CN106674446A - Special decolorization resin for starch saccharification liquid - Google Patents
Special decolorization resin for starch saccharification liquid Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
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Abstract
The invention discloses a special decolorization resin for starch saccharification liquid and relates to the technical field of processing of resin. The resin is prepared from the following raw materials in parts by weight: 70-80 parts of styrene, 40-50 parts of hydroxyethyl methylacrylate, 20-30 parts of divinyl benzene, 15-20 parts of pore-foaming agents, 6-11 parts of chlorinated polyethylene, 4-8 parts of linear low-density polyethylene, 4-8 parts of water-soluble chitosan, 3-6 parts of N,N-dimethylamino ethyl ester, 3-6 parts of sesbania gum, 3-6 parts of anionic polyacrylamide, 2-4 parts of N-phenylmaleimide, 2-4 parts of sodium tripolyphosphate, 1-2 parts of sodium polystyrenesulfonate, 1-2 parts of agar powder, 0.5-1 part of methyl hydroxybenzoate, 0.5-1 part of vitamin C magnesium phosphate, 20-30 parts of ethyl alcohol and 250-300 parts of water. The prepared resin is capable of effectively removing colored impurities in the starch saccharification liquid; the decolorization rate reaches over 98%; moreover, the decolorization time is short; the processing cycle of starch saccharification can be shortened.
Description
Technical field：
The present invention relates to resin processing technique field, and in particular to a kind of starch saccharificating liquid special decolouring resin.
Background technology：
Typically can all there is the phenomenon of color burn when saccharification react is carried out in starch sugar, and need to add when refined and live
Property charcoal is sloughing color.The reason for causing color burn is mainly, in reducing sugar carbonyl relevant with the carbonyl ammonia reaction occurred during saccharifying
Base reacts with the free amino acid of amino acid residue in free amino acid or protein molecule, and this reaction is referred to as " Mei La
Moral is reacted ".And required decolorizing effect can not once be reached using activated carbon decolorizing, needs carry out activity twice or more than twice
Carbon decoloring, which adds decolouring cycle and cost input.For this case, our company develops a kind of starch saccharificating liquid
Special decolouring resin, only using the foreign pigment that once effectively can be sloughed in starch saccharificating liquid, and the decolorizing resin regenerates
Good, the long service life of property.
The content of the invention：
The technical problem to be solved is to provide that a kind of good decolorizing effect, used time be short and the shallow lake of long service life
Powder saccharified liquid special decolouring resin.
The technical problem to be solved is realized using following technical scheme：
A kind of starch saccharificating liquid special decolouring resin, is made up of the raw material of following parts by weight：
Styrene 70-80 parts, hydroxyethyl methylacrylate 40-50 parts, divinylbenzene 20-30 part, porogen 15-20
Part, chlorinated polyethylene 6-11 parts, linear low density polyethylene 4-8 part, water-soluble chitosan 4-8 parts, N, N- dimethylaminoethyls
3-6 parts, sesbania gum 3-6 parts, PAMA 3-6 parts, N-phenylmaleimide 2-4 parts, sodium tripolyphosphate 2-4
Part, Sodium Polystyrene Sulfonate 1-2 part, agar powder 1-2 parts, methyl hydroxybenzoate 0.5-1 parts, Magnesium L-Asacorbic Acid 2-O-Phosphate 0.5-1 parts, second
Alcohol 20-30 parts, water 250-300 parts.
Using front through modification, its processing method is the sesbania gum：By the addition of 10-15 parts sesbania gum, 3-5 times weighs
In amount part water, and reflux state insulation mixing 5-10min is heated to, adds 2-3 parts polyvinyl butyral resin and 0.5-1 part 2-
Picoline, continues, in reflux state insulation mixing 15-30min, then to proceed to rapidly sealing and standing in 0-5 DEG C of environment, 3-5h
1-2 parts microwax and 0.5-1 part Oleum Terebinthinaes are added in backward gained mixture, reflux state insulation mixing 10- is again heated to
15min, is subsequently sent in freezer dryer, Jing after being fully dried by gained solid abrasive into powder, is eventually adding 0.5-1 parts oil
Sour amide and 0.3-0.5 part ferrocene, are sufficiently mixed microwave treatment 3-5min under microwave frequency 2450MHz, power 700W,
Obtain final product modified sesbania gum.
