CN106732451B - A kind of saccharification liquid decolorizer - Google Patents
A kind of saccharification liquid decolorizer Download PDFInfo
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- CN106732451B CN106732451B CN201611105604.8A CN201611105604A CN106732451B CN 106732451 B CN106732451 B CN 106732451B CN 201611105604 A CN201611105604 A CN 201611105604A CN 106732451 B CN106732451 B CN 106732451B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/12—Purification of sugar juices using adsorption agents, e.g. active carbon
Abstract
The present invention provides a kind of novel saccharification liquid decolorizer, preparation step are as follows: 1) pre-processes；2) preparation of magnetic attapulgite；3) preparation of magnetic attapulgite grafting hydrophilic copolymers；4) preparation of saccharification liquid decolorizer.Have the beneficial effect that the saccharification liquid decolorizer of preparation is magnetic, good hydrophilic property, strong adsorption is low in cost, can be recycled and recycles；Iron ion is set to be supported on nano-attapulgite surface using ethylene glycol and ammonium acetate dipping, calcining can be such that the bond strength of magnetic-particle and attapulgite enhances, and extend the magnetic action time, and product magnetic property improves；Magnetic nano-particle size uniformity, is evenly distributed；Grafting rate is high, and hydroxyl functional group is more after grafting, and hydrophilicity is good, and it is simple sufficiently react preparation step with saccharified liquid, suitable the factorial production.
Description
Technical field
The present invention relates to decolorising agent preparation technical field, specifically a kind of saccharification liquid decolorizer.
Background technique
Saccharified liquid is in food and medicine trade using very extensive, and saccharified liquid color is one of product critically important
Organoleptic indicator, therefore selecting a kind of not only economic but also highly effective decoloration reagent is the problem of producer extremely pays close attention to.Saccharified liquid
Production will liquefy by high-temperature injection, then some pigments can be generated in this production process, a kind of pigment be sugar with before coloring matter
The product of precursor reactant, another kind of pigment are that sugared degradation generates.Some coloring matters generate under alkaline condition, have two
Close property not only has hydrophily, but also has hydrophobicity.If colour removal not will seriously affect the organoleptic indicator of finished product, factory is restricted
Family's economic interests.The saccharification liquid decolorizer being widely used now is wood activated charcoal, good decolorizing effect but is involved great expense.
Attapulgite is also known as palygorskite or slope thread compiles stone, is a kind of aqueous rich magnesium silicate clay mine for having chain layer structure
Object has unique appearance structure, dispersibility, high temperature resistant, saline-alkali tolerance, high surface charge and big specific surface area.Due to it
Special appearance structure and performance is led in environment adsorbent, catalyst carrier, insecticide and fertilizer carrier and pattern controlling agent etc.
It is widely answered in domain.Attapulgite in nature is bad to the adsorption effect of saccharified liquid pigment, needs to carry out it grafting and changes
Property, improve adsorption efficiency.
Have the research structurally-modified to attapulgite now, if Authorization Notice No. is CN103599756B, discloses one
The magnetic attapulgite's surface trace hydrophilic nanometer composite material of kind, belongs to technical field of environment function material preparation.Pass through dipping
Method and high temperature reduction method synthesizing magnetic attapulgite clay nano composite material, magnetic nano-particle size uniformity are evenly distributed；Pass through
Surface silanization reaction, by vinyl graft copolymer in magnetic halloysite surface, passes through reverse phase atom transferred free radical precipitation polymerization, magnetic
Property attapulgite's surface cladding molecular engram polymer layer preferably control in tens nanometer；Due to outer surface ATRP active group
In the presence of being successfully grafted hydrophilic polymer brush, and it is successfully applied in water environment the selective removal of sulfamethazine and fast
Fast Magneto separate, and there is excellent regenerability.Authorization Notice No. is CN104226263B, and it is recessed to disclose a kind of amino modified
The preparation of convex stick earth adsorbing and the method for removing Cr VI in water removal, amino agents and silane coupling agent are reacted to obtain molten
Liquid A；Graft reaction is carried out to pretreated attapulgite's surface using solution A to obtain.Amino modified attapulgite can be used as
Adsorbent removes Cr VI in water removal, and the amino modified attapulgite absorption of 0.0005 times of its quality is added in the water body to be purified
Agent, the Cr VI in absorption water under conditions of 25 DEG C, pH are 3.0~9.9, absorption 10min~collect amino modified bumps afterwards for 24 hours
Stick earth adsorbing, the Cr VI in purifying water body.This method is modified attapulgite with amido reagent, and synthesis has high ammonia
The attapulgite clay adsorbent of base content；Modified attapulgite chemical property is stable, is not influenced by outside environmental elements, and this
Inventive method is easy to operate, low in cost, and absorption property is good.
