CN107384630A - A kind of preparation method of reactive dye absorbent-type biology enzyme soaping agent - Google Patents
A kind of preparation method of reactive dye absorbent-type biology enzyme soaping agent Download PDFInfo
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- CN107384630A CN107384630A CN201710510214.7A CN201710510214A CN107384630A CN 107384630 A CN107384630 A CN 107384630A CN 201710510214 A CN201710510214 A CN 201710510214A CN 107384630 A CN107384630 A CN 107384630A
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- Prior art keywords
- soaping agent
- reactive dye
- biology enzyme
- preparation
- parts
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 37
- 108090000790 Enzymes Proteins 0.000 title claims abstract description 31
- 102000004190 Enzymes Human genes 0.000 title claims abstract description 31
- 239000000985 reactive dye Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 210000002268 wool Anatomy 0.000 claims abstract description 55
- 108010076876 Keratins Proteins 0.000 claims abstract description 30
- 102000011782 Keratins Human genes 0.000 claims abstract description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 22
- 108010029541 Laccase Proteins 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000012530 fluid Substances 0.000 claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000855 fermentation Methods 0.000 claims abstract description 13
- 230000004151 fermentation Effects 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 11
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 11
- 241000233866 Fungi Species 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 27
- 229920000159 gelatin Polymers 0.000 claims description 13
- 235000019322 gelatine Nutrition 0.000 claims description 13
- 108010010803 Gelatin Proteins 0.000 claims description 11
- 239000008273 gelatin Substances 0.000 claims description 11
- 235000011852 gelatine desserts Nutrition 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 6
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical class O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001828 Gelatine Substances 0.000 claims description 2
- 238000012870 ammonium sulfate precipitation Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000000502 dialysis Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical class CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 13
- 239000004744 fabric Substances 0.000 abstract description 13
- 239000000344 soap Substances 0.000 abstract description 9
- 238000004043 dyeing Methods 0.000 abstract description 8
- 238000007639 printing Methods 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 5
- 239000006260 foam Substances 0.000 abstract description 5
- 238000010186 staining Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000000975 dye Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000000047 product Substances 0.000 description 13
- 239000003643 water by type Substances 0.000 description 13
- 239000002609 medium Substances 0.000 description 9
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- -1 polypropylene Polymers 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000004094 surface-active agent Substances 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 4
- 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 description 4
- 229930006000 Sucrose Natural products 0.000 description 4
- 240000008042 Zea mays Species 0.000 description 4
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 4
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 4
- 238000007605 air drying Methods 0.000 description 4
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 4
- 235000011130 ammonium sulphate Nutrition 0.000 description 4
- 239000007853 buffer solution Substances 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- 235000015165 citric acid Nutrition 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 235000005822 corn Nutrition 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 239000001963 growth medium Substances 0.000 description 4
- 239000002054 inoculum Substances 0.000 description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 235000019796 monopotassium phosphate Nutrition 0.000 description 4
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical class [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- 239000005720 sucrose Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- HFEWAGKDZLEFCT-UHFFFAOYSA-L C(C)C(COP(=O)(OCC(CCCC)CC)[O-])CCCC.P(=O)(O)([O-])O.[Na+].[Na+] Chemical compound C(C)C(COP(=O)(OCC(CCCC)CC)[O-])CCCC.P(=O)(O)([O-])O.[Na+].[Na+] HFEWAGKDZLEFCT-UHFFFAOYSA-L 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004900 laundering Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- LEAHFJQFYSDGGP-UHFFFAOYSA-K trisodium;dihydrogen phosphate;hydrogen phosphate Chemical compound [Na+].[Na+].[Na+].OP(O)([O-])=O.OP([O-])([O-])=O LEAHFJQFYSDGGP-UHFFFAOYSA-K 0.000 description 1
- 235000015099 wheat brans Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38672—Granulated or coated enzymes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/40—Products in which the composition is not well defined
- C11D7/46—Animal products
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/40—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using enzymes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Zoology (AREA)
- Coloring (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Detergent Compositions (AREA)
Abstract
A kind of preparation method the invention discloses reactive dye with absorbent-type biology enzyme soaping agent, belongs to printing and dyeing assistant preparing technical field.The present invention carries out cultivation and fermentation first with self-control fermentation medium to white-rot fungi, by obtained zymotic fluid through centrifuging to obtain crude enzyme liquid, again alkaline laccase is prepared by raw material of crude enzyme liquid, and prepare wool keratin solution by raw material of wool, again after modified with alkaline laccase, centrifuged after the mixing such as Tween 80/atoleine, then collect and precipitate and wash precipitation with acetone and isopropanol, most afterwards through drying obtained reactive dye absorbent-type biology enzyme soaping agent, gained soaping agent of the invention has preferably soap effect and anti-staining effect, make to soap the soaping fastness of fabric and crock fastness reaches more than 3 grades, and non-foam produces during soaping using soaping agent of the present invention, fabric washing number can effectively be reduced, greatly reduce energy resource consumption.