Sesbania gum can not only significantly increase its thickening property and stability, and be effectively improved which by above-mentioned modification
With the blending of oil phase substance, so as to promote the carrying out of suspension polymerization, feed stock conversion is improved.
Using front through pretreatment, its processing method is the microwax：10-15 part microwaxes are heated to melting completely
Afterwards insulation mixing 5-10min, add 1-2 part hydrophilic fumed silicas, 0.5-1 parts dimethyl diallyl ammonium chloride and
0.5-1 part epoxy soybean oils, are sufficiently mixed microwave treatment 3-5min under microwave frequency 2450MHz, power 700W, stand
Continue microwave treatment 2-3min after 30-60min, then gained fused mass be added drop-wise in 5-10 DEG C of cold water, form spherical particle,
Filter, gained spherical particle is sent in freezer dryer and is fully dried.
Microwax can not only effectively reduce its fusing point, and can improve its hydrophilic through above-mentioned pretreatment.
The preparation method of the starch saccharificating liquid special decolouring resin comprises the steps：
(1) preparation of water phase：It is first that chlorinated polyethylene, sesbania gum and agar powder are added in water, and it is heated to 60-65 DEG C of guarantor
Temperature mixing 10-15min, is subsequently adding water-soluble chitosan and PAMA, continues backflow insulation mixing 10-
15min, gained mixture are cooled to -5-0 DEG C in 3-5min under ice salt bath, and insulation stands 1-2h at -5-0 DEG C, most
Twice homogenization is carried out under 65-70 DEG C of homogenizing temperature, homogenization pressure 20-25MPa afterwards, aqueous phase solution is obtained final product；
(2) preparation of oil phase：Divinylbenzene and porogen are heated to into 75-80 DEG C of insulation mixing 10-15min first, then
Styrene and hydroxyethyl methylacrylate are added, microwave treatment 3- under microwave frequency 2450MHz, power 700W is sufficiently mixed
5min, continues microwave treatment 3-5min after standing 30-60min, obtains final product oil mixture；
(3) suspension polymerization：Linear low density polyethylene and Magnesium L-Asacorbic Acid 2-O-Phosphate are added in aqueous phase solution, plus
Heat adds oil mixture to reflux state isothermal holding 10-15min, continues isothermal holding 3-5h at reflux, so
Add N, N- dimethylaminoethyls and Sodium Polystyrene Sulfonate, insulation mixing 15-20min, by gained mixture in ice afterwards while hot
Cooled with the speed of 10-15 DEG C/min under salt bath, the insulation after temperature is down to 0-5 DEG C stands 1-2h, filters, gained filter cake
Washed 3 times with 60-65 DEG C of 2-3wt% sodium chloride solutions, and 3-5h is dried at 100-105 DEG C, finally with 0.5mm apertures
Screen filtration, obtains final product transparent spherical resin；
(4) functionalization：N-phenylmaleimide, sodium tripolyphosphate and methyl hydroxybenzoate are added in ethanol, heating
To reflux state insulation mixing 10-15min, transparent spherical resin surface is then uniformly sprayed on, 15-30min is stood, then at microwave
Microwave treatment 3-5min under frequency 2450MHz, power 700W, process stand 2-3h in proceeding to rapidly 0-5 DEG C of environment after terminating, then
Secondary microwave treatment 3-5min, is dried 2-3h at gained spherical particle is placed in 100-105 DEG C finally, obtains final product target resin.
The mixed solution of the porogen one kind or toluene and dimethylbenzene in toluene, dimethylbenzene.
