CN102690365B - Process for preparing polysucrose - Google Patents
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- 238000004519 manufacturing process Methods 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
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- 239000000203 mixture Substances 0.000 claims abstract description 29
- 229930006000 Sucrose Natural products 0.000 claims abstract description 27
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- 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 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 15
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- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 30
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- 238000000034 method Methods 0.000 abstract description 13
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- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
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- Epoxy Resins (AREA)
Abstract
The invention discloses a process for preparing polysucrose. The process includes following steps: placing sucrose, distilled water and epibromohydrin after mixing into a device loaded with strong-base anion exchange resin; subjecting the mixture to polymerization reaction on the strong-base anion exchange resin at the temperature of 25 DEG C to 30 DEG C, heating to 60 DEG C to 65 DEG C for re-reaction, eluting the product after the reaction with the distilled water, and absorbing low cross-linked polysucrose of the product on the resin; purifying the product with acetone, and subjecting the purified product to graded eluting with anhydrous ethanol and selecting proper low cross-linked polysucrose; mixing the proper low cross-linked polysucrose with the distilled water and the epibromohydrin, dissolving dispersant into oil phase to be added to the mixture, adjusting the pH of the system with sodium hydroxide solution, performing water bath heating reaction, heating and solidifying; and filtering the obtained product and repeatedly washing with the anhydrous ethanol and the distilled water to get transparent polysucrose granule. The process for preparing the polysucrose is simple, easy to implement and higher in reaction activity, so that productivity and purity of the polysucrose are improved.
Description
Technical field
The present invention relates to compound preparing technical field, especially a kind of processing method of preparing water-soluble polymers.
Background technology
Ficoll is a kind of typical sucrose polymer, and it is a kind of water-soluble white powder shaped polymer, and in solution, particle diameter is 10 nanometer left and right, can at room temperature preserve.According to its molecular size range, be divided into again: ficoll 800, ficoll 400, ficoll 200, ficoll 100, ficoll 70, ficoll 10.Its endogenous viscosity is respectively: 24.5,17,12,8, and 7,2.5 cp.Ficoll has the features such as good biocompatibility, reactive behavior are high, good water solubility, is mainly used at present cellular segregation field.And due to its well behaved feature, in protein adsorption field, field of tissue engineering technology, immunology research, all there is larger application potential.
The synthetic method of And Application of Sucrose-based Polymers is mainly that chemosynthesis and enzymatic are synthetic at present.The synthetic of sucrose polymer is mainly divided into two stages: first, utilize enzyme or chemical reagent to cause its hydrolysis or other chemical transformation, introduce one or more functional groups; Then, the monomer after modification obtains sucrose polymer through polyreaction.The mechanism of this step reaction is mainly radical reaction mechanism, and a few cases is Condensation polymerization mechanism.The people such as Fei Leila (Ferreira) the 41st phase of " carbohydrate polymer " first roll in 2000 from 15 pages to 24 pages (L Ferreira, M M Vidal, C F G C Geraldes, et a1., Preparation and characterisation of gels based on sucrose modified with glyeidyl methacrylate, Carbohydrate Polymers, 2000, 41 (1): 15-24) reported that the non-selectivity chemically modified of sucrose and vinyl group prepares the method for And Application of Sucrose-based Polymers hydrogel, the method is reacted sucrose with mol ratio 1:1 with glyceral methacrylate in dimethyl sulfoxide (DMSO), with 4-N, N dimethylamine pyridine is made catalyzer, generate a kind of new monomer, new monomer and methacrylic acid-2-hydroxy methacrylate react in the mixed solution with 70:30 at ethylene glycol and water, taking ammonium persulphate as initiator, synthesized gel rubber polymkeric substance.In chemosynthesis process, due to 8 activity hydroxies time, exist, make its selective modification very difficult.The feature of chemosynthesis can be summarized as: (1) chemical catalyst easily obtains, but the locational choice is poor; (2) reactions steps is many, and reaction process is tediously long; (3) need High Temperature High Pressure and vacuumize; (4) need to add polymerization starter; (5) product mostly is heterogeneous mixture, and output capacity is low; (6) chemical reagent is easily to environment.
