CN100383194C - Preparation method of liquid disperse dye - Google Patents
Preparation method of liquid disperse dye Download PDFInfo
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- CN100383194C CN100383194C CNB200410016439XA CN200410016439A CN100383194C CN 100383194 C CN100383194 C CN 100383194C CN B200410016439X A CNB200410016439X A CN B200410016439XA CN 200410016439 A CN200410016439 A CN 200410016439A CN 100383194 C CN100383194 C CN 100383194C
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- dispersed dye
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- 239000007788 liquid Substances 0.000 title abstract 5
- 239000000986 disperse dye Substances 0.000 title description 13
- 238000002360 preparation method Methods 0.000 title 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 32
- 239000011259 mixed solution Substances 0.000 claims description 29
- 239000012065 filter cake Substances 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- 239000006185 dispersion Substances 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 7
- 229920001732 Lignosulfonate Polymers 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 6
- 235000019357 lignosulphonate Nutrition 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000004043 dyeing Methods 0.000 abstract description 20
- 239000000047 product Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 93
- 239000008187 granular material Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- FOGYNLXERPKEGN-UHFFFAOYSA-N 3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfopropyl)phenoxy]propane-1-sulfonic acid Chemical class COC1=CC=CC(CC(CS(O)(=O)=O)OC=2C(=CC(CCCS(O)(=O)=O)=CC=2)OC)=C1O FOGYNLXERPKEGN-UHFFFAOYSA-N 0.000 description 6
- 239000012267 brine Substances 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 238000007639 printing Methods 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 235000021463 dry cake Nutrition 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 229920004933 Terylene® Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
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Abstract
The present invention discloses a method for preparing liquid dispersing dye. The crude product of the dispersing dye is obtained by reaction, and filtered cakes are obtained by pressing and filtering. Then, the filtered cakes are dissolved in organic solvent, and a dispersing agent is dissolved in water. The two kinds of solution are mixed under the condition of stirring to obtain mixed liquid which is heated and steamed to remove the organic solvent so that the liquid dispersing dye is obtained. The filtered cakes are dried before being dissolved for the best. The organic solvent can be propanone or ethanol. The present invention is characterized in that the filtered cakes are dissolved by using the organic solvent so that the dye can be sufficiently dispersed in the solvent in a molecular weight grade mode. The solution is mixed with the water solution of the dispersing agent to obtain the liquid dispersing dye with 10 to 100 nanometers of particles. The product has the advantages that dye absorption can be enhanced, the cost of the dispersing dye in a dyeing process can be reduced, an effect of high color for matching various kinds of dispersing dye can be particularly enhanced, dyeing technology can be simplified, and dyeing quality can be enhanced.
Description
Technical field
The present invention relates to a kind of manufacture method of dispersed dye, especially a kind of manufacture method of aqueous ultra-fine dispersed dye.
Background technology
Dispersed dye refer to be scattered in the dye in the dye bath in the presence of dispersion agent.Contain polar group in the molecule, but do not contain water soluble groups such as sulfonic group, carboxylic acid group, the dissolving of dispersed dye in water is atomic.Dispersed dye are used for the dyeing and the stamp of synthon such as terylene, polypropylene fibre, polyamide fibre and spandex, it is the broad-spectrum dyestuff of a class, it is mainly used in the printing and dyeing of terylene and BLENDED FABRIC thereof, therefore the development of dispersed dye is closely related with the increase day by day of terylene output, is maximum a kind of of all dyestuffs uses.
The former dyestuff of dispersed dye by reaction obtains will obtain filter cake through press filtration usually, obtains the dispersed dye finished product again after sand milling and spraying drying.Wherein sand milling technology has determined the granular size of dispersed dye finished products, and the granular size of the dispersed dye that obtain by above-mentioned technology generally about 2 microns, even through long-time sand milling, also is difficult to the granular size of dispersed dye is distributed to below 1 micron.And the granular size of dispersed dye directly has influence on painted cost and dyeing quality, and especially the assembly of widespread use mixes dispersed dye in the printing and dyeing, can influence the color and luster effect greatly because of the particle of dyestuff.The granular size that reduces dispersed dye can improve the color and luster effect of dyestuff, improves the exhaustion of dyestuff, reduces the cost of dispersed dye in the dyeing course, simplifies dyeing and improves dyeing quality.
