CN104311714A - Preparation method of resin for high-selectivity adsorption of gardenia yellow - Google Patents
Preparation method of resin for high-selectivity adsorption of gardenia yellow Download PDFInfo
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- CN104311714A CN104311714A CN201410544134.XA CN201410544134A CN104311714A CN 104311714 A CN104311714 A CN 104311714A CN 201410544134 A CN201410544134 A CN 201410544134A CN 104311714 A CN104311714 A CN 104311714A
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Abstract
The invention discloses a preparation method of resin for high-selectivity adsorption of gardenia yellow. The preparation method comprises the following steps: (1) adding a skeleton raw material, a cross-linking agent and an additive to de-ionized water for conducting a polymerization reaction namely, warming up mixed liquor to 60-80 DEG C within 35-55min and preserving heat for 0.5-2.5h; then warming up the mixed liquor to 60-80 DEG C within 15-20min and preserving heat for 3-5h; and then warming up the mixed liquor to 70-90 DEG C within 20-25min and preserving heat for 3-5h; finally, warming up the mixed liquor to 90-95 DEG C within 20-25min and preserving heat for 3-5h, and conducting solid-liquid separation; (2) cleaning solid phase with water for 2-3 times to obtain milk white spherical particles; and (3) cleaning the milk white spherical particles with vapor to obtain the resin. The prepared resin is high in stability, large in specific surface area, large in adsorption capacity, good in selectivity, rapid in adsorption speed and is capable of efficiently adsorbing gardenia yellow, and the obtained gardenia yellow is high in color value and purity; and in addition, the resin is capable of conveniently conducting regeneration treatment, long in service life and low in production cost.
Description
Technical field
The invention provides a kind of preparation method of resin of high-selectivity adsorption Gardenia Yellow, belong to technical field of polymer chemistry.
Background technology
Gardenia Yellow is from cape jasmine fruit, extract the yellow pigment obtained, it is the rare water-soluble carotenoid class pigment of a kind of nature, belong to natural pigment, it can be used alone, also can with gardenia blue pigment and gardenia red pigment by the composite pigment obtaining a series of different tone, bright in colour, nontoxic, stability is better, colouring power is strong, is widely used in the fields such as food, medicine and makeup.In recent years, because the appearance of synthetic colour food-safety problem makes to expand rapidly as this class natural pigment market of gardenin.The method of the extraction of Gardenia Yellow to be mainly contained: Flavonoids by Macroporous Adsorption Resin, ultrafiltration process, oppositely membrane permeation method, solvent precipitation, solvent reflux extraction etc., but due to the limitation of method, only have Flavonoids by Macroporous Adsorption Resin to have high input scale production.The patent No. is the Chinese patent of CN102911513 discloses a kind of Gardenia Yellow extracting method on March 12nd, 2014, macroporous resin adsorption method is have employed in the method, but adsorption effect is undesirable, and need, by after fruit peeling process, just can reach certain adsorption effect, its operation is more loaded down with trivial details, long flow path, loss of effective components increases relatively, adds the difficulty of technique, improves extraction cost.
Summary of the invention
The object of the invention is for solving above-mentioned Problems existing, a kind of preparation method of the resin for high-selectivity adsorption Gardenia Yellow is provided, stability is high, specific surface area is large, loading capacity is large, rate of adsorption is fast, desorption condition is gentle, is applicable to the adsorbing and extracting of high-performance Gardenia Yellow.
In order to achieve the above object, the present invention adopts following technical scheme: a kind of preparation method of resin of high-selectivity adsorption Gardenia Yellow, comprise the following steps: skeleton raw material and linking agent and additive add in deionized water by (1), and abundant mix and blend, carries out suspension polymerization; Described polyreaction comprises with the next stage: the first stage: mixeding liquid temperature is risen to 60-80 DEG C, insulation 0.5-2.5 hour in 35-55 minute; Subordinate phase: mixeding liquid temperature is risen to 60-80 DEG C, insulation 3-5 hour in 15-20 minute; Phase III: mixeding liquid temperature is risen to 70-90 DEG C, insulation 3-5 hour in 20-25 minute; Fourth stage: mixeding liquid temperature is risen to 90-95 DEG C, insulation 3-5 hour in 20-25 minute, solid-liquid separation obtains solid phase; Described skeleton raw material is the mixture of vinylbenzene and acrylate; Described additive comprises pore-creating agent, initiator and dispersion agent; (2) by the water of described solid phase 80-100 DEG C cleaning 2-3 time, oyster white spherical particle is obtained; (3) by temperature be the water vapour of 120-130 DEG C to described oyster white spherical particle cleaning 1-2 time, obtain resin.
