CN105063092A - Method for preparing lithospermum erythrorhizon natural dyestuff through immobilized enzyme - Google Patents
Method for preparing lithospermum erythrorhizon natural dyestuff through immobilized enzyme Download PDFInfo
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- CN105063092A CN105063092A CN201510554272.0A CN201510554272A CN105063092A CN 105063092 A CN105063092 A CN 105063092A CN 201510554272 A CN201510554272 A CN 201510554272A CN 105063092 A CN105063092 A CN 105063092A
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Abstract
The invention discloses a method for preparing lithospermum erythrorhizon natural dyestuff through immobilized enzyme, which belongs to the technical field of textile dyeing, and utilizes glycidyl methacrylate to prepare resins for immobilized enzyme, and is vibrated with citric acid-sodium citrate buffer solution, cellulose and xylanase mixture in constant temperature, and then deionized water, immobilized enzyme resins, lithospermum erythrorhizon crushed mixture and the citric acid-sodium citrate buffer solution are added to mix in a temperature, thereby obtaining lithospermum erythrorhizon natural dyestuff after enzymolysis, heating, cooling and filtering. The method for preparing the lithospermum erythrorhizon natural dyestuff through the immobilized enzyme has the beneficial effects that the prepared lithospermum erythrorhizon natural dyestuff is green and safe, does not have pollution to environment and does not have harm to human health. The immobilized enzyme can be reused, achieves cyclic utilization of resources, saves production cost of the lithospermum erythrorhizon natural dyestuff, and is worthy of promotion and use.
Description
Technical field
The present invention relates to a kind of method that immobilized enzyme prepares natural gromwell dye, belong to dope dyeing technical field.
Background technology
In recent years, the competition of substantive dyestuff industry, the requirement of people to weaving color is also improving constantly, and the environment-friendly dye also more and more higher to the requirement of dyestuff, bright in luster, dye uptake is high, salt-free liquid dye are favourably welcome; In the traditional processing technology of substantive dyestuff, generally will through oversalting, filtration and the technological process such as concentrated; Object is desalination, removes unreacted raw material, intermediate and secondary dyestuff, sloughs moisture, obtain the dyestuff of desired concn and purity, then carries out in baking oven dry, makes powder or liquid dye.Facts have proved, a large amount of sodium-chlor is employed in salting-out process, a large amount of waste water can be produced again, the discharge of waste water not only makes the useful matter such as industrial chemicals and intermediate wherein contained slattern, desired raw material is many, also can cause great pollution to environment, seriously govern the tremendous expansion of dyestuffs industries, the dyestuff simultaneously made also entail dangers to people's is healthy.
Summary of the invention
Technical problem to be solved by this invention: for the raw material of dyestuff at substantial prepared by traditional technology, discharge a large amount of harmful sewage, the healthy drawback of contaminate environment, harm people, provide a kind of method that immobilized enzyme prepares natural gromwell dye, the method adopts immobilized enzyme method to prepare natural dyestuff, green, safety, great pollution can not be caused to environment, also not entail dangers to people's is healthy, and immobilized enzyme can reuse, and has saved the production cost of dyestuff.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be: a kind of immobilized enzyme prepares the method for natural gromwell dye, and its concrete preparation process is:
(1) in the four-hole bottle of 250mL, add the deionized water of 100mL, carry out after being warming up to 45 DEG C stirring and add polyvinyl alcohol solution continuation stirring 30 ~ 40min that 20mL mass concentration is 1%, count by weight, take the initiator Diisopropyl azodicarboxylate of 5 ~ 10 parts successively, the epoxy based monomers glycidyl methacrylate of 30 ~ 65 parts, the linking agent Ethylene glycol dimethacrylate of 10 ~ 20 parts, the pore-creating agent toluene of 20 ~ 40 parts adds in four-hole bottle, be uniformly mixed;
(2) evenly rear adjusting rotary speed to be mixed is 300 ~ 350r/min, 60 ~ 80min is stirred at 45 DEG C, and stop heating after being incubated 3h react 4h at 65 DEG C after at 80 DEG C, adopt ethanol to carry out washing after making it leave standstill to be cooled to 40 DEG C, suction filtration and after completing with deionized water rinsing at 40 DEG C vacuum-drying 24h, sieved by the resin of drying, choosing size is that the resin of 150 ~ 200 μm is as immobilized enzyme resin;
(3) count by weight, take that 40 ~ 60 parts of pH are the citric acid-sodium citrate buffer of the 0.3mol/L of 5.0, the immobilized enzyme resin of the cellulase of 30 ~ 40 parts and zytase mixing solutions and 10 ~ 20 parts vibrates mixing 5 ~ 6h in constant temperature oscillator, the temperature of described constant temperature oscillator is 50 ~ 60 DEG C, and vibration rotating speed is 60r/min;
(4) Asian puccoon is cleaned, smashed and added distilled water by solid-to-liquid ratio 1:8 and obtained Asian puccoon mixed solution, again by mass percentage, choose the deionized water of 30 ~ 65%, 10 ~ 20% immobilized enzyme resin, 20 ~ 40% Asian puccoon mixed solutions and 5 ~ 10% the citric acid-sodium citrate buffer of 0.3mol/L, add in above-mentioned substance and be fully uniformly mixed, and carry out stirring enzymolysis 30 ~ 40min under 50 DEG C of water-baths after, be warming up to 70 DEG C of insulation 1 ~ 2h;
(5) after insulation completes, leave standstill and be cooled to room temperature, agitation and filtration is carried out to it, can natural gromwell dye be obtained.