Summary of the invention
The problem that quasi-solution of the present invention is determined provides a kind of manufacture method of dispersed dye, the particle diameter that makes dispersed dye improves the exhaustion of dyestuff in the 10-100 nanometer, reduces the cost of dispersed dye in the dyeing course, improve to piece together and mix dispersed dye color and luster effect, simplify dyeing and improve dyeing quality.
For addressing the above problem, the present invention by the following technical solutions: a kind of manufacture method of aqueous dispersed dye, it obtains filter cake by the dispersed dye crude product that reaction obtains through press filtration, it is further comprising the steps of:
A: described filter cake is dissolved in the organic solvent, obtains solution A;
B: dispersion agent is dissolved in the water, obtains solution B;
C: under agitation condition, solution A and solution B are mixed, obtain mixed solution C;
D: to mixed solution C heating, boil off the organic solvent among the described mixed solution C, obtain aqueous dispersed dye.
Filter cake preferably drying processing before dissolving among the above-mentioned steps a; Described organic solvent can be an acetone or alcohol, and the weight ratio of filter cake and acetone or alcohol is 1: 4;
The manufacture method of above-mentioned aqueous dispersed dye, the dispersion agent among the step b are Dispersant MF or dispersion agent sulfonated lignin.The weight ratio of dispersion agent and water is 1: 4.
The manufacture method of above-mentioned aqueous dispersed dye, the solution A of described step c and solution B mixing preferably join A in the solution B; Described stirring preferably adopts the emulsification shears to stir.
The manufacture method of above-mentioned aqueous dispersed dye, in the described steps d to the Heating temperature of mixed solution C for being heated to 90-98 ℃, in heat-processed, preferably stir.
Conventional dispersed dye manufacture method, the filter cake that the dispersed dye crude product obtains after press filtration forms fine and close disperse dyes granule, because intermolecular reactive force in the disperse dyes granule, by mechanical disintegration,, only can make disperse dyes granule be distributed to the 1-2 micron as technologies such as sand millings.And adopted the present invention program, promptly by filter cake is passed through to use organic solvent dissolution, make dyestuff fully be distributed in the solvent with molecular level, when the aqueous solution of this solution and dispersion agent, because solubility change, dispersed dye can be separated out again, at first generate nano level small-particle when separating out, because the effect of factors such as stirring, particularly a large amount of existence of dispersion agent, the dyestuff small-particle is wrapped up by dispersion agent rapidly, forms emulsified disperse dyes granule, stoped intergranular interaction and particulate further to be grown up, obtaining particle is the aqueous dispersed dye of 10～100 nanometers.The dispersed dye that adopt present method to obtain, the exhaustion that can improve dyestuff to reduce the cost of dispersed dye in the dyeing course, especially can improve and piece together the color and luster effect of mixing dispersed dye, simplifies dyeing and improves dyeing quality.In addition, add heat extraction organic solvent cyclically utilizing, so both can save production cost, can not cause environmental pollution again.