The invention has the beneficial effects as follows：The made resin of the present invention is exclusively used in the decolouring of starch saccharificating liquid, by starch saccharificating liquid
The resin is flowed through once, you can effectively remove the foreign pigment in solution, percent of decolourization reaches more than 98%；Decolourize simultaneously to use
When it is short, be conducive to shortening the amylolytic process-cycle；And the resin regeneration after use is good, the decoloring ability after regeneration compared with
By force, extend the service life of resin, so as to increase economic efficiency.
Specific embodiment：
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
(1) preparation of water phase：First 6 parts of chlorinated polyethylenees, 5 parts of sesbania gums and 1 part of agar powder are added in 250 parts of water, and
60-65 DEG C of insulation mixing 15min is heated to, 4 parts of water-soluble chitosans and 3 parts of PAMAs is subsequently adding, is continued
Backflow insulation mixing 15min, gained mixture is cooled to -5-0 DEG C in 5min under ice salt bath, and is incubated at -5-0 DEG C quiet
2h is put, and finally twice homogenization is carried out under 65-70 DEG C of homogenizing temperature, homogenization pressure 20-25MPa, is obtained final product aqueous phase solution；
(2) preparation of oil phase：20 parts of divinylbenzene and 15 parts of porogen are heated to into 75-80 DEG C of insulation mixing first
15min, adds 70 parts of styrene and 45 parts of hydroxyethyl methylacrylates, is sufficiently mixed after microwave frequency 2450MHz, power
Microwave treatment 5min under 700W, continues microwave treatment 5min after standing 45min, obtains final product oil mixture；
(3) suspension polymerization：4 parts of linear low density polyethylene and 0.5 part of vitamin C phosphoric acid are added in aqueous phase solution
Ester magnesium, is heated to reflux state isothermal holding 15min, adds oil mixture, continues isothermal holding 5h at reflux,
Then 3 parts of N, N- dimethylaminoethyls and 2 parts of Sodium Polystyrene Sulfonate, insulation mixing 15min, by gained mixture are added while hot
Cooled with the speed of 10-15 DEG C/min under ice salt bath, the insulation after temperature is down to 0-5 DEG C stands 2h, filters, gained filter
Cake is washed 3 times with 60-65 DEG C of 2-3wt% sodium chloride solutions, and 5h is dried at 100-105 DEG C, finally with 0.5mm apertures
Screen filtration, obtains final product transparent spherical resin；
(4) functionalization：3 parts of N-phenylmaleimides, 2 parts of sodium tripolyphosphates and 0.5 part of methyl hydroxybenzoate are added
In 25 parts of ethanol, reflux state insulation mixing 15min is heated to, transparent spherical resin surface is then uniformly sprayed on, is stood
30min, then at microwave treatment 5min under microwave frequency 2450MHz, power 700W, process proceeds to rapidly 0-5 DEG C of environment after terminating
Middle standing 3h, microwave treatment 5min, is dried 3h at gained spherical particle is placed in 100-105 DEG C finally, obtains final product goal tree again
Fat.
The modification of sesbania gum：15 parts of sesbania gums are added in 5 times of weight portion water, and it is mixed to be heated to reflux state insulation
10min is closed, 2 parts of polyvinyl butyral resins and 0.5 part of 2- picoline is added, is continued in reflux state insulation mixing 30min,
Then sealing and standing in 0-5 DEG C of environment is proceeded to rapidly, 2 parts of microwaxes and 0.5 part of Oleum Terebinthinae after 3h, is added in gained mixture,
Reflux state insulation mixing 15min is again heated to, is subsequently sent in freezer dryer, gained solid is ground Jing after being fully dried
Clay into power, be eventually adding 0.5 part of oleamide and 0.3 part of ferrocene, be sufficiently mixed after microwave frequency 2450MHz, power
Microwave treatment 5min under 700W, obtains final product modified sesbania gum.