Summary of the invention
The purpose of the present invention is to provide one kind to have magnetism, and good hydrophilic property, strong adsorption is low in cost, can be recycled again
The saccharification liquid decolorizer utilized.
The present invention in background technique aiming at the problem that mentioning, the technical solution taken are as follows:
1) it pre-processes: attapulgite being added to mixing 12~25min of ultrasonic disperse in distilled water, filtering removal bottom is big
Particulate matter, centrifugation, drying, grinding, roasting；Baked attapulgite is placed in the hydrochloric acid solution that concentration is 1~6mol/L
Middle ultrasonic disperse filters after reacting 7~8.5h under the conditions of 85~95 DEG C, washing to neutrality, and drying is spare.After pretreated
The gap of attapulgite increase, the Hyarogen-bonding and Van der Waals force between ingredient weaken, between active function key and solvent
Contact rate increase；
2) preparation of magnetic attapulgite: according to ethyl alcohol: attapulgite (ATPs): the mass ratio of Fe(NO3)39H2O is
15:(0.3~1.8): ethyl alcohol, attapulgite and nine hydration nitre are successively added in the ratio of (0.5~1.2) (g/g/g) into flask
Sour iron, ultrasonic disperse is uniform, at room temperature 12~18h of magnetic agitation, is placed in 60~80 DEG C of baking ovens and dries.After grinding, it is packed into magnetic
Boat is added dropwise 10~15 parts of ethylene glycol (EG) and 0.1~0.5 part of ammonium acetate, is sufficiently impregnated 10~15h, in tube furnace with 3.0~
5.0 DEG C/min is warming up to 300~500 DEG C, maintains 1.0~3.0h of the temperature calcination, after calcined product ethanol washing is multiple, does
It is dry to constant weight, obtain magnetic attapulgite (MATPs).Attapulgite has magnetism, after saccharified liquid decoloration, can directly use and inhale
Iron-stone carries out recycling and reusing, easy to operate, environmentally protective.Iron ion is set to be supported on nanometer using ethylene glycol and ammonium acetate dipping
Attapulgite's surface, calcining can be such that the bond strength of magnetic-particle and attapulgite enhances, and extend the magnetic action time, product magnetic
Performance improves.Magnetic nano-particle size uniformity, is evenly distributed.
3) preparation of magnetic attapulgite grafting hydrophilic copolymers: according to 1,6-HD: 1,4- butanediol: silane is even
Join agent: ionic liquid I- butyl -3- methylimidazole borate is 1:(0.5~1.2): (0.0001~0.0003): (150~
250) it, is added sequentially in three-necked flask, reaction temperature is 100~120 DEG C, and the reaction time is 10~15h.Under nitrogen protection
Reaction is filtered, concentration, is added magnetic attapulgite according to solid-liquid volume ratio 1:20~1:40,15~20min of ultrasonic disperse, instead
It should terminate to be washed with the methanol extracting dissolved with 0.02~0.05% phenylpropen ketone, be dried in vacuo, grind under the conditions of 50~70 DEG C
At nanoscale, magnetic attapulgite grafting hydrophilic copolymers are obtained.The magnetic attapulgite grafting of above method preparation is hydrophilic
Property copolymer grafted rate it is high, hydroxyl functional group is more after grafting, and hydrophilicity is good, can sufficiently react with saccharified liquid.
4) preparation of saccharification liquid decolorizer: 50~70 parts of magnetic attapulgites grafting hydrophilic copolymers, 2~4 parts are gathered
Acrylamide and 100~200 parts of distilled water are added in three-necked flask, are slowly added into 5~10 parts of polyurethane, reaction temperature 150
~200 DEG C, the reaction time is 1.5~2h, and temperature drops to room temperature, and 3~7 parts of sodium alginates and 0.00001~0.00003 part is added
Potassium bichromate, concentrate drying obtain saccharification liquid decolorizer.The saccharification liquid decolorizer of above method preparation is magnetic, good hydrophilic property,
Strong adsorption, it is low in cost, it can be recycled and recycle, preparation step is simple, is suitble to the factorial production.