Embodiment
Embodiment 1
Dispersed dye crude product with reaction obtains obtains dyestuff filter cake (solid content about 50%) through press filtration, gets about 200 grams of filter cake, under 80 ℃ condition, dried through 2 hours, obtain 100 gram dry cakes, be dissolved in the 400 gram acetone, obtain 500 gram dispersed dye acetone soln A.Get 100 gram Dispersant MFs-2, be dissolved in the 400 gram water, obtain 500 gram MF-2 aqueous solution B.Under emulsification shears agitation condition, 500 gram dispersed dye acetone soln A are slowly joined among the 500 gram MF-2 aqueous solution B, and continue to stir, obtain 1000 gram mixed solution C.Mixed solution C slowly is warmed up to 93 ℃, at this moment progressively has acetone steam to come out, the acetone steam condensation is reclaimed.In acetone evaporated, also have the part moisture evaporation, can keep the skin wet in case of necessity.After 2 hours, obtain the aqueous dispersed dye of about 500 grams, wherein contain 100 gram dispersed dye, 100 gram Dispersant MFs-2, the disperse dyes granule size is between the 10-100 nanometer.The aforementioned aqueous dispersed dye finished product that obtains both can directly apply to printing and dyeing, also can be spray-dried, make solid disperse dye.
For piecing together the dispersed dye that mix, the dispersed dye filter cake of different varieties can be dissolved into simultaneously and obtain solution A in the acetone; Also can be dissolved into respectively in the acetone and obtain solution A after the mixing; Also can be dissolved into respectively in the acetone and the mixed solution that obtains the different varieties dyestuff after Dispersant MF-2 aqueous solution B mixes, the mixed solution of above-mentioned different varieties dyestuff be mixed obtaining mixed solution C.Then, make aqueous dispersed dye according to the method for narrating in the last paragraph.
Embodiment 2
Dispersed dye crude product with reaction obtains obtains dyestuff filter cake (solid content about 50%) through press filtration, gets about 200 grams of filter cake, under 80 ℃ condition, dried through 2 hours, obtain 100 gram dry cakes, be dissolved in the 400 gram acetone, obtain 500 gram dispersed dye acetone soln A.Get 100 gram dispersion agent sulfonated lignin, be dissolved in the 400 gram water, obtain 500 gram dispersion agent lignosulfonic acid salt brine solution B.Under emulsification shears agitation condition, 500 gram dispersed dye acetone soln A are slowly joined among the 500 gram dispersion agent lignosulfonic acid salt brine solution B, and continue to stir, obtain 1000 gram mixed solution C.Mixed solution C slowly is warmed up to 90 ℃, at this moment progressively has acetone steam to come out, the acetone steam condensation is reclaimed.In acetone evaporated, also have the part moisture evaporation, can keep the skin wet in case of necessity.After 2 hours, obtain the aqueous dispersed dye of about 500 grams, wherein contain 100 gram dispersed dye, 100 gram dispersion agent sulfonated lignin, the disperse dyes granule size is between the 10-100 nanometer.The aforementioned aqueous dispersed dye finished product that obtains both can directly apply to printing and dyeing, also can be spray-dried, make solid disperse dye.
For piecing together the dispersed dye that mix, the dispersed dye filter cake of different varieties can be dissolved into simultaneously and obtain solution A in the acetone; Also can be dissolved into respectively in the acetone and obtain solution A after the mixing; Also can be dissolved into respectively in the acetone and the mixed solution that obtains the different varieties dyestuff after dispersion agent lignosulfonic acid salt brine solution B mixes, the mixed solution of above-mentioned different varieties dyestuff be mixed obtaining mixed solution C.Then, make aqueous dispersed dye according to the method for narrating in the last paragraph.
Embodiment 3
Dispersed dye crude product with reaction obtains obtains dyestuff filter cake (solid content about 50%) through press filtration, gets about 200 grams of filter cake, under 80 ℃ condition, dried through 2 hours, obtain 100 gram dry cakes, be dissolved in the 400 gram ethanol, obtain 500 gram dispersed dye ethanolic soln A.Get 100 gram Dispersant MFs-2, be dissolved in the 400 gram water, obtain 500 gram MF-2 aqueous solution B.Under emulsification shears agitation condition, 500 gram dispersed dye ethanolic soln A are slowly joined among the 500 gram MF-2 aqueous solution B, and continue to stir, obtain 1000 gram mixed solution C.Mixed solution C slowly is warmed up to 98 ℃, at this moment progressively has alcohol vapour to come out, the alcohol vapour condensation is reclaimed.In ethanol evaporation, also have the part moisture evaporation, can keep the skin wet in case of necessity.After 2 hours, obtain the aqueous dispersed dye of about 500 grams, wherein contain 100 gram dispersed dye, 100 gram Dispersant MFs-2, the disperse dyes granule size is between the 10-100 nanometer.The aforementioned aqueous dispersed dye finished product that obtains both can directly apply to printing and dyeing, also can make solid disperse dye through spraying.