The pretreatment of microwax：By 15 parts of microwaxes be heated to completely melting after insulation mixing 5min, add 2 parts it is hydrophilic
Property aerosil, 0.5 part of dimethyl diallyl ammonium chloride and 0.5 part of epoxy soybean oil, are sufficiently mixed after Microwave Frequency
Microwave treatment 5min under rate 2450MHz, power 700W, continues microwave treatment 3min after standing 30min, then by gained fused mass
It is added drop-wise in 5-10 DEG C of cold water, forms spherical particle, filter, gained spherical particle is sent in freezer dryer and is fully dried.
Embodiment 2
(1) preparation of water phase：First 8 parts of chlorinated polyethylenees, 4 parts of sesbania gums and 1 part of agar powder are added in 300 parts of water, and
60-65 DEG C of insulation mixing 15min is heated to, 6 parts of water-soluble chitosans and 3 parts of PAMAs is subsequently adding, is continued
Backflow insulation mixing 15min, gained mixture is cooled to -5-0 DEG C in 5min under ice salt bath, and is incubated at -5-0 DEG C quiet
2h is put, and finally twice homogenization is carried out under 65-70 DEG C of homogenizing temperature, homogenization pressure 20-25MPa, is obtained final product aqueous phase solution；
(2) preparation of oil phase：25 parts of divinylbenzene and 15 parts of porogen are heated to into 75-80 DEG C of insulation mixing first
15min, adds 80 parts of styrene and 50 parts of hydroxyethyl methylacrylates, is sufficiently mixed after microwave frequency 2450MHz, power
Microwave treatment 5min under 700W, continues microwave treatment 5min after standing 45min, obtains final product oil mixture；
(3) suspension polymerization：6 parts of linear low density polyethylene and 0.5 part of vitamin C phosphoric acid are added in aqueous phase solution
Ester magnesium, is heated to reflux state isothermal holding 15min, adds oil mixture, continues isothermal holding 5h at reflux,
Then 5 parts of N, N- dimethylaminoethyls and 1 part of Sodium Polystyrene Sulfonate, insulation mixing 15min, by gained mixture are added while hot
Cooled with the speed of 10-15 DEG C/min under ice salt bath, the insulation after temperature is down to 0-5 DEG C stands 2h, filters, gained filter
Cake is washed 3 times with 60-65 DEG C of 2-3wt% sodium chloride solutions, and 5h is dried at 100-105 DEG C, finally with 0.5mm apertures
Screen filtration, obtains final product transparent spherical resin；
(4) functionalization：4 parts of N-phenylmaleimides, 2 parts of sodium tripolyphosphates and 0.5 part of methyl hydroxybenzoate are added
In 25 parts of ethanol, reflux state insulation mixing 15min is heated to, transparent spherical resin surface is then uniformly sprayed on, is stood
30min, then at microwave treatment 5min under microwave frequency 2450MHz, power 700W, process proceeds to rapidly 0-5 DEG C of environment after terminating
Middle standing 3h, microwave treatment 5min, is dried 3h at gained spherical particle is placed in 100-105 DEG C finally, obtains final product goal tree again
Fat.
The modification of sesbania gum：15 parts of sesbania gums are added in 5 times of weight portion water, and it is mixed to be heated to reflux state insulation
10min is closed, 3 parts of polyvinyl butyral resins and 0.5 part of 2- picoline is added, is continued in reflux state insulation mixing 30min,
Then sealing and standing in 0-5 DEG C of environment is proceeded to rapidly, after 3h, 1 part of microwax and 1 part of Oleum Terebinthinae is added in gained mixture, then
It is secondary to be heated to reflux state insulation mixing 10min, it is subsequently sent in freezer dryer, Jing after being fully dried by gained solid abrasive
Into powder, 0.5 part of oleamide and 0.5 part of ferrocene are eventually adding, are sufficiently mixed after microwave frequency 2450MHz, power
Microwave treatment 5min under 700W, obtains final product modified sesbania gum.