Description
Technical field
A kind of preparation method the invention discloses reactive dye with absorbent-type biology enzyme soaping agent, belongs to printing and dyeing assistant system
Standby technical field.
Background technology
Non- set or hydrolysis dyestuff be present in fabric surface after dyeing or stamp（Frequently referred to loose colour）, slurry and chemistry
Auxiliary agent.If this some dyes, slurry and chemical assistant are not removed totally, will influence color fastness, the vividness of fabric, because
This must carry out soap washing to dyed fabric, and be risen as the after treatment aid of dyeing and printing process, soaping agent during soaping
Critically important effect.
During soaping, soaping agent washes away the activity dye combined with fiber loosely by the way that chemical action occurs with dyestuff
Expect and slough printing gum, while the dyestuff of removing is not returned and be stained with cloth cover, reach and improve fastness and prevent that PRINTED FABRIC is white
The purpose of ground staining.Traditional soaping agent various types, according to mechanism difference of soaping, conventional soaping agent can be divided into surface-active
Agent class（Such as anion, nonionic surfactant）, chelating class（Such as polyphosphinates class）, the scattered class of chelating（Such as polypropylene
Hydrochlorate）With compounding class etc., wherein the most widely used is surfactant-based soaping agent.
Although conventional surfactant class soaping agent removes effect with good loose colour, phenomenon of stripping simultaneously be present,
The effect that causes to soap is substantially reduced, and conventional surfactant class soaping agent foam is more, and foam is difficult in dyeing process
Wash away and washed, it is necessary to consume massive laundering, energy resource consumption is very big.
Therefore, one kind how is made and soaps that effect is good, the less no alveolitoid soaping agent that can improve fabric color fastness, energy consumption,
It is the important technical difficult point that the research staff of printing and dyeing industry are faced, while is also each printing and dyeing enterprise technology urgently to be resolved hurrily
Problem.
The content of the invention
Present invention mainly solves technical problem：Phenomenon of stripping be present for traditional soaping agent, cause to soap effect significantly
Reduce, and surfactant-based soaping agent foam is more, is difficult to wash away in dyeing process and is washed, it is necessary to consume massive laundering, energy
A kind of the defects of source consumption is larger, there is provided the preparation method of reactive dye absorbent-type biology enzyme soaping agent.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of reactive dye absorbent-type biology enzyme soaping agent, it is wall by modified wool keratin composite gelatin
Material, embed alkaline laccase.
It is specially prepared by following weight parts raw material：
By 100~200 parts of modified wool keratin solutions, 150~300 parts of gelatin solutions, 1~2 part of alkaline laccase is well mixed
It is fitted into afterwards in 600~800 parts of Tween-80/atoleines, 10~15min is stirred at 60~70 DEG C, is cooled to 10~15 DEG C,
30~50 parts of glutaraldehydes are added, are centrifuged after continuing 1~2h of stirring, and are done after washing precipitated product with acetone and isopropanol
It is dry to be made.