For piecing together the dispersed dye that mix, the dispersed dye filter cake of different varieties can be dissolved into simultaneously and obtain solution A in the ethanol; Also can be dissolved into respectively in the ethanol and obtain solution A after the mixing; Also can be dissolved into respectively in the ethanol and the mixed solution that obtains the different varieties dyestuff after Dispersant MF-2 aqueous solution B mixes, the mixed solution of above-mentioned different varieties dyestuff be mixed obtaining mixed solution C.Then, make aqueous dispersed dye according to the method for narrating in the last paragraph.
Embodiment 4
Dispersed dye crude product with reaction obtains obtains dyestuff filter cake (solid content about 50%) through press filtration, gets about 200 grams of filter cake, under 80 ℃ condition, dried through 2 hours, obtain 100 gram dry cakes, be dissolved in the 400 gram ethanol, obtain 500 gram dispersed dye ethanolic soln A.Get 100 gram dispersion agent sulfonated lignin, be dissolved in the 400 gram water, obtain 500 gram dispersion agent lignosulfonic acid salt brine solution B.Under emulsification shears agitation condition, 500 gram dispersed dye ethanolic soln A are slowly joined among the 500 gram dispersion agent lignosulfonic acid salt brine solution B, and continue to stir, obtain 1000 gram mixed solution C.Mixed solution C slowly is warmed up to 96 ℃, at this moment progressively has alcohol vapour to come out, the third ethanol vapor condensation is reclaimed.In ethanol evaporation, also have the part moisture evaporation, can keep the skin wet in case of necessity.After 2 hours, obtain the aqueous dispersed dye of about 500 grams, wherein contain 100 gram dispersed dye, 100 gram dispersion agent sulfonated lignin, the disperse dyes granule size is between the 10-100 nanometer.The aforementioned aqueous dispersed dye finished product that obtains both can directly apply to printing and dyeing, also can be spray-dried, make solid disperse dye.
For piecing together the dispersed dye that mix, the dispersed dye filter cake of different varieties can be dissolved into simultaneously and obtain solution A in the ethanol; Also can be dissolved into respectively in the ethanol and obtain solution A after the mixing; Also can be dissolved into respectively in the ethanol and the mixed solution that obtains the different varieties dyestuff after dispersion agent lignosulfonic acid salt brine solution B mixes, the mixed solution of above-mentioned different varieties dyestuff be mixed obtaining mixed solution C.Then, make aqueous dispersed dye according to the method for narrating in the last paragraph.
Behind the aqueous dispersed dye that make according to the method for embodiment 1-4, also can add conventional subsidiary material, as draw back powder, Sodium Benzoate, urea etc., satisfy application demand.
Claims (9)
1. the manufacture method of aqueous dispersed dye, it obtains filter cake by the dispersed dye crude product that reaction obtains through press filtration, it is characterized in that it is further comprising the steps of:
A: described filter cake is dissolved in the organic solvent, obtains solution A, described organic solvent is an acetone or alcohol;
B: dispersion agent is dissolved in the water, obtains solution B;
C: under agitation condition, solution A is slowly joined in the solution B, obtain mixed solution C;
D: to mixed solution C heating, boil off the organic solvent among the described mixed solution C, obtain aqueous dispersed dye.
2. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that filter cake drying before dissolving is handled among the described step a.
3. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that the weight ratio of filter cake and acetone or alcohol is 1: 4 among the described step a;
4. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that the dispersion agent among the described step b is Dispersant MF or dispersion agent sulfonated lignin.
5. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that the weight ratio of dispersion agent and water is 1: 4 among the described step b.
6. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that the solution A of described step c and solution B mixing are that solution A is joined in the solution B.
7. according to the manufacture method of claim 1 or 6 described aqueous dispersed dye, it is characterized in that the emulsification shears is adopted in the stirring of described step c.
8. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that in the described steps d stirring in the mixed solution C heat-processed.
9. the manufacture method of aqueous dispersed dye according to claim 1 is characterized in that in the described steps d that Heating temperature to mixed solution C is for being heated to 90-98 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410016439XA CN100383194C (en) | 2004-02-17 | 2004-02-17 | Preparation method of liquid disperse dye |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410016439XA CN100383194C (en) | 2004-02-17 | 2004-02-17 | Preparation method of liquid disperse dye |
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| CN1657570A CN1657570A (en) | 2005-08-24 |
| CN100383194C true CN100383194C (en) | 2008-04-23 |
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| CNB200410016439XA Expired - Fee Related CN100383194C (en) | 2004-02-17 | 2004-02-17 | Preparation method of liquid disperse dye |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040865A (en) * | 2009-10-14 | 2011-05-04 | 江南大学 | Preparation method of liquid ultra-fine dispersion dye |
| CN104448933B (en) * | 2014-12-31 | 2017-07-07 | 浙江闰土股份有限公司 | Red liquid disperse dyes and its preparation method and purposes |
| CN104530760B (en) * | 2014-12-31 | 2017-06-23 | 浙江闰土股份有限公司 | Red liquid disperse dyes and its preparation method and purposes |
| CN104530762B (en) * | 2014-12-31 | 2017-06-23 | 浙江闰土染料有限公司 | Orange liquid disperse dyes and its preparation method and purposes |
| CN104497631B (en) * | 2014-12-31 | 2017-06-06 | 浙江闰土股份有限公司 | Blue liquid disperse dyes and its preparation method and purposes |
| CN106380893A (en) * | 2016-08-25 | 2017-02-08 | 上海盛丘材料科技有限公司 | Preparation method and dyeing method of liquid disperse dye composition |
| CN107793792A (en) * | 2016-08-30 | 2018-03-13 | 江苏吉华化工有限公司 | A kind of preparation method of liquid ultra-fine dispersion dye |
| CN110499043B (en) * | 2018-05-17 | 2020-12-25 | 北京化工大学 | Preparation method of nano disperse dye |
| CN109054442A (en) * | 2018-09-17 | 2018-12-21 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of environment-friendly high-intensity liquid disperse dyes |
| CN109705619A (en) * | 2018-12-07 | 2019-05-03 | 浙江名毅新能源股份有限公司 | A kind of preparation method of superfine disperse dye |
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|---|---|---|---|---|
| CN1231843A (en) * | 1998-02-23 | 1999-10-20 | 霍夫曼-拉罗奇有限公司 | Preparation of finely divided pulverous carotenoid preparation |
| CN1302559A (en) * | 1999-11-26 | 2001-07-11 | Basf公司 | Curcumin preparation |
| CN1367167A (en) * | 2001-01-24 | 2002-09-04 | 株式会社可乐丽 | Method for preparing carotenoid emulsion |
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- 2004-02-17 CN CNB200410016439XA patent/CN100383194C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1231843A (en) * | 1998-02-23 | 1999-10-20 | 霍夫曼-拉罗奇有限公司 | Preparation of finely divided pulverous carotenoid preparation |
| CN1302559A (en) * | 1999-11-26 | 2001-07-11 | Basf公司 | Curcumin preparation |
| CN1367167A (en) * | 2001-01-24 | 2002-09-04 | 株式会社可乐丽 | Method for preparing carotenoid emulsion |
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