The people such as old (Chen) and Martin (Martin) is (X Chen in the 28th phase of " carbohydrate polymer " first roll nineteen ninety-five from 15 pages to 2 pages, Martin T K, Neubauer, et a1., Enzymatic and chemoenzymatic approaches to synthesis of sugar-based polymer and hydrogels, Carbohydrate Polymers, 1995, 28 (1): 15-2l) delivered and adopted proteolytic enzyme catalysis sucrose and the hexanodioic acid derivatives reaction of basic hydrolysis to obtain a kind of linear polyester replacing, sucrose molecules is included on polyester backbone.Their work concentrates on development enzyme or chemical enzyme process is prepared glycosyl polymkeric substance.Use enzyme catalysis synthetic copolymer completely, the directly copolymerization of catalysis sugar and diester, result obtains the polymkeric substance of sugar and diprotic acid alternating copolymerization.The feature of enzyme process may be summarized to be: high efficiency, and selectivity, reaction conditions gentleness, pollution-free.More existing unfavorable aspects of enzyme process: it is fewer that (1) can be used for the number of the synthetic enzyme of sucrose polymer; (2) reaction process can only slowly be carried out under the temperature of specifying and condition; (3) stability of enzyme in organic solvent medium is not high; (4) enzymatic reaction is easily suppressed by substrate or product; (5) need to add acylating agent, selecting suitable acylating agent is important problem.These problems all can limit the application of enzyme process.
Ficoll is generally taking sucrose and epoxy chloropropane as raw material, a kind of synthesizing water-solubility superpolymer that utilizes sucrose and epichlorohydrin interpolymerization to make, and molecular weight is about 4 × 105.The Yang Jing of University Of Tianjin adopts two-step reaction to prepare ficoll micro-sphere in the academic dissertation " the synthetic and sign of polysucrose gel microballoon " of 2006, it is first synthesis of soluble type ficoll, select the solvable type ficoll of suitable molecular weight and molecular weight distribution, then prepare polysucrose gel microballoon by inverse suspension polymerization method, and be tentatively applied in the Separation Research of protein, separating effect is better.Through test, the product purity that the method obtains is 95～97%, but the method reaction process is longer, and operation is many, and productive rate is 85-87%, may not too adapt to and large-scale industrial production.
Summary of the invention
The object of this invention is to provide a kind of processing method of preparing ficoll, this method can be prepared ficoll under the condition of milder, and solves productive rate and the not high enough problem of purity that prior art is prepared ficoll.
In order to address the above problem, the technical solution used in the present invention is: this processing method of preparing ficoll, include following steps: (1) mixes sucrose, distilled water and epoxy bromopropane to pack in the device that is loaded with strongly basic anion exchange resin, at 25～30 DEG C, react 2～2.5 hours, make mixture on strongly basic anion exchange resin, carry out polymerization, the pH value of reaction is 12～13, be warming up to 60～65 DEG C, react again 2～2.5 hours, by reaction solution distilled water wash-out, gained low cross-linking ficoll is adsorbed on resin; (2) with acetone, the low cross-linking ficoll of gained is carried out to purifying, with dehydrated alcohol, purified product is carried out to elution fractionation again, choose weight-average molecular weight and be 30～500,000 low cross-linking ficoll: (3) are that 30～500,000 low cross-linking ficoll and distilled water and epoxy bromopropane are mixed to get mixture by described weight-average molecular weight, again dispersion agent is dissolved in to oil phase thing and adds described mixture, with pH value to 12～13 of aqueous sodium hydroxide solution regulation system, 70～75 DEG C of reactions of heating in water bath 1.5～2 hours, be warming up to 90～95 DEG C, solidify 9～10 hours; (4) will solidify rear products therefrom and filter, with dehydrated alcohol and distilled water wash, obtain transparent ficoll particle; (5) gained ficoll particle is carried out completing after drying treatment.