The modified wool keratin solution is through cetyl trimethyl ammonium chloride and epoxychloropropane modified wool
Keratin solution.
The wool keratin solution modifying process is specially by 60~80 parts by weight cetyl trimethyl ammonium chlorides, is added
Enter 15~20min of stirring in 60~100 parts by weight absolute ethyl alcohols, then 10~15 parts by weight epoxy chloropropanes are added dropwise, 25~32
At DEG C, 3~4h of stirring reaction, 100~300 parts by weight wool keratin solutions are added, at 50~70 DEG C, stir 3~5h
It is made.
Institute's gelatine solution is the gelatin solution of mass fraction 10%.
The alkaline laccase is that white-rot fungi oscillation and fermentation in alkaline medium centrifuges zymotic fluid after 8~10 days,
Again through the tert-butyl alcohol and ammonium sulfate precipitation, with citric acid 30~50min will be stood under ice-water bath after the scattered dialysis of precipitation, then from
The heart is separated and dried and is made.
Tween-80/the atoleine is the Tween-80 atoleine of mass fraction 5%.
Compared with other method, advantageous effects are the present invention：
The present invention by amino, hydroxyl, carboxyl isoreactivity group present on modified wool keratin and gelatin macromolecular chain, with
Hydroxyl, amino, azo group, sulfonic group in reactive dyestuff molecule are combined in a manner of ionic bond or hydrogen bond, so as to improve dyestuff
Active force between fiber, reduces dyestuff water solubility, and the reactive group contained simultaneously can occur with hydrolised dye and fiber
Reaction, and then by the crosslinked action of cationic protein, hydrolised dye is crosslinked fixation on fiber, reduce the loose colour on fabric
Amount, recycle alkaline laccase that the dyestuff of non-set and hydrolised dye are catalytically decomposed, be scattered in the dye stabilizer for making to come off and wash
In liquid, dyestuff staining fabric again is prevented, can effectively remove remaining loose colour, reduces washing water consumption.
Embodiment
Weigh 50~55g ammonium chlorides, 1.5~2.0g potassium dihydrogen phosphates, 1.0~1.2g Salzburg vitriols, 1~2g chlorinations
Sodium, 0.8~1.0g magnesium sulfate, 100~120g wheat brans, 10~12g corn flour, 15~20g sucrose, 0.5~0.8g calcium chloride, add
Enter in 1.0~1.2L deionized waters, 20~30min is stirred with 200~300r/min, obtains fermentation medium, then with quality point
Number adjusts medium pH to 9.0~9.5 for 1% sodium hydroxide solution, and by inoculum concentration 10~15%, white-rot fungi is seeded into fermentation
In culture medium, at 30~32 DEG C, with 200~240r/min oscillation and fermentations 8~10 days, 9~10L deionized waters are added,
At 28~30 DEG C, 2~3h is vibrated with 200~240r/min, obtains zymotic fluid, then zymotic fluid is placed in supercentrifuge, with
10000~12000r/min centrifuges 8~10min, collects supernatant, obtains crude enzyme liquid, then add the tertiary fourths of 2.0~2.4L to crude enzyme liquid
Alcohol, 200~220g ammonium sulfate, at 25~30 DEG C, it is transferred in centrifuge after standing 1~2h, is centrifuged in 5000~5500r/min
12~15min, precipitation is collected, the disodium hydrogen phosphate-phosphate sodium dihydrogen buffer solution that will be precipitated with 150~200mLpH is 7.5, dress
Enter and dialysed 2~3 times in the bag filter that flux is 5000~10000 dalton, take trapped fluid and add 3~5g citric acids, in ice
30~50min is stood under water-bath, adds 100~150mL-20 DEG C of acetone, and is transferred in centrifuge, at 2~4 DEG C, with
12000~12500r/min centrifuges 5~8min, collects sediment, obtains alkaline laccase after natural air drying, take wool, use matter successively
It is that 1% acetum and deionized water wash wool 2~3 times to measure fraction, then the wool after cleaning is fitted into baking oven, 50~