Compared with the prior art, the advantages of the present invention are as follows: the saccharification liquid decolorizer of preparation is magnetic, good hydrophilic property, inhales
Attached property is strong, low in cost, can be recycled and recycles；Iron ion is set to be supported on nano-attapulgite using ethylene glycol and ammonium acetate dipping
Surface, calcining can be such that the bond strength of magnetic-particle and attapulgite enhances, and extend the magnetic action time, and product magnetic property mentions
It is high；Magnetic nano-particle size uniformity, is evenly distributed；Grafting rate is high, and hydroxyl functional group is more after grafting, and hydrophilicity is good, can be with
Saccharified liquid sufficiently reacts；Preparation step is simple, is suitble to the factorial production.
Specific embodiment
Below by embodiment, technical scheme of the present invention is further explained:
Embodiment 1:
A kind of saccharification liquid decolorizer, specific preparation step are as follows:
1) it pre-processes: attapulgite being added to mixing 12~25min of ultrasonic disperse in distilled water, filtering removal bottom is big
Particulate matter, centrifugation, drying, grinding, roasting；Baked attapulgite is placed in the hydrochloric acid solution that concentration is 1~6mol/L
Middle ultrasonic disperse filters after reacting 7~8.5h under the conditions of 85~95 DEG C, washing to neutrality, and drying is spare.After pretreated
The gap of attapulgite increase, the Hyarogen-bonding and Van der Waals force between ingredient weaken, between active function key and solvent
Contact rate increase；
2) preparation of magnetic attapulgite: according to ethyl alcohol: attapulgite (ATPs): the mass ratio of Fe(NO3)39H2O is
15:(0.3~1.8): ethyl alcohol, attapulgite and nine hydration nitre are successively added in the ratio of (0.5~1.2) (g/g/g) into flask
Sour iron, ultrasonic disperse is uniform, at room temperature 12~18h of magnetic agitation, is placed in 60~80 DEG C of baking ovens and dries.After grinding, it is packed into magnetic
Boat is added dropwise 10~15 parts of ethylene glycol (EG) and 0.1~0.5 part of ammonium acetate, is sufficiently impregnated 10~15h, in tube furnace with 3.0~
5.0 DEG C/min is warming up to 300~500 DEG C, maintains 1.0~3.0h of the temperature calcination, after calcined product ethanol washing is multiple, does
It is dry to constant weight, obtain magnetic attapulgite (MATPs).Attapulgite has magnetism, after saccharified liquid decoloration, can directly use and inhale
Iron-stone carries out recycling and reusing, easy to operate, environmentally protective.Iron ion is set to be supported on nanometer using ethylene glycol and ammonium acetate dipping
Attapulgite's surface, calcining can be such that the bond strength of magnetic-particle and attapulgite enhances, and extend the magnetic action time, product magnetic
Performance improves.Magnetic nano-particle size uniformity, is evenly distributed.
3) preparation of magnetic attapulgite grafting hydrophilic copolymers: according to 1,6-HD: 1,4- butanediol: silane is even
Join agent: ionic liquid I- butyl -3- methylimidazole borate is 1:(0.5~1.2): (0.0001~0.0003): (150~
250) it, is added sequentially in three-necked flask, reaction temperature is 100~120 DEG C, and the reaction time is 10~15h.Under nitrogen protection
Reaction is filtered, concentration, is added magnetic attapulgite according to solid-liquid volume ratio 1:20~1:40,15~20min of ultrasonic disperse, instead
It should terminate to be washed with the methanol extracting dissolved with 0.02~0.05% phenylpropen ketone, be dried in vacuo, grind under the conditions of 50~70 DEG C
At nanoscale, magnetic attapulgite grafting hydrophilic copolymers are obtained.The magnetic attapulgite grafting of above method preparation is hydrophilic
Property copolymer grafted rate it is high, hydroxyl functional group is more after grafting, and hydrophilicity is good, can sufficiently react with saccharified liquid.