Described cellulase and zytase mixing solutions cellulase and zytase mass ratio are 3:2.
Application method of the present invention: garlic polysaccharide fixation natural gromwell dye and water are carried out proportioning by 1:20, form dye-dilution solution, by laundry soaMng in natural dyestuff diluent, can dye successfully after slow stirring 20 ~ 24h, clothing after dyeing is exposed to the sun and repetitive scrubbing 30 ~ 40 times in the sun, without any decolouring phenomenon.
The present invention is compared with additive method, and Advantageous Effects is:
(1) immobilized enzyme is reusable, achieves the reusable edible of resource, has saved the production cost of dyestuff;
(2) dyestuff prepared is green, safety, environmentally safe, healthy without harm to people.
Embodiment
First in the four-hole bottle of 250mL, add the deionized water of 100mL, carry out after being warming up to 45 DEG C stirring and add polyvinyl alcohol solution continuation stirring 30 ~ 40min that 20mL mass concentration is 1%, count by weight, take the initiator Diisopropyl azodicarboxylate of 5 ~ 10 parts successively, the epoxy based monomers glycidyl methacrylate of 30 ~ 65 parts, the linking agent Ethylene glycol dimethacrylate of 10 ~ 20 parts, the pore-creating agent toluene of 20 ~ 40 parts adds in four-hole bottle, be uniformly mixed; Evenly rear adjusting rotary speed to be mixed is 300 ~ 350r/min, 60 ~ 80min is stirred at 45 DEG C, and stop heating after being incubated 3h react 4h at 65 DEG C after at 80 DEG C, adopt ethanol to carry out washing after making it leave standstill to be cooled to 40 DEG C, suction filtration and after completing with deionized water rinsing at 40 DEG C vacuum-drying 24h, sieved by the resin of drying, choosing size is that the resin of 150 ~ 200 μm is as immobilized enzyme resin; Count by weight, take that 40 ~ 60 parts of pH are the citric acid-sodium citrate buffer of the 0.3mol/L of 5.0, the immobilized enzyme resin of the cellulase of 30 ~ 40 parts and zytase mixing solutions and 10 ~ 20 parts vibrates mixing 5 ~ 6h in constant temperature oscillator, the temperature of described constant temperature oscillator is 50 ~ 60 DEG C, and vibration rotating speed is 60r/min; Asian puccoon is cleaned, smashed and added distilled water by solid-to-liquid ratio 1:8 and obtained Asian puccoon mixed solution, again by mass percentage, choose the deionized water of 30 ~ 65%, 10 ~ 20% immobilized enzyme resin, 20 ~ 40% Asian puccoon mixed solutions and 5 ~ 10% the citric acid-sodium citrate buffer of 0.3mol/L, add in above-mentioned substance and be fully uniformly mixed, and carry out stirring enzymolysis 30 ~ 40min under 50 DEG C of water-baths after, be warming up to 70 DEG C of insulation 1 ~ 2h; Finally after insulation completes, leave standstill and be cooled to room temperature, agitation and filtration is carried out to it, can natural gromwell dye be obtained; Described cellulase and zytase mixing solutions cellulase and zytase mass ratio are 3:2.