By this technical scheme, special skeleton raw material and proportioning thereof, in conjunction with the resin obtaining efficiently being cross-linked with Gardenia Yellow, specific surface area is large, loading capacity is large, selectivity is good, rate of adsorption is fast; The usage quantity of the pore-creating agent that cost is high is few, reaches the performance requriements of required resin, which decreases cost, then Bound moisture steam purge removes pore-creating agent, and reduce technology difficulty, removal effect is good, and basic noresidue improves the quality of resin.
As preferably, the mass mixing ratio of described vinylbenzene and described acrylate is 1-3:1-3.
As preferably, described linking agent to be mass concentration be 60% divinylbenzene.
As preferably, the add-on of described linking agent is the 30-50% of described skeleton raw materials quality.
As preferably, the add-on of described pore-creating agent is the 0.5-1% of described skeleton raw materials quality, and described pore-creating agent is one or both in octane-iso and toluene.
As preferably, described pore-creating agent is the mixture of octane-iso and toluene, and the mass mixing ratio of described octane-iso and toluene is 1:1-5.
As preferably, the add-on of described initiator is the 1-3% of described skeleton raw materials quality, and described initiator is benzoyl peroxide.
As preferably, the add-on of described dispersion agent is the 1-3% of described skeleton raw materials quality, and described dispersion agent is polyvinyl alcohol.
By implementing technique scheme, the present invention compares with prior art, there is following beneficial effect: the resin physical and chemical stability obtained is high, specific surface area is large, loading capacity is large, selectivity is good, rate of adsorption is fast, can efficient adsorption Gardenia Yellow, obtain High color values, highly purified Gardenia Yellow, and the desorption condition of resin is gentle, manipulation of regeneration is convenient, life cycle is long, greatly reduces production cost.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
A kind of preparation method of resin of high-selectivity adsorption Gardenia Yellow, comprise the following steps: ratio of mixture is the skeleton raw material that forms of the mixture of the vinylbenzene of 1:1 and acrylate and quality by (1) is 30% of described skeleton raw materials quality, concentration is the divinylbenzene of 60%, and quality is the octane-iso by 1:1 mixing and the toluene mixture of 0.5% of described skeleton raw materials quality, quality is the benzoyl peroxide of 1% of described skeleton raw materials quality, quality is the polyvinyl alcohol of 1% of described skeleton raw materials quality, add together in deionized water, the mass volume ratio of skeleton raw material and water is 1:100, abundant mix and blend, carry out suspension polymerization, temperature and the polymerization reaction time of polymerization are: first mixeding liquid temperature risen to 60 ° of C in 35 minutes, maintain 2.5 hours, mixeding liquid temperature risen to 70 ° of C again in 20 minutes, maintain 3 hours, then mixeding liquid temperature risen to 80 ° of C in 20 minutes, maintain 4 hours, finally mixeding liquid temperature risen to 95 ° of C in 20 minutes, maintain 5 hours, solid-liquid separation, the solid phase hot water of 90 ° of C washes 3 times, obtains oyster white spherical particle resin.
Embodiment 2:
A kind of preparation method of resin of high-selectivity adsorption Gardenia Yellow, comprise the following steps: ratio of mixture is the skeleton raw material that forms of the mixture of the vinylbenzene of 1:2 and acrylate and quality by (1) is 40% of described skeleton raw materials quality, concentration is the divinylbenzene of 60%, and quality is the octane-iso by 1:3 mixing and the toluene mixture of 1% of described skeleton raw materials quality, quality is the benzoyl peroxide of 1% of described skeleton raw materials quality, quality is the polyvinyl alcohol of 3% of described skeleton raw materials quality, add together in deionized water, the mass volume ratio of skeleton raw material and water is 1:150, abundant mix and blend, carry out suspension polymerization, temperature and the polymerization reaction time of polymerization are: first mixeding liquid temperature risen to 80 ° of C in 45 minutes, maintain 0.5 hour, mixeding liquid temperature risen to 85 ° of C again in 15 minutes, maintain 3 hours, then mixeding liquid temperature risen to 90 ° of C in 20 minutes, maintain 3 hours, finally mixeding liquid temperature risen to 95 ° of C in 20 minutes, maintain 5 hours, solid-liquid separation, the solid phase hot water of 80 ° of C washes 5 times, obtain oyster white spherical particle, be that the water vapour of 125 DEG C cleans 2 times to described oyster white spherical particle by temperature, obtain resin.