2~3h is dried at 55 DEG C, dried wool is transferred in cutter shearing to 2~5mm, obtains short wool, then weigh 100~
200g short wools add 1~2L mass fractions, under 80~90 DEG C of waters bath with thermostatic control, with 300~
400r/min stirs 3~5h, adds 10~20g activated carbons, is filtered after stirring 1~2h with 500~600r/min, collects filter
Liquid, wool keratin solution is obtained, then weigh 60~80g cetyl trimethyl ammonium chlorides, add 80~100mL absolute ethyl alcohols
In, 15~20min is stirred with 300~400r/min, then 10~12mL epoxychloropropane is added dropwise with 0.5mL/min, 28~32
Under DEG C water bath with thermostatic control, 3~4h of stirring reaction, 100~200mL wool keratin solutions are added, at 50~70 DEG C, continue to stir
3~5h is mixed, obtains modified wool keratin solution, finally takes 100~200g modified wool keratin solutions, 150~300g mass
Fraction is 10% gelatin solution, and it is 5% Tween-80/liquid to load 600~800g mass fractions after 1~2g alkalescence laccase is well mixed
In body paraffin, 10~15min is stirred with 300~400r/min at 60~70 DEG C, is cooled to 10~15 DEG C, add 30~
50g glutaraldehydes, continue to be transferred in centrifuge after 1~2h of stirring to centrifuge, precipitated product is collected, successively with acetone and isopropanol
Wash precipitated product 5~8 times, the precipitated product after washing is placed in drying box, 3~5h is dried at 70~80 DEG C, obtains work
Property dyestuff absorbent-type biology enzyme soaping agent.
Example 1
Weigh 50g ammonium chlorides, 1.5g potassium dihydrogen phosphates, 1.0g Salzburg vitriols, 1g sodium chloride, 0.8g magnesium sulfate, 100g brans
Skin, 10g corn flour, 15g sucrose, 0.5g calcium chloride, add in 1.0L deionized waters, 20min is stirred with 200r/min, must be fermented
Culture medium, it is then that 1% sodium hydroxide solution adjusts medium pH to 9.0 with mass fraction, by inoculum concentration 10%, by white-rot fungi
It is seeded in fermentation medium, at 30 DEG C, with 200r/min oscillation and fermentations 8 days, adds 9L deionized waters, at 28 DEG C,
2h is vibrated with 200r/min, obtains zymotic fluid, then zymotic fluid is placed in supercentrifuge, 8min is centrifuged with 10000r/min, received
Collect supernatant, obtain crude enzyme liquid, then the 2.0L tert-butyl alcohols are added to crude enzyme liquid, 200g ammonium sulfate, at 25 DEG C, stand be transferred to after 1h from
In scheming, 12min is centrifuged in 5000r/min, collects precipitation, the disodium hydrogen phosphate-di(2-ethylhexyl)phosphate that will be precipitated with 150mLpH is 7.5
Hydrogen sodium buffer solution, it is fitted into the bag filter that flux is 5000 dalton and dialyses 2 times, take trapped fluid and add 3g citric acids, in ice
Stand 30min under water-bath, add 100mL-20 DEG C of acetone, and be transferred in centrifuge, at 2 DEG C, with 12000r/min from
Heart 5min, sediment is collected, alkaline laccase is obtained after natural air drying, takes wool, for 1% acetum and gone with mass fraction successively
Ion water washing wool 2 times, then the wool after cleaning is fitted into baking oven, 2h is dried at 50 DEG C, dried wool is turned
Enter shearing in cutter and, to 2mm, obtain short wool, then it is 2% sodium hydroxide solution to weigh 100g short wools to add 1L mass fractions
In, under 80 DEG C of water bath with thermostatic control, 3h is stirred with 300r/min, adds 10g activated carbons, is filtered after stirring 1h with 500r/min,
Filtrate is collected, obtains wool keratin solution, then weighs 60g cetyl trimethyl ammonium chlorides, is added in 80mL absolute ethyl alcohols, with