In the above-mentioned processing method technical scheme of preparing ficoll, technical scheme can also be more specifically: distilled water described in step (1) be described sucrose quality weight percent 30～40%, described epoxy bromopropane be described sucrose quality weight percent 30～50%, filter membrane is equipped with at least one end of described device; Described in step (3), the volume of oil phase thing and the volume ratio of described distilled water are 5:1～8:1, and the volume of described dispersion agent accounts for 2～3% of described oil phase volume percent.Epoxy bromopropane described in step (1) be described sucrose quality weight percent 40～50%, the thickness of described filter membrane is 2～3 centimetres; Described in step (3), the volume of oil phase thing and the volume ratio of described distilled water are 6:1～8:1.Described filter membrane is ceramic membrane or poly tetrafluoroethylene.Described dispersion agent is Si Ban or tween; Described oil phase thing is chlorobenzene or whiteruss.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect: reaction process is shorter, and operation is few, simple, and reaction conditions is more gentle; Mixed to sucrose, distilled water and epoxy bromopropane mixture is packed in the device that is loaded with strongly basic anion exchange resin for subsequent use, compared with the method for preparing ficoll of commonly using, adopt fixed bed, avoided the step of product and catalyst separating, reduced pollution; Employing epoxy bromopropane is linking agent, and compared with conventional epoxy chloropropane linking agent, reaction has higher activity, and the productive rate of ficoll and purity are all increased, and the productive rate of the ficoll making reaches 92～96%, and purity is 98～99.5%.
Brief description of the drawings
Fig. 1 is the structural representation that is loaded with the device of anionite-exchange resin.
Embodiment
Below in conjunction with accompanying drawing embodiment, the invention will be further described:
The device of what following examples were used be loaded with anionite-exchange resin as shown in Figure 1, it comprises cylindrical shell 1, anionite-exchange resin 2, filter membrane 3, anionite-exchange resin 2 is filled in cylindrical shell 1, and it is the filter membrane 3 of 2～3 centimetres that the both ends open place of cylindrical shell 1 is all coated with thickness.Wherein embodiment 1～3 filter membrane 3 is ceramic membrane; Embodiment 4～16 filter membranes 3 are poly tetrafluoroethylene.
By 80g sucrose, 24ml(is 24g) distilled water, 40g epoxy bromopropane packs into and is loaded with in the device that the ceramic membrane thickness of D201 resin is 2cm, at 25 DEG C, react 2 hours, the pH value of reaction is 12, makes mixture on strongly basic anion exchange resin, carry out polymerization, be warming up to 60 DEG C, react 2 hours again, then use distilled water elution of reactive liquid, product low cross-linking ficoll is adsorbed on resin.Product is carried out to purifying with acetone, low cross-linking ficoll is carried out to elution fractionation with dehydrated alcohol, the weight-average molecular weight of the low cross-linking ficoll of choosing is 300,000.
In the there-necked flask of the 250ml with whipping appts, add low cross-linking ficoll 5g, distilled water 20ml, epoxy bromopropane 3ml, fully stirs and makes it to mix.Add 150ml chlorobenzene to add in mixture class of 3ml department 85, adjusting pH with aqueous sodium hydroxide solution is 12.Then, there are a large amount of microballoons in 70 DEG C of water-baths reaction 1.5 hours, and 90 DEG C solidify 10 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 92.7%, the purity of product is 98.6%.
The low cross-linking ficoll 5g that adds embodiment 1 to make in the there-necked flask of the 250ml with whipping appts, distilled water 20ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 150ml chlorobenzene to add in mixture 3ml polysorbate85, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of water-baths reaction 1.5 hours, and 90 DEG C solidify 9.5 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 95.9%, the purity of product is 98.2%.