4) preparation of saccharification liquid decolorizer: 50~70 parts of magnetic attapulgites grafting hydrophilic copolymers, 2~4 parts are gathered
Acrylamide and 100~200 parts of distilled water are added in three-necked flask, are slowly added into 5~10 parts of polyurethane, reaction temperature 150
~200 DEG C, the reaction time is 1.5~2h, and temperature drops to room temperature, and 3~7 parts of sodium alginates and 0.00001~0.00003 part is added
Potassium bichromate, concentrate drying obtain saccharification liquid decolorizer.Polyurethane can improve system after mixing with potassium bichromate to a certain extent
Characterization of adsorption, the above method preparation saccharification liquid decolorizer be magnetic, good hydrophilic property, strong adsorption is low in cost, can be recycled
It recycles, preparation step is simple, is suitble to the factorial production.
Embodiment 2:
A kind of saccharification liquid decolorizer, most preferably preparation step are as follows:
1) it pre-processes: attapulgite is added to mixing ultrasonic disperse 20min in distilled water, filtering removal bottom bulky grain
Substance, centrifugation, drying, grinding, roasting；Baked attapulgite is placed in ultrasound point in the hydrochloric acid solution that concentration is 3mol/L
It dissipates, is filtered after reacting 7.5h under the conditions of 90 DEG C, washing to neutrality is dried, spare.The gap of attapulgite after pretreated
Increase, the Hyarogen-bonding and Van der Waals force between ingredient weaken, and the contact rate between active function key and solvent increases；
2) preparation of magnetic attapulgite: according to ethyl alcohol: attapulgite (ATPs): the mass ratio of Fe(NO3)39H2O is
It is equal that ethyl alcohol, attapulgite and Fe(NO3)39H2O, ultrasonic disperse is successively added in the ratio of 15:1:0.6 (g/g/g) into flask
Even, magnetic agitation 15h, is placed in 70 DEG C of baking ovens and dries at room temperature.After grinding, be packed into magnetic boat, be added dropwise 14 parts of ethylene glycol (EG) and
0.3 part of ammonium acetate, is sufficiently impregnated 13h, is warming up to 400 DEG C in tube furnace with 4.0 DEG C/min, maintains temperature calcination 2.3h,
It is dry to constant weight after calcined product ethanol washing is multiple, obtain magnetic attapulgite (MATPs).Attapulgite has magnetism,
After saccharified liquid decoloration, recycling and reusing directly can be carried out with magnet, it is easy to operate, it is environmentally protective.Using ethylene glycol and
Ammonium acetate dipping makes iron ion be supported on nano-attapulgite surface, and calcining can make the bond strength of magnetic-particle and attapulgite
Enhancing extends the magnetic action time, and product magnetic property improves.Magnetic nano-particle size uniformity, is evenly distributed.
3) preparation of magnetic attapulgite grafting hydrophilic copolymers: according to 1,6-HD: 1,4- butanediol: silane is even
Join agent: ionic liquid I- butyl -3- methylimidazole borate is 1:0.8:0.0002:200, is added sequentially in three-necked flask,
Reaction temperature is 110 DEG C, reaction time 12h.It reacts, filters under nitrogen protection, concentration adds according to solid-liquid volume ratio 1:30
Entering magnetic attapulgite, ultrasonic disperse 18min, reaction terminates to extract washing with the methanol dissolved with 0.03% phenylpropen ketone, and 60
It is dried in vacuo under the conditions of DEG C, is ground into nanoscale, obtain magnetic attapulgite grafting hydrophilic copolymers.Above method preparation
Magnetic attapulgite grafting hydrophilic copolymers grafting rate is high, and hydroxyl functional group is more after grafting, and hydrophilicity is good, energy and saccharified liquid
Sufficiently reaction.