300r/min stirs 15min, then 10mL epoxychloropropane, under 28 DEG C of waters bath with thermostatic control, stirring reaction is added dropwise with 0.5mL/min
3h, 100mL wool keratin solutions are added, at 50 DEG C, continue to stir 3h, obtain modified wool keratin solution, finally take
100g modified wool keratin solutions, 150g mass fractions are 10% gelatin solution, load 600g after 1g alkalescence laccase is well mixed
Mass fraction is in 5% Tween-80/atoleine, stirs 10min with 300r/min at 60 DEG C, is cooled to 10 DEG C, adds
30g glutaraldehydes, continue to be transferred in centrifuge and centrifuge after stirring 1h, collect precipitated product, washed successively with acetone and isopropanol
Wash precipitated product 5 times, the precipitated product after washing is placed in drying box, 3h is dried at 70 DEG C, obtain reactive dye absorption
Type biology enzyme soaping agent.Example 2
Weigh 53g ammonium chlorides, 1.8g potassium dihydrogen phosphates, 1.1g Salzburg vitriols, 1g sodium chloride, 0.9g magnesium sulfate, 110g brans
Skin, 11g corn flour, 18g sucrose, 0.7g calcium chloride, add in 1.1L deionized waters, 25min is stirred with 250r/min, must be fermented
Culture medium, it is then that 1% sodium hydroxide solution adjusts medium pH to 9.3 with mass fraction, by inoculum concentration 13%, by white-rot fungi
It is seeded in fermentation medium, at 31 DEG C, with 220r/min oscillation and fermentations 9 days, adds 9L deionized waters, at 29 DEG C,
2h is vibrated with 220r/min, obtains zymotic fluid, then zymotic fluid is placed in supercentrifuge, 9min is centrifuged with 11000r/min, received
Collect supernatant, obtain crude enzyme liquid, then the 2.2L tert-butyl alcohols are added to crude enzyme liquid, 210g ammonium sulfate, at 28 DEG C, stand be transferred to after 1h from
In scheming, 14min is centrifuged in 5250r/min, collects precipitation, the disodium hydrogen phosphate-di(2-ethylhexyl)phosphate that will be precipitated with 175mLpH is 7.5
Hydrogen sodium buffer solution, it is fitted into the bag filter that flux is 7500 dalton and dialyses 2 times, take trapped fluid and add 4g citric acids, in ice
Stand 40min under water-bath, add 125mL-20 DEG C of acetone, and be transferred in centrifuge, at 3 DEG C, with 12250r/min from
Heart 7min, sediment is collected, alkaline laccase is obtained after natural air drying, takes wool, for 1% acetum and gone with mass fraction successively
Ion water washing wool 2 times, then the wool after cleaning is fitted into baking oven, 2h is dried at 53 DEG C, dried wool is turned
Enter shearing in cutter and, to 4mm, obtain short wool, then it is 2% sodium hydroxide solution to weigh 150g short wools to add 1L mass fractions
In, under 85 DEG C of water bath with thermostatic control, 4h is stirred with 350r/min, adds 15g activated carbons, is filtered after stirring 1h with 550r/min,
Filtrate is collected, obtains wool keratin solution, then weighs 70g cetyl trimethyl ammonium chlorides, is added in 90mL absolute ethyl alcohols, with
350r/min stirs 18min, then 11mL epoxychloropropane, under 30 DEG C of waters bath with thermostatic control, stirring reaction is added dropwise with 0.5mL/min
3h, 150mL wool keratin solutions are added, at 60 DEG C, continue to stir 4h, obtain modified wool keratin solution, finally take
150g modified wool keratin solutions, 225g mass fractions are 10% gelatin solution, load 700g after 1g alkalescence laccase is well mixed
Mass fraction is in 5% Tween-80/atoleine, stirs 13min with 350r/min at 65 DEG C, is cooled to 13 DEG C, adds
40g glutaraldehydes, continue to be transferred in centrifuge and centrifuge after stirring 1h, collect precipitated product, washed successively with acetone and isopropanol