The low cross-linking ficoll 5g that adds embodiment 1 to make in the there-necked flask of the 250ml with whipping appts, distilled water 20ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 150ml whiteruss to add in mixture class of 4.2ml department 85, adjusting pH with aqueous sodium hydroxide solution is 12.Then, there are a large amount of microballoons in 75 DEG C of water-baths reaction 1.5 hours, and 95 DEG C solidify 10 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 94.6%, the purity of product is 99.2%.
Embodiment 4
The low cross-linking ficoll 5g that adds embodiment 1 to make in the there-necked flask of the 250ml with whipping appts, distilled water 20ml, epoxy bromopropane 3.5ml, fully stirs and makes it to mix.Add 150ml chlorobenzene to add in mixture class of 4ml department 85, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of water-baths reaction 2 hours, and 90 DEG C solidify 10 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, dry yields 93.5%, and the purity of product is 98.0%.
Embodiment 5
By 80g sucrose, 28ml(is 28g) distilled water, 32g epoxy bromopropane packs into and is loaded with in the device that the ceramic membrane thickness of D296 resin is 3cm, at 30 DEG C, react 2 hours, the pH value of reaction is 13, makes mixture on strongly basic anion exchange resin, carry out polymerization, be warming up to 65 DEG C, react 2 hours again, then use distilled water elution of reactive liquid, low cross-linking ficoll is adsorbed on resin.Product is carried out to purifying with acetone, low cross-linking ficoll is carried out to elution fractionation with dehydrated alcohol, the weight-average molecular weight of the low cross-linking ficoll of choosing is 400,000.
In the there-necked flask of the 250ml with whipping appts, add low cross-linking ficoll 5g, distilled water 25ml, epoxy bromopropane 3ml, fully stirs and makes it to mix.Add 125ml chlorobenzene to add in mixture class of 3ml department 80, adjusting pH with aqueous sodium hydroxide solution is 12.Then, there are a large amount of microballoons in 75 DEG C of water-baths reaction 1.5 hours, and 90 DEG C solidify 10 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 92.8%, the purity of product is 98.7%.
Embodiment 6
The low cross-linking ficoll 5g that adds embodiment 5 to make in there-necked flask with the 250ml of whipping appts, distilled water 25ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 150ml chlorobenzene to add in mixture 3ml tween, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of water-baths reaction 2 hours, and 90 DEG C solidify 9.5 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 93.7%, the purity of product is 99.5%.
Embodiment 7
The low cross-linking ficoll 5g that adds embodiment 5 to make in there-necked flask with the 250ml of whipping appts, distilled water 25ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 150ml whiteruss to add in mixture class of 4.2ml department 80, adjusting pH with aqueous sodium hydroxide solution is 12.Then, there are a large amount of microballoons in 70 DEG C of water-baths reaction 1.5 hours, and 90 DEG C solidify 10 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 95.3%, the purity of product is 98.3%.
Embodiment 8
The low cross-linking ficoll 5g that adds embodiment 5 to make in there-necked flask with the 250ml of whipping appts, distilled water 25ml, epoxy bromopropane 3.5ml, fully stirs and makes it to mix.Add 150ml chlorobenzene to add in mixture class of 4ml department 80, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of water-baths reaction 1.5 hours, and 90 DEG C solidify 9.5 hours, and product is filtered, and repeatedly washs with dehydrated alcohol and distilled water, obtains transparent sphere particle, be dried, and productive rate 95.8%, the purity of product is 98.0%.
Embodiment 9
By 80g sucrose, 28ml(is 28g) distilled water, 24g epoxy bromopropane packs into and is loaded with in the device that the tetrafluoroethylene film thickness of NDA900 resin is 2cm, at 25 DEG C, react 2.5 hours, the pH value of reaction is 12, makes mixture on strongly basic anion exchange resin, carry out polymerization, be warming up to 60 DEG C, react 2.5 hours again, then use distilled water elution of reactive liquid, low cross-linking ficoll is adsorbed on resin.Product is carried out to purifying with acetone, low cross-linking ficoll is carried out to elution fractionation with dehydrated alcohol, the weight-average molecular weight of the low cross-linking ficoll of choosing is 400,000.