4) 60 parts of magnetic attapulgites the preparation of saccharification liquid decolorizer: are grafted hydrophilic copolymers, 3 parts of polyacrylamides
It being added in three-necked flask with 150 parts of distilled water, is slowly added into 7 parts of polyurethane, reaction temperature is 180 DEG C, reaction time 1.9h,
Temperature drops to room temperature, and 5 parts of sodium alginates and 0.00001 part of potassium bichromate are added, and concentrate drying obtains saccharification liquid decolorizer.It is above-mentioned
The saccharification liquid decolorizer of method preparation is magnetic, and good hydrophilic property, strong adsorption is low in cost, can be recycled and recycles, preparation step
Simply, it is suitble to the factorial production.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of saccharification liquid decolorizer, it is characterised in that be made of following composition and its parts by weight: 50~70 parts of magnetic concave convex rods
Soil grafting hydrophilic copolymers, 5~10 parts of polyurethane, 3~7 parts of sodium alginates, 0.00001~0.00003 part of potassium bichromate and 2
~4 parts of polyacrylamides；
The magnetic attapulgite is grafted hydrophilic copolymers preparation step are as follows:
Pretreatment: attapulgite being added in distilled water and mixes ultrasonic disperse, is filtered, and is centrifuged, and is dried, and is ground, and roasting will roast
The attapulgite burnt is placed in ultrasonic disperse in hydrochloric acid solution, filtering, washing to neutrality, and drying is spare；
The preparation of magnetic attapulgite: ethyl alcohol, attapulgite and Fe(NO3)39H2O being added into flask, and ultrasonic disperse is uniform,
Magnetic agitation at room temperature is placed in baking oven after reaction and dries, and grinding is packed into magnetic boat, ethylene glycol and ammonium acetate is added dropwise, sufficiently
Dipping, is calcined in tube furnace, dry to constant weight after calcined product ethanol washing is multiple, obtains magnetic attapulgite；
The preparation of magnetic attapulgite grafting hydrophilic copolymers: by 1,6- hexylene glycol, 1,4-butanediol and silane coupling agent add
Enter into ionic liquid I- butyl -3- methylimidazole borate, react under nitrogen protection, filter, concentration is added magnetic concave-convex
Stick soil, ultrasonic disperse, reaction end are extracted with methanol and are washed, and are dried in vacuo, grinding, obtain magnetic attapulgite grafting hydrophily
Copolymer.
2. a kind of saccharification liquid decolorizer according to claim 1, it is characterised in that: concentration of hydrochloric acid is in the pretreatment
1~5mol/L, reaction temperature are 80~90 DEG C, and the reaction time is 8~9h.
3. a kind of saccharification liquid decolorizer according to claim 1, it is characterised in that: the preparation of the magnetic attapulgite
Middle dip time is 10~15h, is warming up to 300~500 DEG C in tube furnace with 3.0~5.0 DEG C/min, maintains the temperature calcination
1.0~3.0h.
4. a kind of saccharification liquid decolorizer according to claim 1, it is characterised in that: the magnetic attapulgite is grafted parent
Washing methanol is dissolved with 0.02~0.05% phenylpropen ketone in the preparation of aqueous copolymer.
5. a kind of saccharification liquid decolorizer according to claim 1, it is characterised in that: the magnetic attapulgite is grafted parent
Reaction temperature is 100~120 DEG C before magnetic attapulgite is added in the preparation of aqueous copolymer, and the reaction time is 10~15h.
6. a kind of saccharification liquid decolorizer according to claim 1, it is characterised in that: the magnetic attapulgite is grafted parent
15~20min of ultrasonic disperse, vacuum drying temperature are 50~70 after the magnetic attapulgite of addition in the preparation of aqueous copolymer
℃。
7. a kind of saccharification liquid decolorizer according to claim 1, it is characterised in that: the decolorising agent preparation step are as follows:
50~70 parts of magnetic attapulgite grafting hydrophilic copolymers, 2~4 parts of polyacrylamides and 100~200 parts of distilled water are added to
In three-necked flask, be slowly added into 5~10 parts of polyurethane, heat, temperature drops to room temperature, be added 3~7 parts of sodium alginates and
0.00001~0.00003 part of potassium bichromate, concentrate drying obtain saccharification liquid decolorizer.
8. a kind of saccharification liquid decolorizer according to claim 7, it is characterised in that: the heating temperature is 150~200
DEG C, heating time is 1.5~2h.
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| CN102994653A (en) * | 2012-12-10 | 2013-03-27 | 浙江海洋学院普陀科学技术学院 | Saccharification liquid decoloring method |
| CN103012611A (en) * | 2012-12-10 | 2013-04-03 | 浙江海洋学院普陀科学技术学院 | Resin cation saccharification liquid decolorization method |
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