Embodiment 3:
A kind of preparation method of resin of high-selectivity adsorption Gardenia Yellow, comprise the following steps: ratio of mixture is the skeleton raw material that forms of the mixture of the vinylbenzene of 3:2 and acrylate and quality by (1) is 50% of described skeleton raw materials quality, concentration is the divinylbenzene of 60%, and quality is the octane-iso by 1:5 mixing and the toluene mixture of 0.6% of described skeleton raw materials quality, quality is the benzoyl peroxide of 2% of described skeleton raw materials quality, quality is the polyvinyl alcohol of 2% of described skeleton raw materials quality, add together in deionized water, the mass volume ratio of skeleton raw material and water is 1:150, abundant mix and blend, carry out suspension polymerization, temperature and the polymerization reaction time of polymerization are: first mixeding liquid temperature risen to 70 ° of C in 55 minutes, maintain 2 hours, mixeding liquid temperature risen to 75 ° of C again in 18 minutes, maintain 4 hours, then mixeding liquid temperature risen to 80 ° of C in 22 minutes, maintain 4 hours, finally mixeding liquid temperature risen to 93 ° of C in 22 minutes, maintain 4 hours, solid-liquid separation, the solid phase hot water of 100 ° of C washes 2 times, obtain oyster white spherical particle, be that the water vapour of 130 DEG C cleans 2 times to described oyster white spherical particle by temperature, obtain resin.
Claims (8)
1. a preparation method for the resin of high-selectivity adsorption Gardenia Yellow, is characterized in that: comprise the following steps: skeleton raw material and linking agent and additive add in deionized water by (1), and abundant mix and blend, carries out suspension polymerization; Described polyreaction comprises with the next stage: the first stage: mixeding liquid temperature is risen to 60-80 DEG C, insulation 0.5-2.5 hour in 35-55 minute; Subordinate phase: mixeding liquid temperature is risen to 70-85 DEG C, insulation 3-5 hour in 15-20 minute; Phase III: mixeding liquid temperature is risen to 70-90 DEG C, insulation 3-5 hour in 20-25 minute; Fourth stage: mixeding liquid temperature is risen to 90-95 DEG C, insulation 3-5 hour in 20-25 minute, solid-liquid separation obtains solid phase; Described skeleton raw material is the mixture of vinylbenzene and acrylate; Described additive comprises pore-creating agent, initiator and dispersion agent; (2) by the water of described solid phase 80-100 DEG C cleaning 2-5 time, oyster white spherical particle is obtained; (3) by temperature be the water vapour of 120-130 DEG C to described oyster white spherical particle cleaning 1-2 time, obtain resin.
2. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 1, is characterized in that: the mass mixing ratio of described vinylbenzene and described acrylate is 1-3:1-3.
3. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 1, is characterized in that: described linking agent to be mass concentration be 60% divinylbenzene.
4. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 3, is characterized in that: the add-on of described linking agent is the 30-50% of described skeleton raw materials quality.
5. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 1, is characterized in that: the add-on of described pore-creating agent is the 0.5-1% of described skeleton raw materials quality, and described pore-creating agent is one or both in octane-iso and toluene.
6. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 5, it is characterized in that: described pore-creating agent is the mixture of octane-iso and toluene, the mass mixing ratio of described octane-iso and toluene is 1:1-5.
7. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 1, it is characterized in that: the add-on of described initiator is the 1-3% of described skeleton raw materials quality, described initiator is benzoyl peroxide.
8. the preparation method of a kind of resin of high-selectivity adsorption Gardenia Yellow according to claim 1, it is characterized in that: the add-on of described dispersion agent is the 1-3% of described skeleton raw materials quality, described dispersion agent is polyvinyl alcohol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029028A (en) * | 2020-09-01 | 2020-12-04 | 陕西蓝深特种树脂有限公司 | Macroporous adsorption resin for extracting vitamin B12 and preparation method thereof |
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- 2014-10-15 CN CN201410544134.XA patent/CN104311714A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029028A (en) * | 2020-09-01 | 2020-12-04 | 陕西蓝深特种树脂有限公司 | Macroporous adsorption resin for extracting vitamin B12 and preparation method thereof |
| CN112029028B (en) * | 2020-09-01 | 2023-10-17 | 陕西蓝深特种树脂有限公司 | Macroporous adsorption resin for extracting vitamin B12 and preparation method thereof |
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Application publication date: 20150128 |