In the there-necked flask of the 250ml with whipping appts, add low cross-linking ficoll 4g, distilled water 17.5ml, epoxy bromopropane 3ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture class of 3ml department 85, adjusting pH with aqueous sodium hydroxide solution is 12.Then, there are a large amount of microballoons in 70 DEG C of reactions of water-bath 1.5 hours.90 DEG C solidify 10 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 94.7%, the purity of product is 99.1%.
Embodiment 10
The low cross-linking ficoll 4g that adds embodiment 9 to make in the there-necked flask of the 250ml with whipping appts, distilled water 17.5ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture class of 3ml department 85, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of reactions of water-bath 1.5 hours.90 DEG C solidify 9.5 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 95.1%, the purity of product is 98.9%.
Embodiment 11
The low cross-linking ficoll 4g that adds embodiment 9 to make in the there-necked flask of the 250ml with whipping appts, distilled water 17.5ml, epoxy bromopropane 3ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture class of 4.2ml department 85, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 75 DEG C of reactions of water-bath 1.5 hours.95 DEG C solidify 10 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 93.5%, the purity of product is 99.5%.
Embodiment 12
The low cross-linking ficoll 4g that adds embodiment 9 to make in the there-necked flask of the 250ml with whipping appts, distilled water 17.5ml, epoxy bromopropane 3.5ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture class of 4ml department 85, adjusting pH with aqueous sodium hydroxide solution is 12.Then, there are a large amount of microballoons in 70 DEG C of reactions of water-bath 1.5 hours.95 DEG C solidify 9.5 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 95.2%, the purity of product is 98.7%.
Embodiment 13
By 80g sucrose, 32ml(is 32g) distilled water, 36g epoxy bromopropane packs into and is loaded with in the device that the tetrafluoroethylene film thickness of D202 resin is 3cm, at 25 DEG C, react 2.5 hours, the pH value of reaction is 13, makes mixture on strongly basic anion exchange resin, carry out polymerization, be warming up to 60 DEG C, react 2.5 hours again, then use distilled water elution of reactive liquid, low cross-linking ficoll is adsorbed on resin.Product is carried out to purifying with acetone, low cross-linking ficoll is carried out to elution fractionation with dehydrated alcohol, the weight-average molecular weight of the low cross-linking ficoll of choosing is 500,000.
In the there-necked flask of the 250ml with whipping appts, add the low cross-linking ficoll 4g choosing, distilled water 20ml, epoxy bromopropane 3ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture class of 3ml department 80, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 75 DEG C of reactions of water-bath 1.5 hours.90 DEG C solidify 10 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 94.5%, the purity of product is 99.4%.
Embodiment 14
The low cross-linking ficoll 4g that adds embodiment 13 to make in the there-necked flask of the 250ml with whipping appts, distilled water 20ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture 3ml tween, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of reactions of water-bath 1.5 hours.95 DEG C solidify 10 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 93.7%, the purity of product is 98.3%.
Embodiment 15
The low cross-linking ficoll 4g that adds embodiment 13 to make in the there-necked flask of the 250ml with whipping appts, distilled water 20ml, epoxy bromopropane 3ml, fully stirs and makes it to mix.Add 140ml whiteruss to add in mixture class of 4ml department 80, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of reactions of water-bath 2 hours.90 DEG C solidify 9.5 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, be dried, and productive rate 94.8%, the purity of product is 99.1%.
Embodiment 16
The low cross-linking ficoll 4g that adds embodiment 13 to make in the there-necked flask of the 250ml with whipping appts, distilled water 20ml, epoxy bromopropane 4ml, fully stirs and makes it to mix.Add 140ml chlorobenzene to add in mixture class of 4ml department 80, adjusting pH with aqueous sodium hydroxide solution is 13.Then, there are a large amount of microballoons in 70 DEG C of reactions of water-bath 1.5 hours.90 DEG C solidify 10 hours, and product is filtered, and repeatedly wash with dehydrated alcohol and distilled water, obtain transparent sphere particle, are dried.Productive rate 95.1%, the purity of product is 98.4%.