The pretreatment of microwax：By 15 parts of microwaxes be heated to completely melting after insulation mixing 5min, add 1 part it is hydrophilic
Property aerosil, 1 part of dimethyl diallyl ammonium chloride and 0.5 part of epoxy soybean oil, are sufficiently mixed after microwave frequency
Microwave treatment 5min under 2450MHz, power 700W, continues microwave treatment 3min after standing 60min, then drips gained fused mass
It is added in 5-10 DEG C of cold water, forms spherical particle, filter, gained spherical particle is sent in freezer dryer and is fully dried.
Embodiment 3
5 parts will be divided into after being sufficiently mixed with batch starch saccharificating liquid, be utilized respectively 1 and 2 made tree of the embodiment of the present invention
Fat carries out desolventing technology, and compares commercial resins D318, DM-301 and AB-8, and its percent of decolourization is measured, as a result such as 1 institute of table
Show.
The decolorizing effect of 1 embodiment of table, 1 and 2 made resin
| Project | Embodiment 1 | Embodiment 2 | D318 | DM-301 | AB-8 |
| Percent of decolourization | 98.8% | 98.5% | 91.2% | 92.4% | 91.8% |
As shown in Table 1,1 and 2 made resin of the embodiment of the present invention is better than commercially available tree to the decolorizing effect of starch saccharificating liquid
Fat D318, DM-301 and AB-8, percent of decolourization reach more than 98%.
1 and 2 made resin of the embodiment of the present invention is regenerated twice, the resin after regeneration is re-used for into starch then
The desolventing technology of saccharified liquid, is measured to its primary recycling and the percent of decolourization after secondary recycling, as a result as shown in table 2 respectively.
Treatment effect after 2 made resin regeneration of table
As shown in Table 2, percent of decolourization of the 1 and 2 made attached resin of the embodiment of the present invention Jing after primary recycling to starch saccharificating liquid
More than 93%, the percent of decolourization Jing after secondary recycling illustrates 1 and 2 made resin of the embodiment of the present invention still more than 90%, thus
Reproducibility it is good, long service life.
The ultimate principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and description this
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement is both fallen within scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (5)
1. a kind of starch saccharificating liquid special decolouring resin, it is characterised in that be made up of the raw material of following parts by weight：
Styrene 70-80 parts, hydroxyethyl methylacrylate 40-50 parts, divinylbenzene 20-30 part, porogen 15-20 parts, chlorine
Change polyethylene 6-11 parts, linear low density polyethylene 4-8 part, water-soluble chitosan 4-8 parts, N, N- dimethylaminoethyl 3-6 parts,
Sesbania gum 3-6 parts, PAMA 3-6 parts, N-phenylmaleimide 2-4 parts, sodium tripolyphosphate 2-4 parts, polyphenyl
Vinyl sulfonic acid sodium 1-2 parts, agar powder 1-2 parts, methyl hydroxybenzoate 0.5-1 parts, Magnesium L-Asacorbic Acid 2-O-Phosphate 0.5-1 parts, ethanol 20-30
Part, water 250-300 parts.
2. starch saccharificating liquid special decolouring resin according to claim 1, it is characterised in that：The sesbania gum uses front Jing
Modification is crossed, its processing method is：10-15 parts sesbania gum is added in 3-5 times of weight portion water, and is heated to reflux state guarantor
Temperature mixing 5-10min, adds 2-3 parts polyvinyl butyral resin and 0.5-1 part 2- picolines, continues to be incubated in reflux state
Mixing 15-30min, then proceeds to rapidly sealing and standing in 0-5 DEG C of environment, adds 1-2 parts micro- after 3-5h in gained mixture
Brilliant wax and 0.5-1 part Oleum Terebinthinaes, are again heated to reflux state insulation mixing 10-15min, are subsequently sent in freezer dryer,
Gained solid abrasive is eventually adding 0.5-1 parts oleamide and 0.3-0.5 part ferrocene, is filled into powder Jing after being fully dried
Divide mixing microwave treatment 3-5min under microwave frequency 2450MHz, power 700W, obtain final product modified sesbania gum.