Example 1
First in the four-hole bottle of 250mL, add the deionized water of 100mL, carry out after being warming up to 45 DEG C stirring and add the polyvinyl alcohol solution continuation stirring 30min that 20mL mass concentration is 1%, count by weight, take the initiator Diisopropyl azodicarboxylate of 5 parts successively, the epoxy based monomers glycidyl methacrylate of 45 parts, the linking agent Ethylene glycol dimethacrylate of 10 parts, the pore-creating agent toluene of 40 parts adds in four-hole bottle, be uniformly mixed; Evenly rear adjusting rotary speed to be mixed is 300r/min, 60min is stirred at 45 DEG C, and stop heating after being incubated 3h react 4h at 65 DEG C after at 80 DEG C, adopt ethanol to carry out washing after making it leave standstill to be cooled to 40 DEG C, suction filtration and after completing with deionized water rinsing at 40 DEG C vacuum-drying 24h, sieved by the resin of drying, choosing size is that the resin of 150 μm is as immobilized enzyme resin; Count by weight, take that 40 parts of pH are the citric acid-sodium citrate buffer of the 0.3mol/L of 5.0, the immobilized enzyme resin of the cellulase of 40 parts and zytase mixing solutions and 20 parts vibrates mixing 5h in constant temperature oscillator, the temperature of described constant temperature oscillator is 50 DEG C, and vibration rotating speed is 60r/min; Asian puccoon is cleaned, smashed and added distilled water by solid-to-liquid ratio 1:8 and obtained Asian puccoon mixed solution, again by total mass 100g, choose the citric acid-sodium citrate buffer of the 0.3mol/L of the deionized water of 50g, the immobilized enzyme resin of 20g, 25g Asian puccoon mixed solution and 5g, add in above-mentioned substance and be fully uniformly mixed, and carry out stirring enzymolysis 30min under 50 DEG C of water-baths after, be warming up to 70 DEG C of insulation 1h; Finally after insulation completes, leave standstill and be cooled to room temperature, agitation and filtration is carried out to it, can natural gromwell dye be obtained; Described cellulase and zytase mixing solutions cellulase and zytase mass ratio are 3:2.
Garlic polysaccharide fixation natural gromwell dye and water are carried out proportioning by 1:20, form dye-dilution solution, by laundry soaMng in natural dyestuff diluent, can dye successfully after slowly stirring 20h, clothing after dyeing is exposed to the sun and repetitive scrubbing 30 times in the sun, without any decolouring phenomenon.
Example 2
First in the four-hole bottle of 250mL, add the deionized water of 100mL, carry out after being warming up to 45 DEG C stirring and add the polyvinyl alcohol solution continuation stirring 35min that 20mL mass concentration is 1%, count by weight, take the initiator Diisopropyl azodicarboxylate of 8 parts successively, the epoxy based monomers glycidyl methacrylate of 39 parts, the linking agent Ethylene glycol dimethacrylate of 15 parts, the pore-creating agent toluene of 38 parts adds in four-hole bottle, be uniformly mixed; Evenly rear adjusting rotary speed to be mixed is 325r/min, 70min is stirred at 45 DEG C, and stop heating after being incubated 3h react 4h at 65 DEG C after at 80 DEG C, adopt ethanol to carry out washing after making it leave standstill to be cooled to 40 DEG C, suction filtration and after completing with deionized water rinsing at 40 DEG C vacuum-drying 24h, sieved by the resin of drying, choosing size is that the resin of 175 μm is as immobilized enzyme resin; Count by weight, take that 50 parts of pH are the citric acid-sodium citrate buffer of the 0.3mol/L of 5.0, the immobilized enzyme resin of the cellulase of 40 parts and zytase mixing solutions and 10 parts vibrates mixing 5.5h in constant temperature oscillator, the temperature of described constant temperature oscillator is 55 DEG C, and vibration rotating speed is 60r/min; Asian puccoon is cleaned, smashed and added distilled water by solid-to-liquid ratio 1:8 and obtained Asian puccoon mixed solution, again by total mass 100g, choose the citric acid-sodium citrate buffer of the 0.3mol/L of the deionized water of 45g, the immobilized enzyme resin of 20g, 30g Asian puccoon mixed solution and 10g, add in above-mentioned substance and be fully uniformly mixed, and carry out stirring enzymolysis 35min under 50 DEG C of water-baths after, be warming up to 70 DEG C of insulation 1.5h; Finally after insulation completes, leave standstill and be cooled to room temperature, agitation and filtration is carried out to it, can natural gromwell dye be obtained; Described cellulase and zytase mixing solutions cellulase and zytase mass ratio are 3:2.
Garlic polysaccharide fixation natural gromwell dye and water are carried out proportioning by 1:20, form dye-dilution solution, by laundry soaMng in natural dyestuff diluent, can dye successfully after slowly stirring 22h, clothing after dyeing is exposed to the sun and repetitive scrubbing 35 times in the sun, without any decolouring phenomenon.