Claims (3)
1. prepare a processing method for ficoll, it is characterized in that including following steps:
(1) sucrose, distilled water and epoxy bromopropane are mixed and packed in the device that is loaded with strongly basic anion exchange resin, at 25～30 DEG C, react 2～2.5 hours, make mixture on strongly basic anion exchange resin, carry out polymerization, the pH value of reaction is 12～13, be warming up to 60～65 DEG C, react again 2～2.5 hours, by reaction solution distilled water wash-out, gained low cross-linking ficoll is adsorbed on resin;
(2) with acetone, the low cross-linking ficoll of gained is carried out to purifying, then purified product is carried out to elution fractionation with dehydrated alcohol, choose weight-average molecular weight and be 30～500,000 low cross-linking ficoll:
(3) be that 30～500,000 low cross-linking ficoll and distilled water and epoxy bromopropane are mixed to get mixture by described weight-average molecular weight, again dispersion agent is dissolved in to oil phase thing and adds described mixture, with pH value to 12～13 of aqueous sodium hydroxide solution regulation system, 70～75 DEG C of reactions of heating in water bath 1.5～2 hours, be warming up to 90～95 DEG C, solidify 9～10 hours;
(4) will solidify rear products therefrom and filter, with dehydrated alcohol and distilled water wash, obtain transparent ficoll particle;
(5) gained ficoll particle is carried out completing after drying treatment;
Wherein, distilled water described in step (1) be described sucrose quality weight percent 30～40%, described epoxy bromopropane be described sucrose quality weight percent 30～50%, filter membrane is equipped with at least one end of described device; Described in step (3), the volume of oil phase thing and the volume ratio of described distilled water are 5:1～8:1, and the volume of described dispersion agent accounts for 2～3% of described oil phase volume percent; Described dispersion agent is class of liquid department 85 or class 80 of department or tween; Described oil phase thing is chlorobenzene or whiteruss.
2. the processing method of preparing ficoll according to claim 1, is characterized in that: epoxy bromopropane described in step (1) be described sucrose quality weight percent 40～50%, the thickness of described filter membrane is 2～3 centimetres; Described in step (3), the volume of oil phase thing and the volume ratio of described distilled water are 6:1～8:1.
3. the processing method of preparing ficoll according to claim 1 and 2, is characterized in that: described filter membrane is ceramic membrane or poly tetrafluoroethylene.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0209169A1 (en) * | 1985-07-05 | 1987-01-21 | Institut National Polytechnique | Process for obtaining agar-agar from the juices extracted from seaweeds |
| CN1834109A (en) * | 2006-01-12 | 2006-09-20 | 武汉大学 | Cross-linked pachyman, its prepn. and uses |
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2012
- 2012-06-03 CN CN201210178690.0A patent/CN102690365B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0209169A1 (en) * | 1985-07-05 | 1987-01-21 | Institut National Polytechnique | Process for obtaining agar-agar from the juices extracted from seaweeds |
| CN1834109A (en) * | 2006-01-12 | 2006-09-20 | 武汉大学 | Cross-linked pachyman, its prepn. and uses |
Non-Patent Citations (3)
| Title |
|---|
| 基于强碱阴离子交换树脂固定床催化制备生物柴油;柯中炉等;《中国粮油学报》;20110531;第26卷(第5期);第71-75页 * |
| 杨晶.聚蔗糖微球的制备及应用研究.《中国优秀硕士学位论文全文数据库(电子期刊),工程科技第Ⅰ辑》.2007,(第05期),第B020-98页. * |
| 柯中炉等.基于强碱阴离子交换树脂固定床催化制备生物柴油.《中国粮油学报》.2011,第26卷(第5期),第71-75页. |
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