Wash precipitated product 7 times, the precipitated product after washing is placed in drying box, 4h is dried at 75 DEG C, obtain reactive dye absorption
Type biology enzyme soaping agent.Example 3
Weigh 55g ammonium chlorides, 2.0g potassium dihydrogen phosphates, 1.2g Salzburg vitriols, 2g sodium chloride, 1.0g magnesium sulfate, 120g brans
Skin, 12g corn flour, 20g sucrose, 0.8g calcium chloride, add in 1.2L deionized waters, 30min is stirred with 300r/min, must be fermented
Culture medium, it is then that 1% sodium hydroxide solution adjusts medium pH to 9.5 with mass fraction, by inoculum concentration 15%, by white-rot fungi
It is seeded in fermentation medium, at 32 DEG C, with 240r/min oscillation and fermentations 10 days, 10L deionized waters is added, at 30 DEG C
Under, 3h is vibrated with 240r/min, obtains zymotic fluid, then zymotic fluid is placed in supercentrifuge, centrifuged with 12000r/min
10min, supernatant is collected, obtain crude enzyme liquid, then the 2.4L tert-butyl alcohols are added to crude enzyme liquid, 220g ammonium sulfate, at 30 DEG C, stand 2h
After be transferred in centrifuge, 5500r/min centrifuge 15min, collect precipitation, will precipitate with 200mLpH be 7.5 phosphoric acid hydrogen two
Sodium-phosphate sodium dihydrogen buffer solution, it is fitted into the bag filter that flux is 10000 dalton and dialyses 3 times, take trapped fluid and add 5g lemons
Lemon acid, stands 50min under ice-water bath, adds 150mL-20 DEG C of acetone, and is transferred in centrifuge, at 4 DEG C, with
12500r/min centrifuges 8min, collects sediment, obtains alkaline laccase after natural air drying, take wool, is successively 1% with mass fraction
Acetum and deionized water washing wool 3 times, then wool after cleaning are fitted into baking oven, and 3h is dried at 55 DEG C, will be done
Wool after dry is transferred to shearing in cutter and, to 5mm, obtains short wool, then it is 2% hydrogen to weigh 200g short wools to add 2L mass fractions
In sodium hydroxide solution, under 90 DEG C of waters bath with thermostatic control, 5h is stirred with 400r/min, 20g activated carbons is added, is stirred with 600r/min
Filtered after 2h, collect filtrate, obtain wool keratin solution, then weigh 80g cetyl trimethyl ammonium chlorides, add 100mL without
In water-ethanol, 20min is stirred with 400r/min, then 12mL epoxychloropropane is added dropwise with 0.5mL/min, in 32 DEG C of waters bath with thermostatic control
Under, stirring reaction 4h, 200mL wool keratin solutions are added, at 70 DEG C, continue to stir 5h, obtain modified wool keratin
Solution, 200g modified wool keratin solutions are finally taken, 300g mass fractions are 10% gelatin solution, and the mixing of 2g alkalescence laccase is equal
It is fitted into 800g mass fractions after even in 5% Tween-80/atoleine, to stir 15min with 400r/min at 70 DEG C, being cooled to
15 DEG C, 50g glutaraldehydes are added, continues to be transferred in centrifuge and centrifuge after stirring 2h, collects precipitated product, use acetone successively
Precipitated product is washed with isopropanol 8 times, and the precipitated product after washing is placed in drying box, 5h is dried at 80 DEG C, is obtained active
Dyestuff absorbent-type biology enzyme soaping agent.It is with absorbent-type biology enzyme soaping agent by reactive dye made from present example 1~3
Example and commercially available soaping agent（Comparative example）Application effect contrast is carried out, its result is as shown in table 1：
Soaping agent application process：In mass ratio 1:500, soaping agent and water are stirred 5min, must soap liquid, then by bath raio
1:20, after the 20min that soaped in dyed cotton fabric and liquid of soaping, further take out after the dyed cotton fabric after soaping is cleaned with 15 DEG C of water and dry
.