3. starch saccharificating liquid special decolouring resin according to claim 2, it is characterised in that：The microwax uses front Jing
Pretreatment is crossed, its processing method is：10-15 part microwaxes are heated to into insulation mixing 5-10min after melting completely, 1- is added
2 parts of hydrophilic fumed silicas, 0.5-1 parts dimethyl diallyl ammonium chloride and 0.5-1 part epoxy soybean oils, are sufficiently mixed
Microwave treatment 3-5min under microwave frequency 2450MHz, power 700W, continues microwave treatment 2- after standing 30-60min
3min, is then added drop-wise to gained fused mass in 5-10 DEG C of cold water, forms spherical particle, filters, and gained spherical particle is sent into
Fully it is dried in freezer dryer.
4. starch saccharificating liquid special decolouring resin according to claim 1, it is characterised in that its preparation method includes as follows
Step：
(1) preparation of water phase：It is first that chlorinated polyethylene, sesbania gum and agar powder are added in water, and it is mixed to be heated to 60-65 DEG C of insulation
10-15min is closed, water-soluble chitosan and PAMA is subsequently adding, continues backflow insulation mixing 10-15min, institute
Obtain mixture and -5-0 DEG C is cooled in 3-5min under ice salt bath, and insulation stands 1-2h at -5-0 DEG C, finally in homogenizing
Twice homogenization is carried out under temperature 65-70 DEG C, homogenization pressure 20-25MPa, aqueous phase solution is obtained final product；
(2) preparation of oil phase：Divinylbenzene and porogen are heated to into 75-80 DEG C of insulation mixing 10-15min first, are added
Styrene and hydroxyethyl methylacrylate, are sufficiently mixed microwave treatment 3- under microwave frequency 2450MHz, power 700W
5min, continues microwave treatment 3-5min after standing 30-60min, obtains final product oil mixture；
(3) suspension polymerization：Linear low density polyethylene and Magnesium L-Asacorbic Acid 2-O-Phosphate are added in aqueous phase solution, is heated to
Reflux state isothermal holding 10-15min, adds oil mixture, continues isothermal holding 3-5h at reflux, then takes advantage of
Heat adds N, N- dimethylaminoethyls and Sodium Polystyrene Sulfonate, insulation mixing 15-20min, by gained mixture in ice salt bath
Under cooled with the speed of 10-15 DEG C/min, after temperature is down to 0-5 DEG C insulation stand 1-2h, filter, gained filter cake use
60-65 DEG C of 2-3wt% sodium chloride solutions are washed 3 times, and 3-5h is dried at 100-105 DEG C, finally with the sieve in 0.5mm apertures
Net filtration, obtains final product transparent spherical resin；
(4) functionalization：N-phenylmaleimide, sodium tripolyphosphate and methyl hydroxybenzoate are added in ethanol, is heated to back
Stream mode insulation mixing 10-15min, is then uniformly sprayed on transparent spherical resin surface, stands 15-30min, then at microwave frequency
Microwave treatment 3-5min under 2450MHz, power 700W, process stand 2-3h in proceeding to rapidly 0-5 DEG C of environment after terminating, micro- again
Ripple processes 3-5min, is dried 2-3h, obtains final product target resin at gained spherical particle is placed in 100-105 DEG C finally.
5. starch saccharificating liquid special decolouring resin according to claim 1, it is characterised in that：The porogen is selected from first
The mixed solution of one kind or toluene and dimethylbenzene in benzene, dimethylbenzene.
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| CN201611166808.2A CN106674446A (en) | 2016-12-16 | 2016-12-16 | Special decolorization resin for starch saccharification liquid |
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| CN201611166808.2A CN106674446A (en) | 2016-12-16 | 2016-12-16 | Special decolorization resin for starch saccharification liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278105A (en) * | 2021-04-30 | 2021-08-20 | 广西叁万生物科技有限公司 | Decolorizing resin for lactase and preparation method thereof |
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