Example 3
First in the four-hole bottle of 250mL, add the deionized water of 100mL, carry out after being warming up to 45 DEG C stirring and add the polyvinyl alcohol solution continuation stirring 40min that 20mL mass concentration is 1%, count by weight, take the initiator Diisopropyl azodicarboxylate of 10 parts successively, the epoxy based monomers glycidyl methacrylate of 35 parts, the linking agent Ethylene glycol dimethacrylate of 20 parts, the pore-creating agent toluene of 35 parts adds in four-hole bottle, be uniformly mixed; Evenly rear adjusting rotary speed to be mixed is 350r/min, 80min is stirred at 45 DEG C, and stop heating after being incubated 3h react 4h at 65 DEG C after at 80 DEG C, adopt ethanol to carry out washing after making it leave standstill to be cooled to 40 DEG C, suction filtration and after completing with deionized water rinsing at 40 DEG C vacuum-drying 24h, sieved by the resin of drying, choosing size is that the resin of 200 μm is as immobilized enzyme resin; Count by weight, take that 52 parts of pH are the citric acid-sodium citrate buffer of the 0.3mol/L of 5.0, the immobilized enzyme resin of the cellulase of 33 parts and zytase mixing solutions and 15 parts vibrates mixing 6h in constant temperature oscillator, the temperature of described constant temperature oscillator is 60 DEG C, and vibration rotating speed is 60r/min; Asian puccoon is cleaned, smashed and added distilled water by solid-to-liquid ratio 1:8 and obtained Asian puccoon mixed solution, again by total mass 100g, choose the citric acid-sodium citrate buffer of the 0.3mol/L of the deionized water of 53g, the immobilized enzyme resin of 15g, 24g Asian puccoon mixed solution and 8g, add in above-mentioned substance and be fully uniformly mixed, and carry out stirring enzymolysis 40min under 50 DEG C of water-baths after, be warming up to 70 DEG C of insulation 2h; Finally after insulation completes, leave standstill and be cooled to room temperature, agitation and filtration is carried out to it, can natural gromwell dye be obtained; Described cellulase and zytase mixing solutions cellulase and zytase mass ratio are 3:2.
Garlic polysaccharide fixation natural gromwell dye and water are carried out proportioning by 1:20, form dye-dilution solution, by laundry soaMng in natural dyestuff diluent, can dye successfully after slowly stirring 24h, clothing after dyeing is exposed to the sun and repetitive scrubbing 40 times in the sun, without any decolouring phenomenon.
Claims (2)
1. immobilized enzyme prepares a method for natural gromwell dye, it is characterized in that concrete preparation process is:
(1) in the four-hole bottle of 250mL, add the deionized water of 100mL, carry out after being warming up to 45 DEG C stirring and add polyvinyl alcohol solution continuation stirring 30 ~ 40min that 20mL mass concentration is 1%, count by weight, take the initiator Diisopropyl azodicarboxylate of 5 ~ 10 parts successively, the epoxy based monomers glycidyl methacrylate of 30 ~ 65 parts, the linking agent Ethylene glycol dimethacrylate of 10 ~ 20 parts, the pore-creating agent toluene of 20 ~ 40 parts adds in four-hole bottle, be uniformly mixed;
(2) evenly rear adjusting rotary speed to be mixed is 300 ~ 350r/min, 60 ~ 80min is stirred at 45 DEG C, and stop heating after being incubated 3h react 4h at 65 DEG C after at 80 DEG C, adopt ethanol to carry out washing after making it leave standstill to be cooled to 40 DEG C, suction filtration and after completing with deionized water rinsing at 40 DEG C vacuum-drying 24h, sieved by the resin of drying, choosing size is that the resin of 150 ~ 200 μm is as immobilized enzyme resin;
(3) count by weight, take that 40 ~ 60 parts of pH are the citric acid-sodium citrate buffer of the 0.3mol/L of 5.0, the immobilized enzyme resin of the cellulase of 30 ~ 40 parts and zytase mixing solutions and 10 ~ 20 parts vibrates mixing 5 ~ 6h in constant temperature oscillator, the temperature of described constant temperature oscillator is 50 ~ 60 DEG C, and vibration rotating speed is 60r/min;
(4) Asian puccoon is cleaned, smashed and added distilled water by solid-to-liquid ratio 1:8 and obtained Asian puccoon mixed solution, again by mass percentage, choose the deionized water of 30 ~ 65%, 10 ~ 20% immobilized enzyme resin, 20 ~ 40% Asian puccoon mixed solutions and 5 ~ 10% the citric acid-sodium citrate buffer of 0.3mol/L, add in above-mentioned substance and be fully uniformly mixed, and carry out stirring enzymolysis 30 ~ 40min under 50 DEG C of water-baths after, be warming up to 70 DEG C of insulation 1 ~ 2h;
(5) after insulation completes, leave standstill and be cooled to room temperature, agitation and filtration is carried out to it, can natural gromwell dye be obtained.
2. a kind of immobilized enzyme according to claims 1 prepares the method for natural gromwell dye, it is characterized in that, described cellulase and zytase mixing solutions cellulase and zytase mass ratio are 3:2.
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2015
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Patent Citations (4)
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| CN102432744A (en) * | 2011-09-07 | 2012-05-02 | 天津大学 | Method for preparing monodispersed functional polymer microspheres |
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