1 reactive dye of the present invention of table are soaped Contrast on effect with absorbent-type biology enzyme soaping agent and commercially available soaping agent
In summary, reactive dye produced by the present invention absorbent-type biology enzyme soaping agent has preferable anti-staining effect and soap
Effect is washed, the color fastness of fabric after soaping can be effectively provided, and non-foam produces during soaping, and can substantially reduce water consumption,
Raising soap efficiency while reduce energy consumption.
Claims (7)
1. a kind of reactive dye preparation method of absorbent-type biology enzyme soaping agent, it is characterised in that by modified wool keratin
Composite gelatin is wall material, embeds alkaline laccase.
A kind of 2. preparation method of reactive dye absorbent-type biology enzyme soaping agent as claimed in claim 1, it is characterised in that
Specially prepared by following weight parts raw material：
By 100~200 parts of modified wool keratin solutions, 150~300 parts of gelatin solutions, 1~2 part of alkaline laccase is well mixed
It is fitted into afterwards in 600~800 parts of Tween-80/atoleines, 10~15min is stirred at 60~70 DEG C, is cooled to 10~15 DEG C,
30~50 parts of glutaraldehydes are added, are centrifuged after continuing 1~2h of stirring, and are done after washing precipitated product with acetone and isopropanol
It is dry to be made.
A kind of 3. preparation method of reactive dye absorbent-type biology enzyme soaping agent as claimed in claim 2, it is characterised in that
The modified wool keratin solution is molten through cetyl trimethyl ammonium chloride and epoxychloropropane modified wool keratin
Liquid.
A kind of 4. preparation method of reactive dye absorbent-type biology enzyme soaping agent as claimed in claim 3, it is characterised in that
The wool keratin solution modifying process is specially by 60~80 parts by weight cetyl trimethyl ammonium chlorides, add 60~
15~20min is stirred in 100 parts by weight absolute ethyl alcohols, then 10~15 parts by weight epoxy chloropropanes are added dropwise, at 25~32 DEG C, is stirred
3~4h of reaction is mixed, adds 100~300 parts by weight wool keratin solutions, at 50~70 DEG C, 3~5h of stirring is made.
A kind of 5. preparation method of reactive dye absorbent-type biology enzyme soaping agent as claimed in claim 2, it is characterised in that
Institute's gelatine solution is the gelatin solution of mass fraction 10%.
A kind of 6. preparation method of reactive dye absorbent-type biology enzyme soaping agent as claimed in claim 2, it is characterised in that
The alkaline laccase is that white-rot fungi oscillation and fermentation in alkaline medium centrifuges zymotic fluid after 8~10 days, then through tertiary fourth
Alcohol and ammonium sulfate precipitation, after the scattered dialysis of precipitation, 30~50min is stood under ice-water bath with citric acid, then centrifuge simultaneously
Dry and be made.
A kind of 7. preparation method of reactive dye absorbent-type biology enzyme soaping agent as claimed in claim 2, it is characterised in that
Tween-80/the atoleine is the Tween-80 atoleine of mass fraction 5%.
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| CN112642404A (en) * | 2020-12-01 | 2021-04-13 | 安徽鸿昌糖业科技有限公司 | Degradable adsorbent and preparation method and application thereof |
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