption post on the clarifying Yellow Color TH-S liquid, the high 3m of post, diameter 0.8m, loaded resin 300kg, feed rate are 10kg/min, with the pure water cleaning of specific conductivity 30us.Then, with aqueous ethanolic solution wash-out, separation, extremely neutral with washed with de-ionized water again.
Wherein the classification wash-out is with embodiment 1.
(3) protect look
Elutriant is collected in together, transfers between the pH6.0, add 2% inhibitor again.
Wherein inhibitor is with embodiment 1.
(4) concentrated and ultrafiltration
Elutriant is concentrated Yellow Color TH-S with being pumped into vacuum-evaporator, and vacuum tightness is 0.08MPa, and temperature is controlled at 80 ℃, treats that the Yellow Color TH-S liquor ratio weighs to stop to concentrate in 1.1 o'clock.Liquid concentrator is used ultrafiltration membrance filter.
(5) micro encapsulation
With behind the embedding medium XG 550 dissolution filter with ultrafiltration after liquid concentrator mix, through high pressure homogenizer, make pigment composition parcel fully, homogenization pressure is 60MPa.
(6) spraying drying
With micro encapsulation pigment solution employing completely spraying drying, inlet temperature is 220 ℃, and temperature out is 90 ℃, obtains pale brown toner end product.
(7) mixing of sieving
The pale brown toner end product that the different batches spraying drying is obtained is through 80 purpose screen cloth and tramp iron separators, places the homogeneous Yellow Color TH-S product that obtains look valency >=250 behind the powder mixing machine thorough mixing to the powder after sieving then.
Embodiment 4:
With embodiment 1, wherein the model of adsorption resin column is D1400.
Wherein the classification wash-out is the gradient elution that carries out four-stage from capital, at the bottom of post, collects flow point, and elution requirement is:
Fs: it is 60% ethanol that the volume of elutriant is formed proportioning;
Subordinate phase: it is 40% ethanol that the volume of elutriant is formed proportioning;
Collect the flow point in two stages.
Wherein pure electrical conductivity of water is 40ms.
Obtain the natural carthamin yellow powder-product.
Embodiment 5:
With embodiment 2, wherein inhibitor is the mixture that 50% sodium-metaphosphate, 50% Hydrocerol A are formed.
Obtain the natural carthamin yellow powder-product.
Embodiment 6:
With embodiment 3, wherein the model of adsorption resin column is LX-60.
Wherein the classification wash-out is to carry out wash-out from capital, at the bottom of post, collects flow point, and elution requirement is: it is 60% ethanol that the volume of elutriant is formed proportioning.
Wherein pure electrical conductivity of water is 10ms.
Inhibitor Hydrocerol A wherein.
Obtain the natural carthamin yellow powder-product.
Each embodiment quality examination result:
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| The look valency | 263.9 | 263.8 | 263.7 | 218.9 | 263.8 | 200.5 |
| Productive rate | 7.98% | 7.96% | 7.94% | 6.03% | 7.96% | 5.36% |
| Heat loss rate | 2.3% | 2.5% | 2.6% | 2.3% | 7.6% | 10.5% |
| The light loss rate | 0.8% | 0.9% | 0.9% | 0.8% | 6.9% | 11.6% |
Can find out that from the test result of above embodiment the macroporous resin that the present invention has utilized model is the technology of wash-out stage by stage, the pure water of particular electrical conductance and the method for mixing the inhibitor coupling; It is high to have obtained a kind of look valency; Productive rate is high, fast light, heat-resisting, more stable Yellow Color TH-S.
Claims (7)
1. the preparation method of a high-quality Yellow Color TH-S; With safflower 500kg; With 3 tons/hour safflower is sent in the multi-function extractor by travelling belt; Press safflower: the acidic aqueous solution extraction of solution=1:15-30, the PH=2.5-5 of acidic aqueous solution collects the Yellow Color TH-S aqueous solution at the multi-function extractor liquid outlet; The red pigment solution of collecting is filtered with diatomite filter, get clarifying Yellow Color TH-S liquid; With macroporous resin adsorption post on the clarifying Yellow Color TH-S liquid, the high 3m of post, diameter 0.8m, loaded resin 300kg, feed rate is 2-10kg/min, cleans with pure water; Then, with aqueous ethanolic solution wash-out, separation, extremely neutral with washed with de-ionized water again; Elutriant is collected in together, transfers between the pH3.5-6.0, add the inhibitor of 0.5%-2% again; Elutriant is concentrated Yellow Color TH-S with being pumped into vacuum-evaporator, and vacuum tightness is 0.02-0.08MPa, and temperature is controlled at 40-80 ℃, treats that the Yellow Color TH-S liquor ratio weighs to stop to concentrate in 1.1 o'clock, and liquid concentrator is used ultrafiltration membrance filter; With behind the embedding medium dissolution filter with ultrafiltration after liquid concentrator mix, through high pressure homogenizer, make pigment composition parcel fully, homogenization pressure is 20-60MPa; With micro encapsulation pigment solution employing completely spraying drying, inlet temperature is 160-220 ℃, and temperature out is 70-90 ℃, obtains pale brown toner end product; The pale brown toner end product that the different batches spraying drying is obtained is through 80 purpose screen cloth and tramp iron separators, places the homogeneous Yellow Color TH-S product that obtains look valency >=250 behind the powder mixing machine thorough mixing to the powder after sieving then.
2. the preparation method of a kind of high-quality Yellow Color TH-S as claimed in claim 1 is characterized by: acidic aqueous solution is a kind of in Hydrocerol A, lactic acid, the acetic acid.
3. the preparation method of a kind of high-quality Yellow Color TH-S as claimed in claim 1 is characterized by: the model of adsorption resin column is a kind of among D101, DM-21, the NSA-9.
4. the preparation method of a kind of high-quality Yellow Color TH-S as claimed in claim 1, it is characterized by: the classification wash-out is the gradient elution that carries out four-stage from capital, at the bottom of post, collects flow point, elution requirement is:
Fs: it is 70% ethanol that the volume of elutriant is formed proportioning;
Subordinate phase: it is 60% ethanol that the volume of elutriant is formed proportioning;
Phase III: it is 50% ethanol that the volume of elutriant is formed proportioning;
Stage: it is 40% ethanol that the volume of elutriant is formed proportioning;
Collect the flow point of four-stage.
5. the preparation method of a kind of high-quality Yellow Color TH-S as claimed in claim 1, it is characterized by: pure electrical conductivity of water is 20-30ms.
6. the preparation method of a kind of high-quality Yellow Color TH-S as claimed in claim 1 is characterized by: inhibitor is the mixture that 10%L-sodium ascorbate, 60% sodium-metaphosphate, 10% alum, 20% Hydrocerol A are formed.
7. the preparation method of a kind of high-quality Yellow Color TH-S as claimed in claim 1 is characterized by: embedding medium is a kind of in maltodextrin, beta-cyclodextrin, the XG 550.
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| CN102660139B (en) | 2013-09-11 |
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